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Dc in Vit Nam III
1-ACID ACETYLSALICYLIC
Acidum acetylsalicylicum
Aspirin
C9H8O4
P.t.l: 180,2
Acid acetylsalicylic l acid 2-acetoxybenzoic, phi cha t 99,5 n l01,0%

C9H8O4, tnh theo ch phm lm kh.
Tnh cht
Tinh th khng mu hoc bt kt tinh trng, khng mi hoc gn nh
khng mi. Kh tan trong nc, d tan trong ethanol 96%, tan trong ether v
cloroform.
Chy khong 143oC (Ph lc 5. 19, Phng php 3).
nh tnh
C th chn mt trong hai nhm nh tnh sau:
Nhm I: A, B
Nhm II: B, C, D
A. Ph hng ngoi (Ph lc 3.2) ca ch phm phi ph hp vi ph hng
ngoi ca acid acetylsalicylic chun.
B. un si 0,2 g ch phm vi 4 ml dung dch natri hydroxyd long (TT)
trong 3 pht, ngui v thm 5 ml dung dch acid sulfuric l0% (TT). Ta kt tinh
c to thnh. Ta sau khi c lc, ra vi nc v sy kh l00 - l05oC, c
im chy t 156 n 161oC (Ph lc 5.19).
C. Trong mt ng nghim, trn 0,1 g ch phm vi 0,5 g calci hydroxyd
(TT).
un hn hp v cho khi sinh ra tip xc vi ming giy lc tm 0,05 ml

dung dch nitrobenzaldehyd (TT) s xut hin mu xanh l cy hi vng, hoc
xanh l cy hi xanh lam. Lm m t giy lc vi dung dch acid hydrocloric
long (TT), mu s chuyn thnh xanh lam.
D. Ha tan bng cch un nng khong 20 mg ta thu c t php th B
trong l0 ml nc v lm ngui. Dung dch thu c cho phn ng ca salicylat
(Ph lc 7.l).
trong v mu sc ca dung dch
Ha tan l,0 g ch phm trong 9 ml ethanol 96% (TT). Dung dch phi trong
(Ph lc 5.12) v khng mu (Ph lc 5.17, phng php 2).
Tp cht lin quan
Trong bnh nh mc dung tch l00 ml, ha tan 0,15 g ch phm trong l0 ml
dung dch tetrabutylamoni hydroxyd 0,1 M trong 2 - propanol, yn 10 pht.
Thm 8,0 ml dung dch acid hydrocloric 0,1 N v 20,0 ml natri tetraborat l,9% v
trn u. Thm 2,0 ml dung dch aminopyrazolon l,0% v 2,0 ml dung dch kali
fericyanid l,0%, trong qu trnh thm cc dung dch ny lc lin tc. Sau 2 pht,
pha long n 100,0 ml bng nc. yn 20 pht. o hp th ca dung dch
bc sng 505 nm trong cc o dy 2 cm, dng nc lm mu trng. hp th
thu c khng c ln hn 0,25 (khong 0,l% biu th bng acid
acetylsalicylic).
Acid salicylic
Khng c qu 0,05%.
Ha tan 0,l0 g ch phm trong 5 ml ethanol 96% (TT), thm ngay 15 ml
nc c lm lnh trong nc v 0,05 ml dung dch st (III) clorid 0,5%.
Sau 1pht dung dch ny khng c c mu thm hn mu ca dung dch i
chiu chun b ng thi bng cch cho hn hp gm 0,05 ml dung dch st (III)
clorid 0,5%, 0,1 ml acid acetic (TT), 4 ml ethanol 96% (TT) v 15 ml nc vo 1

ml dung dch ca 5,0 mg acid salicylic trong 100 ml ethanol 96% (TT).
Clorid
Khng c qu 0,015% (Ph lc 7.4.5)
Dung dch S: un si 4,0 g ch phm vi l00 ml nc trong 5 pht,
ngui, thm nc va 100 ml v lc.
Ly 8,3 ml dung dch S, pha long vi nc va 15 ml v tin hnh th.
Sulfat
Khng c qu 0,040% (Ph lc 7.4.12).
Kim loi nng
Khng c qu 20 phn triu (Ph lc 7.4.7).
Ha tan 0,75 g ch phm trong 9 ml aceton (TT) v pha long vi nc va
15 ml. Ly 12 ml dung dch ny th theo phng php 2. Pha long dung dch
ch mu l00 phn triu bng hn hp gm 9 th tch aceton (TT) v 6 th tch nc
c dung dch ch mu 1 phn triu chun b mu i chiu.
Mt khi lng do lm kh
Khng c qu 0,5% (Ph lc 5.16).
(l,00 g; p sut gim; phosphor pentoxyd).
Tro sulfat
Khng c qu 0,l% (Ph lc 7.7, phng php 2)
Dng l,0 g ch phm.
nh lng
Ha tan 1,000 g ch phm trong 10 ml ethanol 96% (TT) trong bnh nn

nt mi. Thm 50,0 ml dung dch natri hydroxyd 0,5 M. y nt bnh v yn
trong 1 gi. Chun bng dung dch acid hydrocloric 0,5 M, dng 0,2 ml dung
dch phenolphtalein (CT) lm ch th.
Song song lm mu trng.
1 ml dung dch natri hydroxyd 0,5 M tng ng vi 45,04 mg C9H8O4.
Bo qun
Ch phm c bo qun trong chai l nt kn, trnh nh sng.
Cng dng
H nhit, gim au, khng vim.
Ch phm
Vin nn aspirin.
2 -ACID ASCORBIC
Acidum ascorbicum
Vitamin C, Acid L-ascorbic
C6H8O6
P.t.l: 176,1
Acid ascorbic l (R)-5-[(S)-1,2-dihydroxyethyl]-3,4-dihydroxy-5H-furan 2on, phi cha t 99,0 n 100,5% C6H8O6.

Tnh cht
Tinh th khng mu hay bt kt tinh trng hoc gn nh trng, b bin mu
khi tip xc vi khng kh, nh sng v m. Khng mi hoc gn nh khng mi.
D tan trong nc, tan trong ethanol 96%, thc t khng tan trong cloroform v
ether. Chy khong 1900C cng vi phn hu.
nh tnh

Nhm I: B,C
Nhm II: A, C, D
Dung dch S: Ha tan 1,0 g ch phm trong nc khng c carbon dioxyd
(TT) v pha long n 20 ml bng cng dung mi.
A. Ho tan 0,10 g ch phm trong nc v pha long ngay n 100,0 ml
bng cng dung mi. Cho 1,0 ml dung dch mi pha vo 10 ml dung dch acid
hydrocloric 0,1 N v pha long n 100,0 ml bng nc. o ph hp th t ngoi
(Ph lc 3.1) ngay sau khi dung dch c pha long. Dung dch ch c duy nht
mt cc i hp th 243 nm. Gi tr A(1%, 1 cm) 243 nm t 545 n 585.
B. Ph hng ngoi (Ph lc 3.2) ca ch phm phi ph hp vi ph hng
ngoi ca acid ascorbic chun. Dp vin cha 1 mg ch phm.
C. pH ca dung dch S nm trong khong 2,1 n 2,6 (Ph lc 5.9).
D. Thm 0,2 ml dung dch acid nitric long (TT) v 0,2 ml dung dch bc
nitrat 2% (TT) vo 1 ml dung dch S, s xut hin ta mu xm.
Dung dch S phi trong (Ph lc 5.12) v mu khng c m hn mu
mu NV7 (Ph lc 5.17, phng php 2).
Gc quay cc ring
+ 20,5 n + 21,5o (Ph lc 5.13)
Ha tan 2,50 g ch phm trong nc v pha long n 25,0 ml bng cng
dung mi tin hnh th.
Acid oxalic
Khng c qu 0,2%.
Chun b ng thi dung dch th v dung dch i chiu nh sau:
Dung dch th: Ha tan 0,25 g ch phm trong 5 ml nc. Trung tnh ha
bng dung dch natri hydroxyd 2 M vi giy qu (CT).
Dung dch i chiu: Ha tan 70 mg acid oxalic trong nc v pha long
n 500 ml bng cng dung mi, dng 5,0 ml dung dch ny chun b mu i
chiu.
Thm ng thi vo mi dung dch trn l ml dung dch acid acetic 2 M
(TT) v 0,5 ml dung dch calci clorid 0,5 M (TT). yn trong 1 gi. Dung dch
th khng c c hn dung dch i chiu.
ng
Khng c qu 5 phn triu.
Xc nh bng phng php quang ph hp th nguyn t. (Ph lc 3.4,
phng php 1).
Dung dch th: Ha tan 2,0 g ch phm trong dung dch acid nitric 0,1 M
va 25,0 ml.
Dung dch chun: Chun b cc dung dch chun ng c cha 0,2; 0,4 v
0,6 phn triu bng cch pha long dung dch ng mu 10 phn triu bng dung
dch acid nitric 0,1 M.
o hp th 324,8 nm, dng n cathod rng ng lm ngun bc x
v ngn la khng kh- acetylen. Dng dung dch acid nitric 0,1 M hiu chnh
my v zero.
St
Xc nh bng phng php quang ph hp th nguyn t. (Ph lc 3.4,
phng php 1).
Dung dch th: Ha tan 5,0 g ch phm trong dung dch acid nitric 0,1 M
va 25,0 ml.
Dung dch chun: Chun b cc dung dch chun st c cha 0,2; 0,4 v 0,6
phn triu bng cch pha long dung dch st mu 20 phn triu bng dung dch
acid nitric 0,1 M.
o hp th 248,3 nm, dng n cathod rng st lm ngun bc x v
ngn la khng kh - acetylen. Dng dung dch acid nitric 0,1 M hiu chnh
my v zero.
Kim loi nng
Ly 2,0 g ch phm th theo phng php 4. Dng 2 ml dung dch ch
mu 10 phn triu chun b mu i chiu.
Tro sulfat
Khng c qu 0,l% (Ph lc 7.7, phng php 2).
Dng 1,0 g ch phm.
nh lng
Ha tan 0,150 g ch phm trong mt hn hp gm 80 ml nc khng c
carbon dioxyd (TT) v 10 ml dung dch acid sulfuric 1 M. Thm 1 ml dung dch
h tinh bt (CT). Chun bng dung dch iod 0,1 N cho ti khi xut hin mu
xanh tm bn vng.
1 ml dung dch iod 0,1 N tng ng vi 8,81 mg C6H8O6.
Bo qun
Trong chai l kn, trnh m, trnh tip xc vi kim loi v nh sng.
Cng dng
Vitamin chng scorbus v l cht n nh dc phm (chng oxy ho).
Dng tr liu thiu vitamin C.
Ch phm
Vin nn, vin nang, thuc tim.
3-ACID BENZOIC
Acidum benzoicum
C7H6O2
P.t.l: 122,1
Acid benzoic l acid benzen carboxylic, phi cha t 99,0 n 100,5%

C7H6O2, tnh theo ch phm lm kh.
Tnh cht
Tinh th hnh kim hay mnh khng mu hoc bt kt tinh trng, khng mi
hoc thong mi cnh kin trng. Kh tan trong nc, tan trong nc si, d tan
trong ethanol 96%, ether, cloroform v du bo.
nh tnh
A. Ho tan 1 g ch phm trong 8 ml dung dch natri hydroxyd 0,1 N v
thm nc va 100 ml. Dung dch ny phi cho phn ng ca ion benzoat (Ph
lc 7.1).
B. im chy: 121 - 124oC (Ph lc 5.19).
Dung dch S: Ho tan 5,0 g ch phm trong ethanol 96% (TT) c
100,0 ml.
Dung dch S phi trong (Ph lc 5.12) v khng mu (Ph lc 5.17, phng
php 2).
Cc hp cht cha clor
Cho vo chn nung 0,50 g ch phm v 0,70 g calci carbonat (TT), trn u
vi mt lng nc nh v sy kh. Nung 600oC n khi than ho hon ton.
Ho tan cn trong 20 ml dung dch acid nitric 2 M ri lc. Ra cn v phu lc
bng 15 ml nc. Tp trung dch lc v nc ra, thm nc va 50 ml; thm
0,5 ml dung dch bc nitrat 0,1 N. Dung dch thu c khng c c hn dung
dch i chiu c chun b nh sau:
Ho tan 0,70 g calci carbonat (TT) trong 20 ml dung dch acid nitric 2 M
(TT) ri lc. Ra cn v phu lc bng 15 ml nc. Tp trung dch lc v nc
ra; thm 1,2 ml dung dch acid hydrocloric 0,01 N v thm nc va 50 ml.
Tip tc thm 0,5 ml dung dch bc nitrat 0,1 N.
Cht kh kali permanganat
Thm tng git dung dch kali permanganat 0,1 N vo 100 ml nc
c acid ho bng 1,5 ml dung dch acid sulfuric 10% (TT) ang si n khi mu
xut hin v bn vng trong 30 giy. Ho tan 1,0 g ch phm trong dung dch
ang nng trn v chun bng dung dch kali permanganat 0,1 N n khi c
mu hng bn vng trong 15 giy. Lng dung dch kali permangant 0,1 N tiu
th khng c qu 0,5 ml.
Tp cht hu c
Ho tan 0,50 g ch phm trong 5 ml acid sulfuric m c (TT) v yn
trong 5 pht. Dung dch thu c khng c c mu thm hn mu ca mu mu
V5 (Ph lc 5.17, phng php 1).
Kim loi nng
Ly 12 ml dung dch S v tin hnh th theo phng php 2. Dung dch i

chiu l dung dch gm 5 ml ethanol 96% (TT) trn u vi 5 ml dung dch ch
mu 1 phn triu v 2 ml dung dch S.
Tro sulfat
Khng c qu 0,1% (Ph lc 7.7, phng php 2).
Dng 1,0 g ch phm.
Mt khi lng do lm kh
Khng c qu 0,5% (Ph lc 5.16).
(1,000 g; silicagel).
nh lng
Ho tan khong 0,200 g ch phm trong 20 ml ethanol 96% (TT) trung
tnh ho bng dung dch natri hydroxyd 0,1 N vi dung dch phenolphtalein (CT),
thm 20 ml nc v vi git dung dch phenolphtalein (CT), chun bng dung
dch natri hydroxyd 0,1 N.
1 ml dung dch natri hydroxyd 0,1 N tng ng vi 12,21 mg C7H6O2.
Bo qun
Ch phm c bo qun trong chai l nt kn.
Cng dng
Khng nm, cht bo qun chng vi sinh vt.
4-ACID CITRIC NGM MT PHN T NC
Acidum citricum monohydricum
C6H8O7. H2O
P.t.l: 210,1
Acid citric ngm mt phn t nc l acid 2 - hydroxypropan - 1,2,3 tricarboxylic, phi cha t 99,5 n 101,0% C6H8O7, tnh theo ch phm khan.
Tnh cht
Bt kt tinh trng hoc tinh th hay dng ht khng mu. Ln hoa. Rt d
tan trong nc, d tan trong ethanol 96%, hi tan trong ether.
nh tnh
Nhm I: B, E
Nhm II: A, C, D, E
A. Ho tan 1 g ch phm trong 10 ml nc, dung dch thu c phi c pH
nh hn 4 (Ph lc 5.9) B. Ph hng ngoi (Ph lc 3.2) ca ch phm phi ph
hp vi ph hng ngoi ca acid citric monohydrat chun, o sau khi mu th v
chun c sy 100 n 105oC trong 24 gi.
C. Thm khong 5 mg ch phm vo hn hp gm 1 ml anhydrid acetic
(TT) v 3 ml pyridin (TT). Mu xut hin.
D. Ho tan 0,5 g ch phm trong 5 ml nc, trung ho bng dung dch natri
hydroxyd 1 M (khong 7 ml), thm 10 ml dung dch calci clorid (TT), un si, kt
ta trng c to thnh.
E. Ch phm phi p ng php th nc.
Ho tan 2,0 g ch phm trong 10 ml nc. Dung dch phi trong (Ph lc
5.12) v khng c c mu m hn mu mu V7, NV7 hay LV7 (Ph lc 5.17,
phng php 2).
Cht d b carbon ho
Cho 1,0 g ch phm vo ng nghim, thm 10 ml acid sulfuric (TT), un

ngay hn hp trong cch thu 900
10C trong 1 gi. Lm ngui tht nhanh,
dung dch khng c c mu m hn mu ca hn hp gm 1 ml dung dch u

mu v 9 ml dung dch u mu vng (Ph lc 5.17, phng php 1).
Acid oxalic
Trung ho 10 ml dung dch ch phm 10% trong nc bng dung dch
amoni hydroxyd 6 N (TT), thm 5 git dung dch acid hydrocloric 3 N (TT),
ngui. Thm 2 ml dung dch calci clorid (TT), dung dch khng c c.
Sulfat
Khng c qu 0,015% (Ph lc 7.4.12)
Ha tan 1,0 g ch phm trong nc c 15 ml v tin hnh th.
Nhm
Khng c qu 0,2 phn triu (Ph lc 7.4.8).
Nu ch phm c dng pha ch dung dch thm phn th phi t php
th ny.
Dung dch th: Ho tan 20 g ch phm trong 100 ml nc, thm 10 ml
dung dch m acetat pH 6,0.
Dung dch i chiu: Hn hp gm 2 ml dung dch nhm mu 2 phn triu,
10 ml dung dch m acetat pH 6,0 v 98 ml nc.
Dung dch mu trng: Hn hp gm 10 ml dung dch m acetat pH 6,0 v
100 ml nc.
Kim loi nng
Ho tan 5,0 g ch phm lm nhiu ln trong 39 ml dung dch natri
hydroxyd long (TT), pha long vi nc n 50 ml. Ly 12 ml dung dch ny tin
hnh th theo phng php 1. Dng dung dch ch mu 1 phn triu chun b
mu i chiu.
Nc
T 7,5 n 9,0% (Ph lc 6.6).
Dng 0,500 g ch phm.
Tro sulfat
Dng 1,0 g ch phm.
Ni c t vi khun
Nu ch phm c dng pha ch cc dng thuc tim phn liu m
khng c phng php no khc loi ni c t vi khun th ch phm phi
khng c c vt qu 0,5 n v ni c t cho mi miligam (Ph lc 10.3).
nh lng
Ho tan 0,550 g ch phm trong 50 ml nc. Chun bng dung dch
natri hydroxyd 1 N, dng 0,5 ml dung dch phenolphtalein (CT) lm ch th.
1 ml dung dch natri hydroxyd 1 N tng ng vi 64,03 mg C6H8O7.
Bo qun
Trong l kn.
5-ACID SALICYLIC
Acidum salicylicum
C7H6O3
P.t.l: 138,1
Acid salicylic l acid 2 - hydroxybenzencarboxylic, phi cha t 99,0 n

100,5% C7H6O3, tnh theo ch phm lm kh.
Tnh cht
Tinh th hnh kim mu trng hoc khng mu hay bt kt tinh trng. Kh
tan trong nc, d tan trong ethanol 96% v ether, hi tan trong cloroform. Dung
dch ch phm c phn ng acid.
nh tnh
Chn mt trong hai nhm nh tnh sau:
Nhm I: A, C
Nhm II: B, C A. Ph hng ngoi (Ph lc 3.2) ca ch phm phi ph
hp vi ph hng ngoi ca acid salicylic chun.
B. Ho tan 0,01 g ch phm trong 5 ml nc bng cch un nng, ngui.
Thm 1 git dung dch st (III) clorid 5% (TT) s xut hin mu tm.
C. im chy: 158 - 161oC (Ph lc 5.19).
Ho tan 1,0 g ch phm trong 10,0 ml ethanol 96% (TT). Dung dch phi
trong (Ph lc 5.12) v khng mu (Ph lc 5.17, phng php 2).
Dung dch S: Ho tan 2,5 g ch phm trong 50 ml nc si, ngui v
lc.
Clorid
Khng c qu 0,010% (Ph lc 7.4.5).
Ly 10 ml dung dch S pha long thnh 15 ml bng nc v tin hnh th.
Sulfat
Khng c qu 0,020% (Ph lc 7.4.12).
Ly 15 ml dung dch S v tin hnh th.

Kim loi nng
Ho tan 2,0 g ch phm trong 15 ml ethanol 96% (TT), sau thm 5 ml
nc. Ly 12 ml dung dch ny th theo phng php 2. Dng dung dch ch mu
100 phn triu pha long bng hn hp dung mi ethanol 96% - nc (3: 1)
c dung dch ch mu 2 phn triu dng chun b mu i chiu.
Mt khi lng do lm kh
Khng c qu 0,5% (Ph lc 5.16).
(1,000 g; p sut gim; silicagel).
Tro sulfat
Dng 2,0 g ch phm.
nh lng
Ho tan khong 0,250 g ch phm trong 25 ml ethanol 96% (TT) c
trung tnh ho bng dung dch natri hydroxyd 0,1 N vi dung dch phenolphtalein
(CT), thm 20 ml nc v vi git dung dch phenolphtalein (CT). Chun bng
dung dch natri hydroxyd 0,1 N.
1 ml dung dch natri hydroxyd 0,1 N tng ng vi 13,81 mg C7H6O3.
Bo qun
Ch phm c bo qun trong chai l nt kn, trnh nh sng.
6-AMINOPHYLIN
Aminophyllinum
Theophylin v ethylendiamin
(C7H8 N4O2)2. C2H8 N2

P.t.l: 420,4 (Aminophylin khan)
(C7H8 N4O2)2. C2H8 N2. 2H2O
P.t.l:
456,6
(Aminophylin
dihydrat)
Aminophylin l hn hp n nh ca theophylin v ethylendiamin. Ch
phm c th khan hoc ngm khng nhiu hn hai phn t nc, phi cha t 84,0
n 87,4% C7H8 N4O2 v t 13,5 n 15,0% C2H8 N2, tnh theo ch phm khan.
Tnh cht
Bt trng hay hi vng, hoc ht nh, thong mi amoniac, v ng. Di
tc dng ca khng kh m, nh sng, nhit cao, aminophylin b bin mu.
ngoi khng kh aminophylin t t b mt ethylendiamin, ng thi hp thu carbon
dioxyd, gii phng theophylin t do. ni thiu nh sng, n b phn hu t t khi
tip xc vi khng kh m. S phn hu xy ra nhanh hn nhit cao.
D tan trong nc (dung dch c th tr nn c khi hp thu carbon
dioxyd), thc t khng tan trong ethanol v ether.
nh tnh
Nhm I: B, C, E.
Nhm II: A, C, D, E, F.
Ho tan 1,0 g ch phm trong 10 ml nc , thm tng git 2 ml dung dch

acid hydrocloric long (TT) v lc, lc. Ta dng lm nh tnh A, B, D v F.
Dch lc dng lm nh tnh C.
A. Ta c ra bng nc v sy kh 100 n 105oC, c im chy t
270 n 274oC (Ph lc 5.19).
B. Ph hng ngoi (Ph lc 3.2) ca ta c ra bng nc v sy kh
100 n 105oC phi ph hp vi ph hng ngoi i chiu ca theophylin hoc
ph hng ngoi ca theophylin chun.
C. Thm 0,2 ml benzoyl clorid (TT) vo dch lc. Kim ho bng dung dch
natri hydroxyd long (TT) v lc k. Lc ly ta, ra bng 10 ml nc , ha tan
trong 5 ml ethanol 96% (TT) nng ri thm 5 ml nc. Ta to thnh, sau khi
c ra v sy kh 100 n 105oC, c im chy t 248 n 252oC (Ph lc
5.19).
D. Ho tan khong 10 mg ta trong 10 ml nc, thm 0,5 ml dung dch
thu ngn (II) acetat 5% v yn, s xut hin ta tinh th trng.
E. Phi p ng php th nc (xem php th nc).
F. Ta cho phn ng ca nhm xanthin (Ph lc 7.1).
Ho tan 0,5 g ch phm trong 10 ml nc khng c carbon dioxyd (TT)
bng cch un nng. Dung dch khng c c hn c mu S2 (Ph lc
5.12) v khng c m mu hn mu mu LV6 (Ph lc 5.17, phng php 2).
Kim loi nng
Ly 1,0 g ch phm th theo phng php 3. Dng 2 ml dung dch ch mu
10 phn triu chun b mu i chiu.
Tp cht lin quan

Khng c qu 0,5%.
Tin hnh theo phng php sc k lp mng (Ph lc 4.4).
Bn mng: Silicagel GF254
Dung mi khai trin: Amoniac m c - aceton - cloroform - butanol (10:
30: 30: 40). Dung dch th: Ho tan 0,2 g ch phm trong 2 ml nc bng cch
un nng v pha long ti 10 ml bng methanol (TT).
Dung dch i chiu: Pha long 0,5 ml dung dch th ti 100 ml bng
methanol (TT).
Cch tin hnh: Chm ring bit ln bn mng 10 l mi dung dch trn.
Trin khai bn mng ti khi dung mi i c khong 15 cm. kh bn mng
ngoi khng kh, v quan st di nh sng t ngoi bc sng 254 nm. Trn
sc k ca dung dch th ngoi vt chnh bt k vt ph no xut hin u
khng c m mu hn vt ca dung dch i chiu.
Nc
Khng c qu 1,5% (i vi dng khan) (Ph lc 6.6). Xc nh trn
2,000 g ch phm ho tan trong 20 ml pyridin khan (TT). T 3,0 n 8,0% (i
vi dng ngm nc) (Ph lc 6.6). Xc nh trn 0,500 g ch phm ho tan trong
20 ml pyridin khan (TT).
Tro sulfat
Dng 1,0 g ch phm.
nh lng
Ethylendiamin: Ho tan 0,250 g ch phm trong 30 ml nc, thm 0,1 ml

dung dch lc bromocresol (CT1). Chun bng dung dch acid hydrocloric 0,1
M cho ti khi xut hin mu xanh lc.
1 ml dung dch acid hydrocloric 0,1 M tng ng vi 3,005 mg C2H8
N2.
Theophylin: Sy khong 0,200 g ch phm 135oC n khi lng khng
i. Ho tan cn trong 100 ml nc bng cch un nng, ngui, thm 20 ml
dung dch bc nitrat 0,1 N v lc. Thm 1 ml dung dch xanh bromothymol (CT)
v chun bng dung dch natri hydroxyd 0,1 M cho ti khi c mu xanh l.
1 ml dung dch natri hydroxyd 0,1 M tng ng vi 18,02 mg C7H8
N4O2.
Bo qun
Trong chai l nt kn, trnh nh sng.
Ch phm
Thuc tim aminophylin. Vin nn aminophylin
Tc dng v cng dng
Gin kh - ph qun, gin c trn mch mu, li tiu. Tr hen suyn.
7-AMPICILIN
Ampicillinum
C16H19 N3O4S
P.t.l: 349,40
Ampicilin l acid (6R) -6 -( - D - phenylglycylamino) penicilanic, phi

cha t 96,0 n 100,5% C16H19 N3O4S, tnh theo ch phm khan.
Tnh cht
Bt kt tinh trng, khng mi hoc hu nh khng mi.
Hi tan trong nc, thc t khng tan trong ethanol, cloroform, ether, du
bo. Tan trong dung dch acid long v dung dch hydroxyd kim.
nh tnh
Nhm I: A, D
Nhm II: B, C, D
ngoi ca ampicilin chun.
B. Tin hnh phng php sc k lp mng theo nh tnh cc penicilin
(Ph lc 7. 2).
Dng pha ng B.
C. Phn ng B trong php th phn ng mu ca cc penicilin v
cephalosporin (Ph lc 7. 3).
D. Phi p ng php th nc (xem php th nc).
pH
T 3,5 n 5,5 (Ph lc 5.9).
Xc nh trn dung dch ch phm 0,25% trong nc khng c carbon
dioxyd (TT).
trong ca dung dch
Ho tan 1,0 g ch phm trong 10 ml dung dch acid hydrocloric 1 M, ng
thi ho tan 1,0 g ch phm trong 10 ml dung dch amoniac 2 M. Quan st ngay
sau khi ho tan. C hai dung dch trn khng c c hn c mu S2 (Ph

lc 5.12).
Gc quay cc ring
T + 280 n + 350o, tnh theo ch phm khan (Ph lc 5.13).
Xc nh trn dung dch ch phm 0,25% trong nc khng c carbon
dioxyd (TT).
Kim loi nng
Ly 1,0 g ch phm tin hnh theo phng php 3. Dng 2 ml dung dch
ch mu 10 phn triu chun b mu i chiu.
N,N- Dimethylanilin
Xc nh bng phng php sc k kh (Ph lc 4.2).
Dung dch chun ni: Dung dch naphthalen 0,005% trong cyclohexan
(TT). Dung dch th: Ho tan 1,0 g trong 5 ml dung dch natri hydroxyd 1 M,
thm 1 ml dung dch chun ni. Lc mnh trong 1 pht, ly tm nu cn v ly lp
trong pha trn.
Dung dch i chiu: Ho tan 50 mg N, N - dimethylanilin trong hn hp
gm 2 ml acid hydrocloric (TT) v 20 ml nc, thm nc va 50 ml. Pha
long 5,0 ml dung dch ny thnh 250 ml bng nc. Ly 1,0 ml dung dch ny
thm 5 ml dung dch natri hydroxyd 1 M v 1 ml dung dch chun ni. Lc mnh
trong 1 pht, ly tm nu cn v ly lp trong pha trn.
iu kin sc k
Ct thu tinh (2 m 2 mm), c nhi bng kieselgur c silan ho v

ra bng acid (Gas Chrom Q hay Chrommosorb W/AW/DMCS l thch hp) c
tm 3% (kl/kl) phenyl methyl silicon lng (OV- 17 hay XE- 60 l thch hp).
Kh mang l nitrogen dng cho sc k kh, lu lng 30 ml/pht.
Detector ion ho ngn la.
Nhit : Ct 120oC, bung tim v detector 150oC.
Th tch tim: 1 l
Tro sulfat
Dng 1,0 g ch phm.
Nc
Khng c qu 2% (Ph lc 6.6).
Dng 0,300 g ch phm.
nh lng
Tin hnh theo php th nh lng trong chuyn lun amoxicilin trihydrat.
1 ml dung dch thu ngn (II) nitrat 0,02 M tng ng vi 6,988 mg
penicilin ton phn, tnh theo C16H19 N3O4S.
1 ml dung dch thu ngn (II) nitrat 0,02 M tng ng vi 6,988 mg sn
phm phn hu, tnh theo C16H19 N3O4S.
Bo qun
ng trong l kn, nhit di 30oC.
Ch phm
Vin nang, vin nn, hn dch, thuc tim, thuc bt
Tc dng v cng dng
Khng khun.
8-AMPICILIN TRIHYDRAT
Ampicillinum trihydratum
C16H19 N3O4S. 3H2O
P.t.l: 403,5
Ampicilin trihydrat l acid (6R) -6 -( - D - phenylglycylamino) penicilanic

trihydrat phi cha t 96,0 n 100,5% C16H19N3O4S, tnh theo ch phm khan.
Tnh cht
Bt kt tinh trng, khng mi hoc hu nh khng c mi.
Kh tan trong nc, thc t khng tan trong ethanol, cloroform, ether, du
bo. Tan trong dung dch acid long v dung dch hydroxyd kim.
nh tnh
Nhm I: A, D
Nhm II: B, C, D
ngoi ca ampicilin trihydrat chun. Cc php th B, C, D c tin hnh nh
m t chuyn lun "Ampicilin".
pH, trong ca dung dch, gc quay cc ring, kim loi nng, N, N dimethylanilin, tro sulfat, nh lng
Phi tun theo cc yu cu v tin hnh th nh m t trong chuyn lun
"Ampicilin".
Nc
12,0 n 15,0% (Ph lc 6.6).
Dng 0,100 g ch phm.
Bo qun
ng trong l kn, nhit di 30oC.
Ch phm
Vin nang, vin nn, thuc tim, thuc bt.
Tc dng v cng dng
Khng khun.
9-BARI SULFAT
Barii sulfas
BaSO4
P.t.l: 233,4
Tnh cht
Bt trng mn, nng, khng ln sn, khng mi. Thc t khng tan trong
nc v cc dung mi hu c, rt kh tan trong cc dung dch acid v hydroxyd
kim.
nh tnh
A. un si 0,2 g ch phm vi 5 ml dung dch natri carbonat 50% trong 5
pht. Thm 10 ml nc vo hn hp v lc. Acid ha dch lc bng dung dch
acid hydrocloric long (TT), thm tip vi git dung dch bari clorid 5% (TT) s
c ta trng xut hin.
B. Ra cn cn li trn phu php th A 3 ln, mi ln vi mt t nc.
Ha cn vi 5 ml dung dch acid hydrocloric long (TT) v lc, thm vo dch lc
vi git dung dch acid sulfuric 10% (TT), ta trng c to thnh. Ta ny

khng tan trong dung dch natri hydroxyd long (TT).
Gii hn acid - kim
un trn cch thu 5,0 g ch phm vi 20 ml nc khng c carbon dioxyd
(TT) trong 5 pht v lc. Thm 2 git dung dch xanh bromothymol (CT) vo 10
ml dung dch lc. Dung dch phi chuyn mu khi thm khng qu 0,5 ml dung
dch acid hydrocloric 0,01 N hoc 0,5 ml dung dch natri hydroxyd 0,01 N.
Mui bari ho tan
Dung dch S: un si 20,0 g ch phm vi mt hn hp gm 40 ml nc v
60 ml dung dch acid acetic 2 M (TT) trong 5 pht, lc v pha long dch lc
ngui bng nc n 100 ml, trn u.
Ly 10 ml dung dch S, thm 1 ml dung dch acid sulfuric 1 M (TT). Sau 1
gi dung dch ny khng c c hn hn hp gm 10 ml dung dch S v 1 ml
nc.
Kim loi nng
Pha long 7,5 ml dung dch S vi nc thnh 15 ml. Ly 12 ml dung dch
ny th theo phng php 1. Dng dung dch ch mu 1 phn triu chun b
mu i chiu.
Cht tan trong acid
Khng c qu 0,3 %.
Bc hi trn cch thu 25 ml dung dch S v sy cn 100 - 1050C n
khi lng khng i. Lng cn sau khi sy kh khng c nhiu hn 15 mg.
Phosphat
Thm mt hn hp gm 3 ml dung dch acid nitric 2 N (TT) v 7 ml nc

vo 1,0 g ch phm. un trn cch thu 5 pht, lc v pha long dch lc vi nc
thnh 10 ml. Thm 5 ml thuc th molybdovanadic (TT) v yn 5 pht. Dung
dch th khng c c mu vng m hn mu ca dung dch i chiu, tin
hnh cng lc, trong cng mt iu kin trn, dng 10 ml dung dch phosphat mu
5 phn triu.
Arsen
Trong bnh Kjeldahl nh, lc 0,5 g ch phm vi 2 ml acid nitric m c
(TT) v 30 ml nc. Cho vo c bnh mt phu thu tinh nh, t bnh v tr
nghing v un trn cch thu trong 2 gi. ngui v thm nc vo cho bng
mc th tch ban u. Lc, thu dch lc, ra cn 3 ln bng cch gn, mi ln vi 5
ml nc. Gp chung dch lc v nc ra, thm 1 ml acid sulfuric m c (TT),
bc hi n kh trn cch thy v un nng n khi khi trng bay ht. Ho tan
cn thu c vi 10 ml dung dch acid sulfuric 1 M (TT), thm 10 ml nc v tin
hnh th theo phng php A.
Hp cht sulfur d b oxy ho
Lc 1,0 g ch phm vi 5 ml nc trong 30 giy v lc. Thm vo dch lc
0,1 ml dung dch h tinh bt (CT), thm 0,1 g kali iodid (TT) v lc cho tan, thm
tip 1,0 ml dung dch kali iodat (3,6 mg/l) mi pha v 1 ml dung dch acid
hydrocloric 1 M, lc mnh. Dung dch th phi c mu m hn dung dch i
chiu pha song song, trong cng iu kin nh trn nhng khng c dung dch kali
iodat.
lng ng
Cho 5,0 g ch phm vo ng ong c dung tch 50 ml c chia 50 vch,
tng ng vi cao 14 cm k t y. Thm nc va 50 ml. Lc mnh hn
hp 5 pht v yn trong 15 pht. Cht th nghim khng c lng xung thp

hn di vch chia mc 15 ml.
Gim khi lng khi nung
Khng c qu 2,0 %.
Nung 1,000 g ch phm 6000C n khi lng khng i.
Bo qun
ng trong l nt kn
Tc dng v cng dng
Cht cn quang, dng trong X quang chn on.
Ch phm
Hn hp bari sulfat ung.
10-BERBERIN CLORID
Berberini chloridum
C20H18NO4Cl. 2H2O
P.t.l: 407,9
Berberin clorid l 5,6 dihydro - 8,9 - dimethoxy -1,3-dioxa - 6aazoniaindeno (5,6-a) anthracen clorid dihydrat, phi cha t 97,0 n 102,0%
C20H18NO4Cl, tnh theo ch phm lm kh.
Tnh cht
Tinh th hay bt kt tinh mu vng, khng mi, c v rt ng. Tan trong
nc nng, kh tan trong ethanol v nc, rt kh tan trong cloroform, khng tan
trong ether.
nh tnh
A. Ho tan 10 mg ch phm trong 20 ml nc nng, lm lnh v thm 1 ml

dung dch kali iodid 16,5%, ta mu vng xut hin.
B. Ho tan 0,1 g ch phm trong 20 ml nc bng cch un nng. Thm 0,5
ml acid nitric m c (TT), lm lnh v lc sau khi yn 10 pht. Ly 3 ml dch
lc v thm 1 ml dung dch bc nitrat 2% (TT), s xut hin ta trng. Ta ny
khng tan trong acid nitric long (TT), nhng tan c trong dung dch amoniac
(TT) qu tha.
C. Ho tan 5 mg ch phm trong 10 ml dung dch acid hydrocloric 10%
(TT). Lc u, thm mt t bt cloramin T (TT), ni tip xc gia hai lp cht
lng s c mu anh o.
D. Ph hp th t ngoi (Ph lc 3.1) ca dung dch ch phm 0,001%
trong nc di sng t 220 nm n 350 nm c 3 cc i hp th 227 nm, 263
nm v 345 nm.
trong ca dung dch
Ho tan 0,1 g ch phm trong 50 ml nc bng cch un nng trn cch
thu, dung dch phi trong (Ph lc 5.12).
Gii hn acid
Lc 0,1 g ch phm vi 30 ml nc khng c carbon dioxyd (TT), lc.
Thm vo dch lc 2 git dung dch phenolphtalein (CT) v 0,10 ml dung dch
natri hydroxyd 0,1 N, mu vng phi chuyn sang vng cam n mu .
Sulfat
Khng c qu 0,048%.
Dung dch th: Lc 1,0 g ch phm vi 48 ml nc v 2 ml dung dch acid
hydroclorid 10% (TT) trong 1 pht, lc. B 5 ml dch lc u, ly 25 ml dch lc
tip theo v thm nc n 50 ml trong ng Nessler.
Dung dch i chiu: Ly 0,50 ml dung dch acid sulfuric 0,01 N, thm 1
ml dung dch acid hydrocloric 10% (TT), thm 5-10 git dung dch xanh
bromophenol 0,1% trong ethanol 50% v thm nc n 50 ml trong ng Nessler.
Cho vo mi ng 2 ml dung dch bari clorid 0,5 M (TT), lc k, yn 10
pht. So snh c to thnh trong ng th v ng i chiu, dung dch th
khng c c hn dung dch i chiu.
Kim loi nng
Tro sulfat
Dng 1,0 g ch phm.
Mt khi lng do lm kh
(1,000 g; 100oC; 5 gi).
Alcaloid khc
Phng php sc k lp mng (Ph lc 4.4).
Bn mng: Cn 10 g silicagel G cho vo ci, nghin mn, thm 2 ml dung
dch natri carboxymethylcelulose 0,1% trong nc, trn u thnh hn dch ng
nht, trng bn mng c dy 0,25 mm v hot ho 110oC trong 1 gi.
Dung mi khai trin 1: Ethyl acetat - cloroform: methanol - diethylamin (8:
2: 2: 1). Dung mi khai trin 2: n-Butanol - acid acetic khan - nc (7: 1: 2).
Dung dch th: Ho tan 2 mg ch phm trong 1 ml ethanol 96% (TT).
Dung dch i chiu 1: Ho tan 0,1 mg jatrorrhizin chun trong 1 ml

ethanol 96% (TT).
Dung dch i chiu 2: Ho tan 0,1 mg palmatin chun trong 1 ml ethanol
96% (TT).
Cch tin hnh:
Jatrorrhizin:
Chm ring bit ln bn mng 3 l dung dch th v dung dch i chiu 1.
Trin khai bn mng trong dung mi khai trin 1 n khi dung mi i c
khong 15 cm, ly ra kh ngoi khng kh. Phun thuc th Dragendorff hoc
soi di nh sng t ngoi bc sng 365 nm. Vt jatrorrhizin xut hin trn sc
k ca dung dch th khng c m mu hn vt jatrorrhizin tng ng ca
dung dch i chiu 1.
Palmatin:
Chm ring bit ln bn mng khc 15 l dung dch th v 6 l dung dch i
chiu 2. Trin khai bn mng trong dung mi khai trin 2 n khi dung mi i
c khong 15 cm, ly ra kh ngoi khng kh. Phun thuc th Dragendorff
hoc soi di nh sng t ngoi bc sng 365 nm. Vt palmatin xut hin trn
sc k ca dung dch th khng c m mu hn vt palmatin tng ng ca
dung dch i chiu 2.
nh lng
Dung dch th: Cn 0,200 g ch phm v ho tan trong 200 ml nc bng
cch un nng. Sau lm lnh v thm nc n 1000 ml. Ly 10 ml dung dch
ny pha long vi nc n 100 ml.
Dung dch chun: Cn chnh xc khong 0,200 g kali dicromat thuc th
chun sy kh 110oC trong 4 gi, ho tan trong nc. Thm 10 ml dung dch
acid sulfuric 1 N v thm nc va 1000 ml.
o hp th (Ph lc 3.1) At v As ca dung dch th v dung dch chun

bc sng 421 nm
Lng ( mg) ca C20H18NO4Cl c tnh bng cng thc sau:
a: Khi lng ( mg) kali dicromat.

Bo qun
ng gi kn, ch thong mt, trnh nh sng.
Ch phm
Vin nn.
Tc dng v cng dng
Khng khun. Tr tiu chy, l amip, l trc khun.
11-BT TALC
Talcum
Bt Talc l magnesi silicat hydrat t nhin c la chn v lm thnh
bt mn, c thnh phn gn ng: 4SiO2. 3MgO. H2O, i khi cha mt lng
nh nhm silicat.
Tnh cht
Bt rt mn, trng hoc gn nh trng, khng mi, khng dnh v trn tay.
Hu nh khng tan trong nc, trong cc acid long, hay kim long v cc
dung mi khc.
nh tnh
A. un chy 0,5 g ch phm vi 1 g kali nitrat (TT) v 3 g natri carbonat
khan (TT) trong mt chn kim loi, thm 20 ml nc nng trn u v lc. Ra
cn cn li trn giy lc bng 50 ml nc. Trn cn vi hn hp gm 0,5 ml acid
hydrocloric m c (TT) v 5 ml nc, lc. Thm vo dch lc 1 ml dung dch

amoniac 9 M v 1 ml dung dch amoni clorid 10% v lc. Thm vo dch lc 1 ml
dung dch dinatri hydrophosphat 12% (TT) kt ta trng to thnh.
B. Trn 0,1 g ch phm vi 10 mg natri fluorid (TT) v vi git acid
sulfuric (TT) trong mt chn ch hoc platin, tri thnh lp mng. y chn bng
mt ming plastic trong sut, mt trong ca n c treo mt git nc, un nh
trong thi gian ngn, mt vng mu trng c to thnh xung quanh git nc.
Gii hn acid - kim
Dung dch S: un 20 g ch phm vi 100 ml nc trong 30 pht, va un
va thm nc cho lun lun 100 ml, lc.
Ly 25 ml dung dch S, thm 0,5 ml dung dch xanh bromothymol (CT),
dung dch phi c mu xanh, mu ny phi chuyn sang mu vng khi thm khng
qu 0,3 ml dung dch acid hydrocloric 0,1 N.
Cht tan trong nc
Khng c qu 0,1%.
Lm bay hi trn cch thu 25 ml dung dch S n kh v sy 100 105oC trong 1 gi. Khi lng cn thu c khng c qu 5 mg.
Carbonat
Cn 1,000 g ch phm, thm 20 ml dung dch acid hydrocloric long (TT),
khng c c hin tng si bt kh.
Cht tan trong acid
Khng c qu 1%.
un nng hn hp ca php th gii hn carbonat 50oC trong 15 pht,
va un va khuy u. Lm ngui, thm nc cho bng th tch ban u. Lc
hoc ly tm nu cn c dung dch trong. Ly 10 ml dch lc, bc hi ti kh
v nung ti khi lng khng i 800oC.
Arsen
Ly 2 ml dch lc trong mc "Cht tan trong acid" th theo phng php A.
Sulfid
Cho vo mt bnh nn 0,60 g ch phm, thm 100 ml dung dch acid
hydrocloric long (TT) v y bnh bng giy tm ch acetat (TT). un hn hp
si nh trong 1 gi, giy khng c c mu nu.
St
Khng c qu 0,025% (Ph lc 7.4.11)
Ly 0,4 g ch phm, thm 100 ml dung dch acid sulfuric 2 M (TT). un
hn hp si trong 1 gi, va un va thm nc duy tr mc th tch ban u.
ngui, lc. Ly 10 ml dch lc tin hnh th.
mn
Ry 10 g ch phm c sy trc 100 - 105oC qua ry c kch thc
l mt ry 0,125 mm, ch phm khng c li cn.
Clorid
Khng c qu 0,014% (Ph lc 7.4.5).
To mt hn dch gm 0,7 g ch phm trong 10 ml nc v thm va 20
ml bng dung dch acid nitric 2 M (TT), lc 15 pht, lc, 10 ml dch lc c pha
long n 15 ml vi nc v tin hnh th.
Mt khi lng do lm kh.
Khng c qu 1% (Ph lc 5.16)
(1,000 g; 180oC; 1 gi).
Cht hu c
Cn thu c trong php th "Mt khi lng do lm kh" khng c c

mu vng nht hay xm nht.
nhim khun
Tng s vi khun hiu kh sng li c khng c qu 1000 trong 1 gam
ch phm, xc nh bng phng php a thch (Ph lc 10.7)
Bo qun
ng trong bao b kn.
Cng dng
Lm t dc.
Ch phm
Bt Talc mn.
12-CC ETHANOL LONG
Dilutum ethanolum
Cc ethanol long dc dng c cha 90, 80, 70, 60, 50, 45, 25 v 20%
(tt/tt) C2H5OH. Cc ethanol long ny c iu ch theo m t di y, iu
chnh th tch cui cng c thc hin nhit nh nhau (20oC) cng ging
nh nhit c o i vi ethanol 96%.
Ch : Hn hp ethanol v nc c km theo s gim th tch v s tng
nhit .
nh tnh, gii hn acid - kim, trong ca dung dch, aldehyd, cht
khng bay hi v clorid.
Phi tun theo cc yu cu v phng php th nh quy nh trong
chuyn lun ethanol 96%.
Kim loi nng

Ly chnh xc 20 ml ch phm cho vo cc v bc hi ht ethanol trn cch
thu. Pha long phn cn li thnh 20 ml bng nc. Ly 12 ml dung dch ny tin
mu i chiu.
Ethanol 90%
Alcol 90%.
Pha long 934 ml ethanol 96% thnh 1000 ml bng nc.
Hm lng ethanol t 89,6 n 90,5% (tt/tt).
T trng biu kin (Ph lc 5.15): T 826,4 n 829,4 kg m-3.
Ethanol 80%
Alcol 80%.
Ethanol 70%
Alcol 70%.
Hm lng ethanol t 69,5 n 70,4 (tt/tt).
Ethanol 60%
Alcol 60%.

Ethanol 50%
Alcol 50%.
Hm lng ethanol t 49,6% n 50,2% (tt/tt).
Ethanol 45%
Alcol 45%.
Ethanol 25%
Alcol 25%.
Ethanol 20%
Alcol 20%.
13-CAFEIN
Caffeinum
C8H10 N4O2 (khan)
P.t.l: 194,2
C8H10 N4O2. H2O (monohydrat)
P.t.l: 212,2
Cafein l 1, 3, 7 trimethyl - 3,7 dihydro - 1 H purin - 2, 6 dion, phi cha t

98,5 n 101,5% C8H10 N4O2, tnh theo ch phm lm kh.
Tnh cht
Tinh th trng, mn, hay bt kt tinh trng. Vn nt ngoi khng kh kh,
un nng 100oC cafein s mt nc v thng hoa khong 200oC. Dung dch
cafein c phn ng trung tnh vi giy qu. D tan trong nc si, cloroform, hi
tan trong nc, kh tan trong ethanol v ether, tan trong cc dung dch acid v
trong cc dung dch m c ca benzoat hay salicylat kim.
nh tnh
Nhm I: A, B, E
Nhm II: A, C, D, E A. im chy: 234 - 239oC (Ph lc 5.19).
Xc nh trn ch phm lm kh.
B. Ph hng ngoi (Ph lc 3.1) phi ph hp vi ph hng ngoi ca
cafein chun. Xc nh trn ch phm lm kh.
C. Cho 0,05 ml dung dch iod - iodid (TT) vo 2 ml dung dch bo ho
cafein. Dung dch vn trong. Thm 0,1 ml dung dch acid hydrocloric long (TT).
C ta nu xut hin, ta ny tan khi trung ho bng dung dch natri hydroxyd 2
M.
D. Cho phn ng ca nhm xanthin (Ph lc 7.1).
E. Ch phm p ng php th mt khi lng do lm kh.

Dung dch S: Ho tan 0,5 g ch phm trong 50 ml nc khng c carbon
dioxyd (TT) bng cch un nng, lm ngui v sau thm cng dung mi va
50 ml.
php 2).
Gii hn acid
Thm 0,05 ml xanh bromothymol (CT) vo 10 ml dung dch S. Dung dch
c mu xanh lc hay vng.
Mu ca dung dch s chuyn thnh xanh lam khi thm khng qu 0,2 ml
dung dch natri hydroxyd 0,01 M.
Sulfat
Khng c qu 0,05%. (Ph lc 7.4.12).
Ly 15 ml dung dch S tin hnh th. chun b mu i chiu ly 7,5 ml
dung dch sulfat mu 10 phn triu v thm nc va 15 ml.
Kim loi nng
Mt khi lng do lm kh
T 5,0 - 9,0% (i vi cafein monohydrat) v khng c qu 0,5% (i
vi cafein khan) (Ph lc 5.16).
(1,000 g; 100oC - 105oC; 1 gi).
Tp cht lin quan

Tin hnh bng phng php sc k lp mng (Ph lc 4.4).
Bn mng: Silicagel GF254
30: 30: 40).
Dung dch th: Ho tan 0,2 g ch phm trong hn hp dung mi methanol cloroform (4:6) v pha long n 10 ml vi cng hn hp dung mi.
Dung dch i chiu: Pha long 0,5 ml dung dch th thnh 100 ml vi hn
hp dung mi trn.
Trin khai bn mng ti khi dung mi i c 15 cm. kh bn mng ngoi
khng kh. Quan st di nh sng t ngoi bc sng 254 nm. Bt c vt no
ngoi vt chnh trn sc k ca dung dch th khng c c mu m hn vt
trn sc k ca dung dch i chiu.
Tro sulfat
Khng c qu 0,1% (Ph lc 7.7, phng php 2)
Dng 1,0 g ch phm.
nh lng
Cn chnh xc khong 150 mg ch phm lm kh. Ho tan trong 15 ml
anhydrid acetic (TT) v 20 ml benzen (TT). Cho thm vi git dung dch tm tinh
th (CT). Chun bng dung dch acid percloric 0,1 N n khi dung dch chuyn
sang mu vng. C th xc nh im kt thc bng phng php chun o
in th (Ph lc 6.12). 1 ml dung dch acid percloric 0,1 N tng ng vi
19,42 mg C8H10N4O2.
Bo qun
ng trong l kn.
Tc dng v cng dng
Kch thch thn kinh trung ng, li tiu.
14-CALCI CARBONAT
Calcii carbonas
CaCO3
P.t.l:100,1
Calci carbonat phi cha t 98,5 n 100,5% CaCO3, tnh theo ch phm
lm kh.
Tnh cht
Bt mn trng, khng mi.
Thc t khng tan trong nc, ethanol 96% v ether. Tan trong cc dung
dch acid long km theo si bt kh carbon dioxyd.
nh tnh
A. Thm 5 ml acid acetic long (TT) vo 0,1 g ch phm, phi c si bt
kh carbon dioxyd. Kh thot ra c dn vo dung dch calci hydroxyd (TT) s
xut hin kt ta trng, ta ny tan trong acid hydrocloric 7 M (TT) qu tha.
B. yn dung dch trn cho n khi si ht bt, thm 2-3 git dung dch
amoni oxalat 4% (TT), phi xut hin ta trng, ta ny khng tan trong dung dch
acid acetic 6 M tan trong dung dch acid hydrocloric long (TT).
Cht khng tan trong acid acetic
Khng c qu 0,2%.
Ho tan 5,0 g ch phm trong 80 ml dung dch acid acetic 2 M (TT), sau
khi si ht bt, un si dung dch trong 2 pht. ngui v pha long thnh 100
ml vi dung dch acid acetic 2 M (TT), lc qua phu thu tinh xp, gi li dch lc
(dung dch S) tin hnh cc th nghim sau. Ra cn trn phu 4 ln, mi ln
vi 5 ml nc nng v sy 100 - 1050C trong 1 gi, khi lng cn cn li

khng c nhiu hn 10 mg.
Arsen
Khng c qu 4 phn triu. (Ph lc 7.4.2).
Ly 5,0 ml dung dch S v tin hnh th theo phng php A.
Kim loi nng
Ly 12 ml dung dch S v tin hnh th theo phng php 1. Dng dung
dch ch mu 1 phn triu chun b mu i chiu.
Clorid
Khng c qu 0,033% (Ph lc 7.4.5).
Ly 3 ml dung dch S, pha long vi nc va 15 ml v tin hnh th.
Sulfat
Khng c qu 0,25% (Ph lc 7.4.12).
Bari
Thm 10 ml dung dch calci sulfat (TT) vo 10 ml dung dch S. Sau 15 pht
dung dch th khng c c hn mt hn hp gm 10 ml dung dch S v 10 ml
nc.
St
Khng c qu 0,02% (Ph lc 7.4.11).
Ho tan 50 mg ch phm trong 5 ml dung dch acid hydrocloric long (TT)
v pha long vi nc thnh 10 ml tin hnh th.
Magnesi v cc kim loi kim
Khng c qu 1,5% (Ph lc 7.4.14).

Ho tan 1,0 g ch phm trong 12 ml dung dch acid hydrocloric long (TT),
un si trong 2 pht v thm 20 ml nc, 1 g amoni clorid (TT) v 0,1 ml dung
dch methyl (CT). Thm tng git dung dch amoniac 10% (TT) cho n khi
dung dch chuyn mu v sau thm tip 2,0 ml dung dch amoniac 10% (TT).
un n si v thm 50 ml dung dch amoni oxalat 4% (TT) nng. yn 4 gi,
sau pha long thnh 100 ml vi nc v lc. Thm 0,25 ml acid sulfuric m
c (TT) vo 50 ml dch lc v un cch thu cho n kh. Nung cn n khi
lng khng i 600oC. Lng cn cn li khng c nhiu hn 7,5 mg.
Mt khi lng do lm kh
Khng c qu 2,0%. (Ph lc 5.16).
(1,000 g; 2000C).
nh lng
Ho tan 0,150 g ch phm trong hn hp gm 3 ml dung dch acid
hydrocloric long (TT) v 20 ml nc. un si 2 pht, ngui v pha long ti
50 ml bng nc. Tin hnh chun theo phng php nh lng calci bng
chun complexon (Ph lc 6.11). 1 ml dung dch natri edetat 0,1 M tng
ng vi 10,01 mg CaCO3.
Bo qun
ng trong chai l nt kn, ni kh ro.
Tc dng v cng dng
Khng acid, b sung cht in gii.
Ch phm
Vin nn calci carbonat v vitamin D; Vin nhai calci carbonat
Tng k
Vi acid.
15-CALCI GLUCONAT
Calcii gluconas
C12H22CaO14. H2O
P.t.l: 448,4
Calci gluconat l calci D-gluconat monohydrat, phi cha t 98,5 n

102,0% C12H22CaO14. H2O.
Tnh cht, nh tnh, tp cht hu c v acid boric, sacarose v ng kh,
nh lng
Tin hnh theo chuyn lun Calci gluconat pha thuc tim.
Dung dch S: Ho tan 1,0 g ch phm trong nc c un nng n
60oC v pha long n 50 ml bng cng dung mi.
60oC mu ca dung dch S khng c m hn mu mu V6 (Ph lc
5.17, phng php 2) v sau khi ngui, dung dch khng c c hn c
mu S2 (Ph lc 5.12).
Clorid
Khng c qu 0,02% (Ph lc 7.4.5).
Ly 12,5 ml dung dch S pha long thnh 15 ml v tin hnh th.
Sulfat
Khng c qu 0,01% (Ph lc 7.4.12).
Ho tan 10,0 g ch phm trong hn hp gm 10 ml acid acetic (TT) v 90
ml nc bng cch un nng. Ly 15 ml dung dch ny tin hnh th.
Kim loi nng
Ly 2,0 g ch phm tin hnh theo phng php 4. un nng dn dn v

cn thn ch phm cho ti khi chuyn hon ton thnh khi mu trng v sau
nung.
Dng 2 ml dung dch ch mu 10 phn triu chun b mu i chiu.
Magnesi v cc kim loi kim
Khng c qu 0,4%.
Ho tan 1,00 g ch phm trong 100 ml nc ang si, thm 10 ml dung
dch amoni clorid 10% (TT), 1 ml amoniac (TT) v thm tng git 50 ml dung
dch amoni oxalat 4% (TT) nng. yn 4 gi, pha long thnh 200 ml bng nc
v lc. Bc hi 100 ml dch lc n kh v nung. Cn thu c khng c qu 2
mg.
nhim khun
Tng s vi khun hiu kh sng li c khng c qu 1000 trn 1 g ch
phm, xc nh bng phng php a thch (Ph lc 10.7).
Bo qun
Trong bao b nt kn.
Tc dng v cng dng
iu tr bnh thiu calci.
Dng bo ch
Vin calci gluconat, vin si bt calci gluconat.
16- CAMPHOR
Camphora
Long no
v cht ng phn i nh
C10H16O
P.t.l: 152,2
Camphor l (1RS,4SR) - 1,7,7 - trimethylbicyclo - [2.2.1] heptan - 2 - on,

uc chit t tinh du ca cy Long no - Cinnamomum camphora (Linn.) Nees et
Eberm, h Lauraceae (camphor thin nhin, hu tuyn) hoc c iu ch bng
tng hp ho hc (camphor tng hp, racemic hoc t tuyn).
Tnh cht
Bt kt tinh trng hoc phin, khi kt tinh khng mu. D nghin mn vi
mt t ethanol, cloroform hay ether. Mi thm mnh, c trng; v lc u nng
sau mt lnh v d chu; d thng hoa ngay nhit thng. un nng cn thn,
ch phm thng hoa hon ton v khng b carbon ho; chy cho khi en v ngn
la sng. Kh tan trong nc, rt tan trong cloroform, trong ethanol 96%, ether,
ether du ho, d tan trong du bo v tinh du.
nh tnh
Nhm I: A, C.
Nhm II: A, B, D.
Dung dch S: Ho tan 2,50 g ch phm trong 10 ml ethanol 96% (TT) v
thm va 25,0 ml vi cng dung mi.
A. Gc quay cc ring. Xc nh trn dung dch S (Ph lc 5.13).
Camphor thin nhin (loi hu tuyn): T +39 n +44o.
Camphor tng hp (loi racemic): T -1,5 n +1,5o; (loi t tuyn): T 39 n -44o.

B. im chy: Camphor thin nhin chy 174 n 181oC; Camphor tng
hp chy 172 n 180oC (Ph lc 5.19).
C. Ph hng ngoi ca ch phm (Ph lc 3.2) ph hp vi ph hng ngoi
i chiu ca camphor hoc ph hng ngoi ca camphor chun. Tin hnh th
ch phm di dng bt nho vi parafin lng (TT).
D. Pha long 0,5 ml dung dch S vi ethanol 96% (TT) thnh 20 ml. o
ph hp th t ngoi (Ph lc 3.1) trong khong bc sng 230 - 350 nm. Dung
dch c mt cc i hp th 289 nm v hp th 289 nm khong 0,53.
php 2).
Gii hn acid, kim
Thm 0,1 ml dung dch phenolphtalein (CT) vo 10 ml dung dch S, dung
dch phi khng mu. Mu s chuyn sang hng, khi thm khng qu 0,2 ml dung
dch natri hydroxyd 0,1 M.
Halogen
Khng c qu 0,01% (Ph lc 7.4.5).
Ho tan 1,0 g ch phm vi 10 ml 2-propanol (TT) trong bnh chng ct.
Thm 1,5 ml dung dch natri hydroxyd 2 M (TT), 50 mg hp kim nhm-nickel
(TT). un cch thu n khi 2-propanol bay hi hon ton. ngui v thm 5 ml
nc. Khuy u v lc qua giy lc t c ra bng nc n khi ht
clorid. Pha long dch lc n 10,0 ml vi nc. Thm vo 5,0 ml dung dch trn
tng git acid niric (TT) n khi ta to thnh tan tr li v pha long n 15 ml
vi nc. Dung dch thu c p ng php th gii hn clorid.
Nc
Ho tan 1 g ch phm trong 10 ml ether du ho (TT). Dung dch phi
trong (Ph lc 5.12).
Cn sau khi bc hi
Khng c qu 0,05%.
Bc hi 2,0 g ch phm trn cch thu v sy kh 100 n 105oC trong 1
gi. Cn cn li khng c qu 1 mg.
Bo qun
Trong chai l nt kn, ni kh mt.
Cc dng ch phm
Cn long no, cn long no - opi, nc long no m c, du xoa long
no.
Tc dng v cng dng
Thuc kch thch da, gim au, chng nga.
Ghi ch
Tng k: To hn hp chy lng (hn hp lng, c st, trong sut) vi
phenol, menthol, thymol, salol, naphthol, resorcin, pyrocatechol, pyrogalol, acid
salicylic, phenylsalicylat, cloralhydrat, antipirin,..
17-CLORAL HYDRAT
Chlorali hydras
C2H3Cl3O2 P.t.l: 165,4
Cloral hydrat l 2,2,2-tricloroethan-1,1-diol, phi cha t 98,5 n 101,0%

C2H3Cl3O2.
Tnh cht
Tinh th trong sut, khng mu, mi c bit, v cay. Rt tan trong nc,
tan trong cloroform, ethanol 96% v ether.
nh tnh
Dung dch S: Ho tan 2,5 g ch phm trong nc khng c carbon dioxyd
(TT) va 25 ml.
A. Ly 10 ml dung dch S, thm 2 ml dung dch natri hydroxyd 2 M (TT),
hn hp tr nn c v khi un nng c mi cloroform.
B. Ly 1 ml dung dch S, thm 2 ml dung dch natri sulfit (TT) mu vng
xut hin v nhanh chng tr nn nu . yn trong mt thi gian ngn ta
c th xut hin.
php 2).
pH
pH ca dung dch S t 3,5 n 5,5 (Ph lc 5.9).
Kim loi nng
Pha long 7,5 ml dung dch S vi nc ti 15 ml. Ly 12 ml tin hnh th
theo phng php 1. Dng dung dch ch mu 1 phn triu chun b mu i
chiu.
Clorid
Khng c qu 0,01% (Ph lc 7.4.5).
Ly 5 ml dung dch S, pha long vi nc ti 15 ml v tin hnh th.

Cloral alcolat
un nng 1,0 g ch phm vi 10 ml dung dch natri hydroxyd 2 M (TT),
lc v thm tng git dung dch iod 0,1 N cho ti khi xut hin mu vng. yn
1 gi, khng c xut hin ta.
Cn khng bay hi
Khng c qu 0,1%.
Bc hi 2,000 g ch phm trn cch thy.
Khi lng cn khng c qu 2 mg.
nh lng
Ho tan 4,000 g ch phm trong 10 ml nc v thm 40,0 ml dung dch
natri hydroxyd 1 N. yn chnh xc 2 pht v chun vi dung dch acid
sulfuric 1 N, dng 0,1 ml dung dch phenolphtalein (CT) lm ch th. Chun
dung dch trung ho vi dung dch bc nitrat 0,1 N, dng 0,2 ml dung dch kali
cromat (CT) lm ch th. Tnh s ml dung dch natri hydroxyd 1 N dng bng
cch ly th tch dung dch natri hydroxyd 1 N cho vo lc bt u chun tr i
th tch dung dch acid sulfuric 1 N dng trong ln chun u tin v hai
phn mi lm th tch dung dch bc nitrat 0,1 N dng trong ln chun th
hai.
1 ml dung dch natri hydroxyd 1 N tng ng vi 165,4 mg
C2H3Cl3O2.
Bo qun
Thuc c bng B. trong l kn.
18- CLOROFORM
Chloroformium
Tricloromethan
CHCl3
P.t.l: 119,38
Tnh cht
Cht lng khng mu, trong sut, d bay hi v c mi c bit. Kh tan
trong nc, trn ln c vi ethanol, ether, cc cht du v a s cc dung mi
hu c theo mi t l.
nh tnh
C th chn mt trong hai nhm nh tnh sau: Nhm I: B, C .
Nhm II: A. A. Ph hng ngoi (Ph lc 3.1) ca ch phm c xc nh
sau khi ra ch phm vi nc v lm khan vi natri sulfat khan (TT) phi ph
hp vi ph hng ngoi i chiu ca cloroform.
B. un vi git ch phm vi vi git anilin (TT) v 1-2 ml dung dch natri
hydroxyd 20% (TT). Hi bc ln mi c bit ca phenylisocyanid.
C. un si 2 - 3 git ch phm vi 2 ml dung dch natri hydroxyd 10%
(TT) trong 1 pht. ngui. Acid ho dung dch ny bng dung dch acid nitric
10% (TT). Thm vi git dung dch bc nitrat 5% (TT). Xut hin ta trng vn;
ta tan trong dung dch amoniac (TT).
Khong chng ct
Khng c qu 5% (tt/tt) c ct di 600C v phn cn li c ct
nhit 60 - 620C (Ph lc 5.20).
T trng
1,474 n 1,479 (Ph lc 5.15).
Cht khng bay hi
Khng c qu 0,004%.
Ly 50,0 ml ch phm cho vo cc thu tinh cn b sn. Bc hi cch

thu n kh. Sy cn 1050C trong 1 gi, khi lng cn khng c qu 2 mg.
Gii hn acid - kim
Dung dch S: Lc 10,0 ml ch phm vi 20,0 ml nc va un si ngui
trong 3 pht. phn lp, ly lp nc.
Ly 5,0 ml dung dch S, thm 0,1 ml dung dch qu trung tnh (CT). Mu
ca dung dch ny phi bng mu ca dung dch gm 5,0 ml nc va un si
ngui v 0,1 ml dung dch qu trung tnh (CT).
Clorid
Ly 5,0 ml dung dch S, thm 5,0 ml nc v 0,2 ml dung dch bc nitrat
5% (TT). Dung dch phi trong (Ph lc 5.12).
Clor t do
Ly 10,0 ml dung dch S, thm 5 git dung dch h tinh bt (CT) v 3 git
dung dch kali iodid 10% (TT). Dung dch khng c c mu xanh.
Aldehyd
Lc 5,0 ml ch phm vi 5 ml nc v 0,2 ml dung dch kali
tetraiodomercurat kim (TT), trong ng nghim c nt mi. ch ti 15 pht. C
2 lp khng c c mu, hoc ch c c mu hi ng vng.
Sn phm phn hu (tin hnh di nh sng du).
Ly 20,0 ml ch phm cho vo bnh c nt mi trng trc bng acid
sulfuric m c (TT), thm 15,0 ml acid sulfuric m c (TT) v 0,2 ml dung
dch formaldehyd (TT). 30 pht, thnh thong lc, sau yn 30 pht na.
Lp acid ch hi c mu.
Cht hu c l
Lc 20,0 ml ch phm trong 5 pht vi 10,0 ml acid sulfuric m c (TT)

trong bnh c nt mi trng trc bng acid sulfuric m c (TT). ch ti
30 pht. Lp acid cng nh lp cloroform phi khng c mu. Gi lp cloroform
th hp cht clor l.
Cho 5,0 ml nc vo mt ng nghim, t vo nc . Nh tng git 2,0
ml lp acid, dung dch vn phi trong, khng mu v khng c mi l. Thm 10,0
ml nc v 0,2 ml dung dch bc nitrat 5% (TT). Dung dch khng c c.
Hp cht clor l
Lc 15 ml lp cloroform trn vi 30,0 ml nc trong bnh c nt mi
trong 3 pht. phn lp. Cho vo lp nc 0,2 ml dung dch bc nitrat 5% (TT).
ch ti 5 pht. Dung dch khng c c.
Bo qun
ng trong l thu tinh mu vng nt kn. ch mt trnh nh sng.
19-CLOROQUIN PHOSPHAT
Chloroquini phosphas
Cloroquin diphosphat, Nivaquin phosphat, Aralen
C18H26ClN3. 2H3PO4
P.t.l: 515,9
Cloroquin
phosphat
(RS)
-4-
(7-cloro-4-quinolylamino)
pentyldiethylamin diphosphat, phi cha t 98,5 n 101,0% C18H26ClN3.

2H3PO4, tnh theo ch phm khan.
Tnh cht
Bt kt tinh trng hoc gn nh trng, khng mi, v ng, d bin mu khi

ngoi nh sng, d ht m.
D tan trong nc, rt kh tan trong cloroform, ethanol 96%, ether v
methanol. Tn ti 2 dng, mt dng chy khong 195oC v dng khc chy
khong 218oC.
nh tnh
Nhm I: A, D.
Nhm II: B, C, D.
A. Ho tan 0,1 g ch phm trong 10 ml nc, thm 2 ml dung dch natri
hydroxyd 2 M (TT), chit 2 ln, mi ln vi 10 ml cloroform (TT). Ra dch
cloroform vi nc, lm khan bng natri sulfat khan (TT) lm bay hi n kh v
ho cn trong 2 ml cloroform (TT). Ph hng ngoi (Ph lc 3.2) ca dung dch
ny phi ging ph hng ngoi ca dung dch thu c t 80 mg cloroquin sulfat
chun vi cch chun b tng t.
B. Ph hp th t ngoi (Ph lc 3.1) ca dung dch ch phm 0,001%
bc sng t 210 n 370 nm cho cc cc i hp th ln lt 220, 235, 256,
329 v 342 nm. A (1%, 1 cm) tng ng ln lt l 600 n 660; 350 n 390;
300 n 330; 325 n 355 v 360 n 390.
C. Ho tan 25 mg ch phm trong 20 ml nc, thm 5 ml dung dch bo
ho acid picric (TT) s xut hin ta vng. Lc v ra ta ln lt vi nc,
ethanol 96% (TT) v ether (TT). Ta ny c im chy t 206 n 209oC (Ph lc
5.19).
D. Ho tan 0,1 g ch phm trong 10 ml nc, thm 2 ml dung dch natri
hydroxyd 2 M (TT), chit 2 ln, mi ln vi 10 ml cloroform (TT). Lp nc c
acid ho bng acid nitric (TT) cho phn ng ca phosphat (Ph lc 7.1).
pH
pH ca dung dch ch phm 10% trong nc khng c carbon dioxyd (TT)
phi t 3,8 n 4,3 (Ph lc 5.9).
Dung dch ch phm 10% trong nc khng c carbon dioxyd (TT) phi
trong (Ph lc 5.12) v mu khng c m hn mu ca mu mu NV5 hay
LV5 (Ph lc 5.17, phng php 2).
Kim loi nng
Ho tan 2,0 g ch phm trong 10 ml nc, thm 5 ml dung dch amoniac
13,5 M (TT) v chit bng 40 ml ether (TT). Lc, ly lp nc, trung ho dch lc
bng acid acetic bng (TT), un nng trn cch thu loi ht ether, lm lnh v
pha long vi nc va 20 ml. Ly 12 ml dung dch ny tin hnh theo phng
php 1. Dng dung dch mu ch 2 phn triu chun b mu i chiu.
Tp cht lin quan
Tin hnh phng php sc k lp mng (Ph lc 4.4).
Bn mng: Silicagel GF254.
Dung mi khai trin: Cloroform - cyclohexan - diethylamin (50: 40: 10).
Dung dch th: 5,0% ch phm trong nc.
Dung dch i chiu (1): 0,050% ch phm trong nc.
Dung dch i chiu (2): 0,025% ch phm trong nc.
Trin khai bn mng n khi dung mi i c khong 12 cm. Sau khi trin khai,
ly bn mng ra kh ngoi khng kh v quan st di nh sng t ngoi
bc sng 254 nm. Bt c vt ph no trn sc k thu c t dung dch th
cng khng c m mu hn vt trn sc k thu c t dung dch i chiu

(1) v ch c c mt vt nh vy m mu hn vt trn sc k thu c t
dung dch i chiu (2).
Nc
Khng c qu 2,0% (Ph lc 6.6).
Ly 1,000 g ch phm em th.
nh lng
Cn 0,200 g ch phm, ho tan trong 50 ml acid acetic khan (TT), thm 2
git dung dch tm tinh th (CT). nh lng bng dung dch acid percloric 0,1 N
cho ti khi dung dch chuyn sang mu xanh lc hoc c th xc nh im kt
thc bng phng php chun o in th (Ph lc 6.12).
1 ml dung dch acid percloric 0,1 N tng ng vi 25,79 mg
C18H26ClN3. 2H3PO4.
Bo qun
Thuc c bng B. Trong l kn, trnh nh sng v khng kh.
Ch phm
Thuc tim, vin bao ng, vin nn.
Tc dng v cng dng
Tr st rt.
20-CODEIN
Codeinum monohydricum
Codein monohydrat
C18H21NO3. H2O P.t.l: 317,4
Codein l (5R, 6S) -4,5-epoxy-3-methoxy-N-methylmorphin-7-en-6-ol

monohydrat, phi cha t 99,0 n 101,0% C18H21NO3, tnh theo ch phm
lm kh.
Tnh cht
Tinh th khng mu hoc bt kt tinh trng, khng mi.
D tan trong cloroform v ethanol 96%, tan trong nc si v trong ether,
kh tan trong nc.
nh tnh
C th chn mt trong 2 nhm nh tnh sau:
Nhm I: A, C.
Nhm II: A, B, D, E.
A. im chy: 155 n 159oC (Ph lc 5.19).
B. Thm vo 2,0 ml dung dch S 50 ml nc, sau 10 ml dung dch natri
hydroxyd 1 M v pha long vi nc va 100,0 ml. o ph t ngoi (Ph lc
3.1) ca dung dch trn di sng t 250 n 350 nm. Dung dch ch c duy nht
mt cc i hp th 284 nm. hp th ring cc i khong 50, tnh theo
ch phm lm kh.
C. Ph hng ngoi (Ph lc 3.2) ca ch phm phi ph hp vi ph hng
ngoi i chiu ca codein. Php th c tin hnh trn ch phm lm kh.
D. Thm 1 ml acid sulfuric (TT) v 0,05 ml dung dch st (III) clorid 1,3%
(TT) vo khong 10 mg ch phm v un nng trn cch thu, s xut hin mu
xanh lam. Thm 0,05 ml acid nitric (TT), mu chuyn sang .
E. Ch phm cho phn ng ca cc alcaloid (Ph lc 7.1).
Dung dch S: Ho tan 50 mg ch phm trong nc khng c carbon dioxyd

(TT) v pha long cho 10 ml vi cng dung mi.
php 2).
pH
pH ca dung dch S phi ln hn 9 (Ph lc 5.9).
Gc quay cc ring
T - 142 n - 146o, tnh theo ch phm lm kh (Ph lc 5.13).
Ho tan 0,50 g ch phm trong ethanol 96% (TT) v pha long va 25,0
ml vi cng dung mi o.
Morphin
Khng c qu 0,13%.
Ho tan 0,10 g ch phm trong dung dch acid hydrocloric 0,1 N v pha
long n 5 ml vi cng dung mi. Thm 2 ml dung dch natri nitrit 1%, yn 15
pht v thm 3 ml dung dch amoniac 6 M (TT). Mu ca dung dch thu c
khng c m hn mu mu N4 (Ph lc 5.17, Phng php 2).
Alcaloid l
Bn mng: Silicagel G .
Dung mi khai trin: Amoniac m c - cyclohexan - ethanol (6: 30: 72).
Dung dch th: Ho tan 0,400 g ch phm trong ethanol (TT) v pha long
n 10 ml vi cng dung mi.
Dung dch i chiu (1): Pha long 1,5 ml dung dch th vi ethanol (TT)
va 100 ml.
Dung dch i chiu (2): Pha long 1 ml dung dch th vi ethanol (TT)
va 100 ml.
Trin khai trong bnh sc k n khi dung mi i c khong 15 cm, ly bn
mng ra kh ngoi khng kh v phun dung dch kali iodobismuthat (TT). Trn
sc k , ngoi vt chnh, bt k vt ph no ca dung dch th u khng c
m mu hn vt ca dung dch i chiu (1) v ch c mt vt ( pha trn vt
chnh) m mu hn vt ca dung dch i chiu (2).
Mt khi lng do lm kh
T 5,0 n 6,0% (Ph lc 5.16).
(1,00 g; 100 - 105oC).
Tro sulfat
Dng 1,0 g ch phm.
nh lng
Ho tan 0,250 g ch phm trong 30 ml acid acetic khan (TT), thm 10 ml
anhydrid acetic (TT) v 4 git dung dch tm tinh th (CT). Chun bng dung
dch acid percloric 0,1 N. Song song lm mu trng.
C18H21NO3.
Bo qun
Trong bnh kn trnh nh sng. c bng B, gy nghin.
Ch phm
Vin nn codein.
Vin codein - terpin hydrat, vin codein - natribenzoat.
Tc dng v cng dng

Gim au, chng ho, tr tiu chy.
21-CODEIN PHOSPHAT
Codeini phosphas
C18H21NO3. H3PO4. 1/2H2O (Hemihydrat) P.t.l: 406,4

C18H21NO3. H3PO4. 3/2H2O (Sesquihydrat) P.t.l: 424,4
Codein phosphat l (5R, 6S, 9R, 13S, 14R) - 4,5 - epoxy - 3 - methoxy - 9 methylmorphin - 7 - en - 6 - ol phosphat hemihydrat hoc sesquihydrat, phi cha
t 98,5 n 101,0% C18H21NO3. H3PO4, tnh theo ch phm lm kh.
Tnh cht
Tinh th nh khng mu hoc bt kt tinh trng, khng mi.
D tan trong nc, kh tan trong ethanol 96%, thc t khng tan trong
ether.
nh tnh
C th chn mt trong 2 nhm nh tnh sau:
Nhm I: B, E.
(TT) v pha long n 25,0 ml vi cng dung mi.
A. Pha long 1,0 ml dung dch S vi nc va 100,0 ml. Thm vo 25,0
ml dung dch ny 25 ml nc, 10 ml natri hydroxyd 1 M v pha long vi nc
va 100,0 ml. o ph t ngoi (Ph lc 3.1) ca dung dch trn di sng t
250 n 350 nm. Dung dch ch c duy nht mt cc i hp th 284 nm. hp

th ring bc sng cc i khong 38, tnh theo ch phm lm kh.
B. Ho tan 0,2 g ch phm trong 4 ml nc. Thm 1 ml hn hp ng th
tch dung dch natri hydroxyd 5 M (TT) v nc. khi mo kt tinh, c th c
vo thnh ng nghim bng mt a thu tinh v lm lnh trong nc . Ra ta
v sy kh 100 n 105oC. Ph hng ngoi (Ph lc 3.2) ca ta thu c phi
ph hp vi ph hng ngoi i chiu ca codein.
C. im chy ca ta thu c php th B t 155 n 159oC (Ph lc
5.19).
D. Thm 1 ml acid sulfuric (TT) v 2 git dung dch st (III) clorid 1,3%
vo khong 10 mg ch phm v un nng trn cch thu, s xut hin mu xanh
lam. Thm 2 git acid nitric (TT), mu chuyn sang .
E. Dung dch S cho phn ng A ca phosphat (Ph lc 7.1).
F. Ch phm cho phn ng ca cc alcaloid (Ph lc 7.1).
mu V6 (Ph lc 5.17, phng php 2).
pH
pH ca dung dch S phi t 4,0 n 5,0 (Ph lc 5.9).
Gc quay cc ring
Pha long 5,0 ml dung dch S vi nc va 10,0 ml o.
Morphin
Khng c qu 0,13%.
Ho tan 0,10 g ch phm trong dung dch acid hydrocloric 0,1 M v pha
long n 5 ml vi cng dung mi. Thm 2 ml dung dch natri nitrit 1%, yn 15
pht v thm 3 ml dung dch amoniac 6 M (TT). Mu ca dung dch thu c
khng c m hn mu mu N4 (Ph lc 5.17, Phng php 2).
Alcaloid l
Bn mng: Silicagel G (TT).
Dung mi khai trin: Amoniac m c - cyclohexan - ethanol (6: 30: 72).
Dung dch th: Ho tan 0,50 g ch phm trong mt hn hp gm 1 th tch
ethanol (TT) v 4 th tch dung dch acid hydrocloric 0,01 M, ri pha long n 10
ml vi cng hn hp dung mi.
Dung dch i chiu (1): Pha long 1,5 ml dung dch th vi hn hp gm
1 th tch ethanol (TT) v 4 th tch dung dch acid hydrocloric 0,01 M va 100
ml.
Dung dch i chiu (2): Pha long 1 ml dung dch th ti 100 ml vi hn
hp gm 1 th tch ethanol (TT) v 4 th tch dung dch acid hydrocloric 0,01 M.
Trin khai sc k n khi dung mi i c khong 15 cm, ly bn mng ra
kh ngoi khng kh v phun dung dch kali iodobismuthat (TT). Trn sc k ,
ngoi vt chnh, bt k vt ph no ca dung dch th, khng c m mu hn
vt ca dung dch i chiu (1) v ch c mt vt nh th ( pha trn vt chnh)
m mu hn vt ca dung dch i chiu (2).
Mt khi lng do lm kh
T 1,5 n 3,0% i vi dng hemihydrat v t 5,0 n 7,5% i vi dng
sesquihydrat (Ph lc 5.16).
(0,50 g; 100oC - 105oC).
Sulfat
Khng c qu 0,1% (Ph lc 7.4.12).
Ly 5 ml dung dch S pha long thnh 20 ml bng nc, ly 15 ml dung
dch ny tin hnh th.
Clorid
Khng c qu 0,05% (Ph lc 7.4.5).
Ly 2,5 ml dung dch S pha long thnh 15 ml bng nc v tin hnh th.
nh lng
anhydrid acetic (TT) v 4 git dung dch tm tinh th (CT). Chun bng dung
dch acid percloric 0,1 N. Song song lm mu trng.
C18H21NO3. H3PO4.
Bo qun
Trong ng kn trnh nh sng. c bng B, gy nghin.
Ch phm
Vin nn codein phosphat, dung dch ung codein phosphat, dung dch tim
codein phosphat.
Tc dng v cng dng
Gim au, chng ho, tr tiu chy.
22-DEXAMETHASON
Dexamethasonum
C22H29FO5 P.t.l: 392,5

Dexamethason l 9 - fluoro - 11 , 17,21- trihydroxy - 16 - methylpregna 1, 4 - dien - 3,20 - dion, phi cha t 97,0 n 103,0% C22H29FO5, tnh theo ch
phm lm kh.
Tnh cht
Bt kt tinh trng hoc gn nh trng, hoc tinh th khng mu, chy
khong 255oC km theo phn hu.
Thc t khng tan trong nc, hi tan trong ethanol 96%, kh tan trong
methylen clorid.
nh tnh
Nhm I: B, C.
Nhm II: A, C, D, E. A. Ho tan 10,0 mg ch phm trong ethanol (TT) v
pha long n 100,0 ml vi cng dung mi. Ly 2,0 ml dung dch ny cho vo ng
nghim thu tinh trn c nt mi, thm 10 ml dung dch phenylhydrazin - acid
sulfuric (TT), trn u v un nng trong cch thu 60oC trong 20 pht. Lm
lnh ngay. hp th (Ph lc 3.1) ca dung dch thu c o bc sng 419
nm phi khng di 0,4. Lm mu trng trong cng iu kin thay 2 ml dung dch
ch phm bng 2 ml ethanol (TT).
ngoi ca dexamethason chun.
C. Phng php sc k lp mng (Ph lc 4.4).

Dung mi khai trin: Butanol c bo ho nc - toluen - ether (5: 10:
85).
Dung dch th: Ho tan 10 mg ch phm trong mt hn hp gm 1 th tch
methanol (TT) v 9 th tch methylen clorid (TT), ri pha long n 10 ml vi
cng hn hp dung mi trn.
Dung dch i chiu (1): Ho tan 20 mg dexamethason chun trong mt
hn hp gm mt th tch methanol (TT) v 9 th tch methylen clorid (TT), ri
pha long n 20 ml vi cng hn hp dung mi trn.
Dung dch i chiu (2): Ho tan 10 mg betamethason chun trong dung
dch i chiu (1) v pha long n 10 ml vi cng dung dch ny.
Trin khai bn mng n khi dung mi i c 15 cm. bn mng kh ngoi
khng kh v kim tra di nh sng t ngoi bc sng 254 nm. Vt chnh thu
c trong sc k ca dung dch th phi tng t v v tr v kch thc vi
vt chnh trong sc k ca dung dch i chiu (1). Phun ln bn mng dung
dch acid sulfuric trong ethanol (TT). Sy bn mng 120oC trong khong 10
pht hoc n khi vt xut hin. ngui. Quan st di nh sng ban ngy v
nh sng t ngoi bc sng 365 nm. Vt chnh thu c trong sc k ca
dung dch th phi tng t v v tr, mu sc di nh sng ban ngy, hunh
quang di nh sng t ngoi 365 nm v kch thc vi vt chnh thu c t
dung dch i chiu (1). Php th ch c gi tr khi sc k ca dung dch i
chiu (2) cho 2 vt, tuy vy 2 vt ny c th khng tch ri nhau hon ton.
D. Thm khong 2 mg ch phm vo 2 ml acid sulfuric (TT) v lc ho
tan. Trong vng 5 pht, mt mu nu nht xut hin. Thm vo dung dch trn
10 ml nc v trn u. Mu bin mt.
E. Trn khong 5 mg ch phm vi 45 mg magnesi oxyd nng (TT) v

nung trong chn nung n khi thu c cn gn nh trng hon ton (thng di
5 pht). ngui, thm 1 ml nc, 0,05 ml dung dch phenolphtalein (CT) v
khong 1 ml dung dch acid hydrocloric long (TT) lm mt mu dung dch.
Lc. Thm 1 ml dch lc vo mt hn hp mi pha gm 0,1 ml dung dch alizarin
S (TT) v 0,1 ml dung dch zirconyl nitrat (TT). Trn u v yn 5 pht, so
snh mu ca dung dch thu c vi mu ca mt mu trng c chun b trong
cng iu kin. Dung dch th c mu vng v dung dch mu trng c mu .
Gc quay cc ring
T + 75 n + 80o, tnh trn ch phm lm kh (Ph lc 5.13).
Ho tan 0,250 g ch phm trong dioxan (TT) v pha long n 25,0 ml vi
cng dung mi o.
Tp cht lin quan
Tin hnh theo phng php sc k lng (Ph lc 4.3).
Pha ng A: Trong bnh nh mc 1000 ml, trn 250 ml acetonitril (TT)
vi 700 ml nc v cho cn bng, thm nc n vch v trn u.
Pha ng B: Acetonitril (TT).
Dung dch th: Ho tan 25,0 mg ch phm trong hn hp: Acetonitril (TT)
- methanol (TT) (1: 1) c 10,0 ml.
Dung dch i chiu: Pha long 1,0 ml dung dch th thnh 100,0 ml bng
pha ng A.
Dung dch phn gii: Ho tan 2 mg dexamethason chun v 2 mg methyl
prednisolon chun trong pha ng A c 100,0 ml.
iu kin sc k: Ct thp khng g (0,25 m x 4,6 mm) c nhi pha tnh
C (octadecylsilyl silica gel dng cho sc k 5 m). Nhit ct c duy tr
45oC.
Detector quang ph hp th t ngoi bc sng 254 nm.

Tc dng: 2,5 ml/pht.
Th tch tim: 20 l.
Cch tin hnh:
Tin hnh chy sc k theo chng trnh bng sau:
Thi gian
(Pht) Pha ng A
(% tt/tt)
Pha ng B
(% tt/tt)
Tin hnh
100
15
100 00 100Bt u gradient tuyn tnh
40
100
Kt thc qu trnh chy sc k, quay v 100% pha
100
Bt u cn bng vi pha ng A
46 - 0 100
Kt thc cn bng, bt u qu trnh chy sc k tip
ng dng
ng A
41
theo
Cn bng ct t nht trong 30 pht vi pha ng B v sau vi pha ng
A trong 5 pht. i vi cc ln chy sc k tip theo dng iu kin nh m t
trong bng trn t pht 40,0 n pht 46,0.
iu chnh nhy sao cho chiu cao ca pic chnh trong sc k ca
dung dch i chiu t nht bng 50% ca thang o.
Tim dung dch phn gii. Trong iu kin sc k m t, thi gian lu
ca methyl prednisolon khong 11,5 pht v ca dexamethason khong 13 pht.
Php th ch c gi tr khi h s phn gii gia pic methyl prednisolon v pic
dexamethason t nht l 2,8. Nu cn thit, iu chnh nng acetonitril trong

pha ng A.
Tim mu trng l hn hp dung mi acetonitril (TT) - methanol (TT) (1:
1), dung dch th v dung dch i chiu. Ghi sc k ca dung dch th trong
thi gian gp hai ln thi gian lu ca pic chnh. Bt c pic ph no ca dung dch
th khng c c din tch ln hn 0,5 ln din tch ca pic chnh ca dung dch
i chiu (0,5%), tng din tch ca tt c cc pic ph khng c ln hn din
tch ca pic chnh ca dung dch i chiu (1,0%). B qua pic ca mu trng v
bt k pic no c din tch nh hn 0,05 ln din tch ca pic chnh trong ca dung
dch i chiu.
Mt khi lng do lm kh
Khng c qu 0,5% (Ph lc 5.16).
(0,500 g; 100 - 105oC).
nh lng
Ho tan 0,100 g ch phm trong ethanol 96% (TT) v pha long n 100,0
ml vi cng dung mi. Pha long 1,0 ml dung dch trn thnh 100 ml vi ethanol
96% (TT) v o hp th (Ph lc 3.1) bc sng cc i 238,5 nm. Tnh hm
lng C22H29FO5 theo A (1%, 1 cm), ly 394 l gi tr A(1%, 1 cm) bc sng
238,5 nm.
Bo qun
Thuc c bng B. Trong l kn, trnh nh sng.
Cng dng
Corticosteroid.
Ch phm
Vin nn dexamethason.
23- DEXAMETHASON ACETAT

Dexamethasoni acetas
C24H31FO6 P.t.l: 434,5

Dexamethason acetat l 9-fluoro-11 , 17,21-trihydroxy-16 methylpregna1,4-dien-3,20-dion-21-acetat, phi cha t 97,0 n 103,0% C24H31FO6, tnh
theo ch phm lm kh.
Tnh cht
Bt kt tinh trng hoc gn nh trng. D tan trong ethanol 96% v aceton,
kh tan trong methylen clorid, thc t khng tan trong nc.
nh tnh
Nhm I: B, C.
A. Ho tan 10,0 mg ch phm trong ethanol (TT) v pha long n 100,0
ml vi cng dung mi. Ly 2,0 ml dung dch ny cho vo ng nghim thu tinh
trn c nt mi, thm 10,0 ml dung dch phenylhydrazin - acid sulfuric (TT), trn
u v un nng trong cch thu 60oC trong 20 pht. Lm lnh ngay. hp
th (Ph lc 3.1) ca dung dch c o bc sng cc i 419 nm phi khng
di 0,35.
ngoi ca dexamethason acetat chun. Nu ph thu c ca mu th v mu
chun khc nhau th ho tan cc mu ny trong cloroform (TT) vi lng ti thiu.
Bay hi dung mi trn ni cch thu ti kh, ly cn thu c o li ph hng

ngoi ln th hai.
Dung mi khai trin: Nc - methanol - ether - methylen clorid (1,2: 8: 15:
77).
Dung dch th: Ho tan 10 mg ch phm trong 10 ml hn hp methanol methylen clorid (1: 9).
Dung dch i chiu (1): Ho tan 20 mg dexamethason acetat chun trong
20 ml hn hp methanol - methylen clorid (1: 9).
Dung dch i chiu (2): Ho tan 10 mg cortison acetat chun trong 10 ml
khng kh v quan st di nh sng t ngoi bc sng 254 nm. Vt chnh ca
dung dch th phi tng ng v v tr v kch thc vi vt chnh ca dung
dch i chiu (1). Phun ln bn mng dung dch acid sulfuric trong ethanol (TT).
Sy bn mng 120oC trong khong 10 pht hoc n khi vt xut hin.
ngui. Quan st di nh sng ban ngy v nh sng t ngoi bc sng 365
nm. Vt chnh thu c trong sc k ca dung dch th phi tng t v v tr,
mu sc di nh sng ban ngy, hunh quang di nh sng t ngoi 365 nm
v kch thc vi vt chnh thu c t dung dch i chiu (1). Php th ch c
gi tr khi sc k ca dung dch i chiu (2) cho 2 vt tch ring bit r.
10 ml nc v trn u. Mu bin mt v dung dch vn trong.

snh mu ca dung dch thu c vi mu ca mt mu trng c pha ch trong
F. Khong 10 mg ch phm cho phn ng ca nhm acetyl (Ph lc 7.1).
Gc quay cc ring
T + 84 n + 90o, tnh theo ch phm lm kh (Ph lc 5.13).
Ho tan 0,250 g ch phm trong 25,0 ml dioxan (TT) o.
Tp cht lin quan
Kim tra bng sc k lng (Ph lc 4.3).
Pha ng: Trn 380 ml acetonitril (TT) vi 550 ml nc v n nh; pha
long vi nc thnh 1000 ml v trn u.
Dung dch th: Ho tan 25,0 mg ch phm trong khong 4 ml acetonitril
(TT) v pha long n 10,0 ml vi nc.
Dung dch i chiu: Pha long 1,0 ml dung dch th thnh 100,0 ml vi
pha ng.
Dung dch phn gii: Ho tan 2 mg dexamethason acetat chun v 2 mg
betamethason acetat chun trong 100,0 ml pha ng.
iu kin sc k:
Ct thp khng g (0,25 m x 4,6 mm) c nhi pha tnh C (octadecylsilyl
silica gel dng cho sc k, 5 m).

Tc dng: 1 ml/pht.
Th tch tim: 20 l.
Cch tin hnh:
Cn bng ct vi pha ng khong 30 pht.
Tim dung dch i chiu v iu chnh nhy ca h thng sao cho chiu
cao ca pic chnh trong sc k thu c phi khng di 50% thang o.
Tim dung dch phn gii. Khi sc k c ghi trong cc iu kin nu
trn th thi gian lu ca Betamethason acetat khong 19 pht v dexamethason
acetat khong 22 pht. Php th ch c gi tr khi phn gii gia hai pic
betamethason acetat v dexamethason acetat t nht l 3,3; nu cn, iu chnh
nng acetonitril trong pha ng.
Tim ring bit dung dch th v dung dch i chiu. Tin hnh sc k
trong khong thi gian gp 1,5 ln thi gian lu ca pic chnh. Trong sc k
thu c ca dung dch th, din tch ca bt c pic ph no ngoi pic chnh
khng c ln hn 0,5 ln din tch pic chnh trong sc k thu c t dung
dch i chiu (0,5%); tng din tch ca tt c cc pic ph khng c ln hn
din tch ca pic chnh trong sc k thu c t dung dch i chiu (1,0%). B
qua bt k pic no c din tch nh hn 0,05 ln din tch pic chnh trong sc k
ca dung dch i chiu.
Mt khi lng do lm kh
Khng c qu 0,5% (Ph lc 5.16).
(0,500 g: p sut gim; phosphor pentoxyd; 100 - 105oC).
nh lng
Ho tan 0,100 g ch phm trong ethanol 96% (TT) v pha long n 100,0
ml vi cng dung mi. Pha long 2,0 ml dung dch trn vi ethanol 96% (TT)
thnh 100,0 ml. o hp th ca dung dch thu c (Ph lc 3.1) bc sng

cc i 238,5 nm. Tnh hm lng C24H31FO6 theo A (1%, 1 cm) ly 357 l gi
tr A (1%, 1 cm) bc sng 238,5 nm.
Bo qun
Ch phm
Vin nn dexamethason acetat.
Tc dng v cng dng
Corticosteroid
24-DEXAMETHASON NATRI PHOSPHAT
Dexamethasoni natrii phosphas
C22H28FNa2O8P P.t.l: 516,4

Dexamethason natri phosphat l 9-fluoro-11 ,17,21-trihydroxy-16 methylpregna-1,4-dien-3,20-dion-21-dinatri phosphat, phi cha t 97,0 n
103,0% C22H28FNa2O8P, tnh theo ch phm khan v khng c ethanol.
Tnh cht
Bt trng hoc gn nh trng, rt d ht m. D tan trong nc, kh tan
trong ethanol 96%, thc t khng tan trong ether v methylen clorid.
nh tnh
Nhm I: B, C.
A. Ho tan 10 mg ch phm trong 5 ml nc v pha long n 100,0 ml vi
ethanol (TT). Ly 2,0 ml dung dch ny cho vo ng nghim thu tinh trn c nt
mi, thm 10,0 ml dung dch phenylhydrazin - acid sulfuric (TT), trn u v un
nng trong cch thu 60oC trong 20 pht. Lm lnh ngay. hp th (Ph lc
3.1) ca dung dch thu c o bc sng cc i 419 nm phi khng di 0,20.
ngoi ca dexamethason natri phosphat chun. Nu ph thu c ca mu th v
mu chun trng thi rn khng ging nhau th ho tan ring bit ch phm v
cht chun trong mt th tch ti thiu ethanol 96% (TT), lm bay hi n kh trn
cch thu v dng nhng cn thu c ghi li ph mi.
Dung mi khai trin: Anhydrid acetic - nc - butanol (2: 2: 6). Dung dch
th: Ho tan 10 mg ch phm trong 10 ml methanol (TT).
Dung dch i chiu (1): Ho tan 20 mg dexamethason natri phosphat
chun trong 20 ml methanol (TT).
Dung dch i chiu (2): Ho tan 10 mg prednisolon natri phosphat chun
trong 10 ml dung dch i chiu (1).
khng kh v quan st di nh sng t ngoi bc sng 254 nm, vt chnh ca
dung dch th phi tng t v v tr v kch thc vi vt chnh ca dung dch i
chiu (1). Phun ln bn mng dung dch acid sulfuric trong ethanol (TT). Sy bn
mng 120oC trong khong 10 pht hoc n khi vt xut hin. ngui. Quan
st di nh sng ban ngy v nh sng t ngoi bc sng 365 nm. Vt chnh

thu c trong sc k ca dung dch th phi tng t v v tr, mu sc di
nh sng ban ngy, hunh quang di nh sng t ngoi 365 nm, v kch thc
vi vt chnh thu c t dung dch i chiu (1). Php th ch c gi tr khi sc
k ca dung dch i chiu (2) cho 2 vt, tuy nhin 2 vt ny c th khng tch
ri nhau hon ton.
10 ml nc v trn u. Mu nht dn v dung dch vn trong.
snh mu ca dung dch thu c vi mu ca mt mu trng c chun b trong
F. Thm vo 40 mg ch phm 2 ml acid sulfuric (TT) v un nh cho n
khi khi trng bay ln, thm tng git acid nitric (TT), tip tc un nng cho n
khi dung dch gn nh khng mu, lm ngui. Thm 2 ml nc, un cho n khi
khi trng bay ln mt ln na, lm ngui, thm 10 ml nc v trung tnh ho vi
giy qu (CT) bng dung dch amoniac long (TT). Dung dch thu c cho phn
ng ca natri v ca phosphat (Ph lc 7.1).
(TT) v pha long n 20 ml vi cng dung mi. Dung dch S phi trong (Ph lc
5.12) v khng c m mu hn mu mu N7 (Ph lc 5.17, phng php 2).
pH
Pha long 1 ml dung dch S n 5 ml vi nc khng c carbon dioxyd
(TT). pH ca dung dch thu c phi t 7,5 - 9,5. (Ph lc 5.9).
Gc quay cc ring
T + 75 n + 83o, tnh theo ch phm khan, khng cha ethanol (Ph lc
5.13). Ho tan 0,250 g ch phm trong 25,0 ml nc o.
Tp cht lin quan
Kim tra bng phng php sc k lng (Ph lc 4.3).
Pha ng: Trong mt bnh nn 250 ml, cn 1,360 g kali dihydrophosphat
(TT) v 0,600 g hexylamin (TT), trn u v yn trong 10 pht, sau ho tan
trong 182,5 ml nc; thm 67,5 ml acetonitril (TT), trn u.
Dung dch th: Ho tan 25 mg ch phm trong pha ng v pha long thnh
10,0 ml vi cng dung mi.
Dung dch i chiu: Pha long 1,0 ml dung dch th thnh 100,0 ml bng
pha ng.
Dung dch phn gii: Ho tan 2 mg dexamethason natri phosphat chun v
2 mg betamethason natri phosphat chun trong pha ng v pha long thnh 100,0
ml vi cng dung mi.
iu kin sc k: Ct thp khng g (0,25 m x 4,6 mm) c nhi pha tnh
C (octadecylsilyl silica gel dng cho sc k, 5 m).
Tc dng: 1 ml/pht.
Th tch tim: 20 l.
Cch tin hnh: Cn bng ct vi pha ng trong khong 45 pht.
Tim dung dch i chiu v iu chnh nhy ca h thng sao cho chiu
cao ca pic chnh trong sc k thu c t nht bng 50% thang o.
Tim dung dch phn gii. Khi sc k c ghi trong cc iu kin nu
trn th thi gian lu ca betamethason natri phosphat khong 12,5 pht v
dexamethason natri phosphat khong 14 pht. Php th ch c gi tr khi phn
gii gia hai nh betamethason natri phosphat v dexamethason natri phosphat t
nht l 2,2. Nu cn, iu chnh nng acetonitril hoc tng nng nc trong
pha ng.
Tim dung dch th v dung dch i chiu. Tin hnh sc k trong khong
thi gian gp 2 ln thi gian lu ca pic chnh. Trong sc k thu c ca dung
dch th: din tch ca bt c pic ph no ngoi pic chnh khng c ln hn 0,5
ln din tch pic chnh trong sc k thu c t dung dch i chiu (0,5%);
tng din tch ca tt c cc pic ph khng c ln hn din tch ca pic chnh
trong sc k thu c t dung dch i chiu (1,0%). B qua bt k pic no c
din tch nh hn 0,05 ln din tch pic chnh trong sc k ca dung dch i
chiu.
Phosphat v c
Khng c qu 1%.
Ho tan 50 mg ch phm trong 100 ml nc. Thm vo 10 ml dung dch
ny 5 ml thuc th molybdovanadic (TT), trn u v yn trong 5 pht. Mu
vng ca dung dch khng c m hn mu vng ca mu i chiu c chun
b ng thi v theo cch tng t vi 10 ml dung dch phosphat mu 5 phn triu.
Ethanol
Khng c qu 8,0% (kl/kl).
Xc nh bng sc k kh (Ph lc 4.2).
Dung dch chun ni: Pha long 1,0 ml n-propanol (TT) vi nc thnh
100,0 ml.
Dung dch th: Ho tan 0,5 g ch phm trong 5,0 ml dung dch chun ni
v pha long vi nc thnh 10,0 ml.
Dung dch chun: Pha long 1,0 g ethanol (TT) vi nc thnh 100,0 ml.
Ly 2,0 ml dung dch ny, thm vo 5,0 ml dung dch chun ni v pha long vi
nc thnh 10,0 ml.
iu kin sc k:
Ct (1 m x 3,2 mm) c nhi cht ng trng hp ethylvinylbenzendivinylbenzen copolymer (150 m - 180 m).
Kh mang l nitrogen dng cho sc k kh, lu lng 30 ml/pht.
Duy tr nhit ct 150oC, nhit ca bung tim 250oC v nhit
detector 280oC.
Th tch tim: 2 l.
Ethanol v nc
Xc nh hm lng nc (Ph lc 6.6) dng 0,200 g ch phm. Tng hm
lng phn trm ca ethanol c tm thy php th ethanol v hm lng phn
trm nc khng c qu 16,0% (kl/kl).
nh lng
Ho tan 0,100 g ch phm trong nc v pha long n 100,0 ml vi cng
dung mi. Pha long 5,0 ml dung dch thu c thnh 250,0 ml vi nc. o
hp th (Ph lc 3.1) ca dung dch bc sng cc i 241,5 nm. Tnh hm
lng C22H28FNa2O8P theo A (1%, 1 cm), ly 303 l gi tr A (1%, 1 cm)
241,5 nm.
Bo qun
Ch phm
Dexamethason natri phosphat tim; Dexamethason natri phosphat nh mt.
25-DIETHYL PHTALAT
Diethylis phthalas
C12H14O4 P.t.l: 222,2

Diethyl phtalat l diethylbenzen - 1,2 - dicarboxylat, phi cha t 99,0 n
101,0% C12H14O4.
Tnh cht
Cht lng snh, trong sut, khng mu hoc c mu vng rt nht, khng
mi hoc hu nh khng mi.
Thc t khng tan trong nc, ho ln vi ethanol 96%, vi ether v
hydrocarbon thm.
nh tnh
Ph hng ngoi (Ph lc 3.2) ca ch phm phi ph hp vi ph hng
ngoi i chiu ca diethyl phtalat hoc ph hng ngoi ca diethyl phtalat chun.
trong v mu sc ca ch phm
Ch phm phi trong (Ph lc 5.12) v khng c c mu m hn mu
T trng 20oC
1,115 n 1,121 (Ph lc 5.15).

Ch s khc x 20oC
1,500 n 1,505 (Ph lc 5.7).
Gii hn acid
Ho tan 20,0 g ch phm trong 50 ml ethanol 96% (TT) c trung ho
trc vi dung dch phenolphtalein (CT). Nh dung dch natri hydroxyd 0,1 N ti
khi xut hin li mu hng bn vng trong 30 giy. Lng dung dch natri
hydroxyd 0,1 N tiu th khng c qu 0,1 ml.
Nc
Dng 5,0 g ch phm th.
Tro sulfat
Dng 1,0 g ch phm
nh lng
Cn 0,750 g ch phm vo bnh thu tinh dung tch 250 ml. Thm 25,0 ml
dung dch kali hydroxyd 0,5 M trong ethanol v vi vin bt. un si trn cch
thu di sinh hn ngc trong 1 gi. Thm 1 ml dung dch phenolphtalein (CT)
v chun ngay bng dung dch acid hydrocloric 0,5 M. Song song lm mu
trng.
1 ml dung dch kali hydroxyd 0,5 M trong ethanol tng ng vi 55,56
mg C12H14O4.
Bo qun
ng trong l kn, ni kh mt.
Ch phm
Thuc m DEP.
Tc dng v cng dng
Tr gh, nga.
26- DIMERCAPROL
Dimercaprolum
B.A.L
C3H8OS2
P.t.l: 124,2
Dimercaprol l (RS)-2,3- dimercaptopropan -1-ol, phi cha t 98,5 n

101,5% C3H8OS2.
Tnh cht
Cht lng trong sut khng mu hoc mu vng nht, c mi ti.
Tan trong nc, ethanol (khong 750 g/l) v methanol.
nh tnh
A. Ho tan 0,05 ml ch phm trong 2 ml nc, thm 1 ml dung dch iod 0,1
N. Mu ca iod bin mt ngay.
B. Ho tan 0,1 ml ch phm trong 5 ml nc, thm 2 ml dung dch ng
sulfat 12,5%. Ta mu xanh en xut hin v chuyn sang mu xm en.
C. Trong bnh nn c nt mi trn 0,6 g natri bismuthat (TT) ( c un
trc 200oC trong 2 gi) vi hn hp gm 2,8 ml dung dch acid phosphoric
10% (kl/kl), 6 ml nc. Thm 0,2 ml ch phm, trn u v 10 pht, thnh
thong lc. Ly 1 ml cht lng pha trn, thm 5 ml dung dch mui natri ca acid
cromotropic 4 g/l trong acid sulfuric m c, trn u. un trong cch thu 15
pht, mu tm xut hin.
trong v mu sc ca ch phm
Ch phm phi trong (Ph lc 5.12) v mu khng c m hn mu mu
N6 hoc NV6 (Ph lc 5.17, phng php 2).
Gii hn acid - kim
Ho tan 0,2 g ch phm trong nc khng c carbon dioxyd (TT) va 10
ml. Thm 0,25 ml dung dch lc bromocresol (CT1) v 0,3 ml dung dch acid
hydrocloric 0,01 N. Mu ca dung dch phi vng. chuyn sang mu xanh,
khng c dng qu 0,5 ml dung dch natri hydroxyd 0,01 N.
Ch s khc x
1,568 - 1,574 (Ph lc 5.7).
Halogen
Ho tan 2,0 g ch phm trong 25 ml dung dch kali hydroxyd trong ethanol
(TT), un hi lu 2 gi. Lm bay hi ethanol bng cch bc hi trong lung kh
nng, thm 20 ml nc, ngui. Thm vo hn hp 40 ml nc v 10 ml dung
dch hydrogen peroxyd 100 th tch, un si nh trong 10 pht, ngui, lc
nhanh. Thm 10 ml dung dch acid nitric 2 M (TT), 5 ml dung dch bc nitrat 0,1
N v 2 ml dung dch st (III) amoni sulfat (CT) lm ch th, nh lng bng dung
dch amoni thiocyanat 0,1 N cho n mu vng . Thc hin mu trng nh trn
nhng khng c ch phm. Th tch dung dch chun dng cho 2 ln nh
lng khng c lch nhau qu 1,0 ml.
nh lng
Ho tan 0,100 g ch phm trong 40 ml methanol (TT). Thm 20 ml dung
dch acid hydrocloric 0,1 N v 50 ml dung dch iod 0,1 N. yn 10 pht ri
chun bng dung dch natri thiosulfat 0,1 N. Thc hin song song mu trng
trong cng iu kin.
1 ml dung dch iod 0,1 N tng ng vi 6,21 mg C3H8OS2.
Bo qun
Trong chai nh, y kn, ni trnh nh sng c nhit t 2 n 8oC.
Ch phm
Dimercaprol tim.
Tc dng v cng dng
Tr ng c arsen, vng v thu ngn.
27- EPHEDRIN HYDROCLORID
Ephedrini hydrochloridum
C10H15NO. HCl
P.t.l: 201,7
Ephedrin hydroclorid l (1R, 2S)-2-methylamino-1-phenylpropan-1-ol

hydroclorid, phi cha t 99,0 n 101,0% C10H15NO. HCl, tnh theo ch phm
lm kh.
Tnh cht
Tinh th nh khng mu hay bt kt tinh trng.
D tan trong nc, tan trong ethanol 96%, thc t khng tan trong ether.
nh tnh
Nhm I: A, E.
Nhm II: B, C, D, E. A. Ph hng ngoi (Ph lc 3.2) ca ch phm phi
ph hp vi ph hng ngoi ca ephedrin hydroclorid chun.
B. Ch phm phi t yu cu trong php th "Gc quay cc ring".

C. Trong php th "Tp cht lin quan", vt chnh thu c t sc k
ca dung dch th (2) phi tng t v v tr, mu sc, kch thc vi vt chnh thu
c t sc k ca dung dch i chiu (1).
D. Ly 0,1 ml dung dch S, thm 1 ml nc, 0,2 ml dung dch ng sulfat
12,5%, 1 ml dung dch natri hydroxyd 40% (TT) s xut hin mu tm. Lc dung
dch ny vi 2 ml ether (TT): Lp ether c mu ta v lp nc c mu lam.
E. Dung dch S phi cho phn ng ca clorid (Ph lc 7.1).
Dung dch S: Ho tan 5,00 g ch phm trong nc va 50,0 ml.
php 2).
Gii hn acid - kim
Ly 10 ml dung dch S, thm 0,1 ml dung dch methyl (CT). Nu dung
dch c mu vng th phi chuyn sang mu hng khi thm khng qu 0,4 ml dung
dch acid hydrocloric 0,01 N hoc nu dung dch c mu hng th phi chuyn
sang mu vng khi thm khng qu 0,2 ml dung dch natri hydroxyd 0,01 N.
Gc quay cc ring
T - 33,5 n - 35,5o, tnh theo ch phm lm kh (Ph lc 5.13).
Pha long dung dch S chnh xc vi nc n gp i o.
im chy
217 - 220oC (Ph lc 5.19).
Sulfat
Khng c qu 0,010% (Ph lc 7.4.12).
Ly 15 ml dung dch S tin hnh th.

Tp cht lin quan
Khng c qu 0,5%.
Thc hin bng phng php sc k lp mng (Ph lc 4.4).
Bn mng: Silicagel G.
Dung mi khai trin: Cloroform - amoniac m c -2-propanol (5: 15: 20).
Dung dch th (1): Ho tan 0,2 g ch phm trong methanol (TT) v pha long
thnh 10 ml vi cng dung mi.
Dung dch th (2): Pha long 1 ml dung dch th (1) thnh 10 ml vi
methanol (TT).
Dung dch i chiu (1): Ho tan 20 mg ephedrin hydroclorid chun trong
methanol (TT) v pha long thnh 10 ml vi cng dung mi.
Dung dch i chiu (2): Pha long 1,0 ml dung dch th (1) thnh 200 ml
vi methanol (TT).
Trin khai n khi dung mi i c 15 cm. bn mng kh ngoi khng kh v
phun bn mng vi dung dch ninhydrin (TT). Sy 110oC trong 5 pht. Ngoi
tr vt chnh, bt c vt no trong sc k ca dung dch th (1) cng khng
c m mu hn vt chnh thu c t sc k ca dung dch i chiu (2).
Khng k n bt c vt no c mu nht hn mu nn.
Mt khi lng do lm kh
Khng c qu 0,5% (Ph lc 5.16).
(1,000 g; 105oC).
Tro sulfat
Dng 1,0 g ch phm.

nh lng
Ho tan 0,170 g ch phm trong 10 ml dung dch thu ngn (II) acetat (TT)
bng cch lm nng, thm 50 ml aceton (TT), 1 ml dung dch bo ho da cam
methyl trong aceton. Chun bng dung dch acid percloric 0,1 N n khi c
mu . Song song lm mt mu trng trong cng iu kin.
C10H15NO. HCl.
Bo qun
Bng B, ng trong l kn, trnh nh sng.
Cng dng
Tc nhn adrenegic.
Ch phm
Thuc tim ephedrin hydroclorid; vin nn ephedrin hydroclorid.
28- ETHANOL
Ethanolum
Alcol tuyt i, alcol khan
CH3 - CH2 - OH
C2H5OH
P.t.l: 46,07
Ethanol phi cha t 99,4% (tt/tt) n 100,0% (tt/tt) hoc t 99,0% (kl/kl)
n 100,0% (kl/kl) C2H5OH.
Tnh cht
Cht lng khng mu, trong, ng v d bay hi, si 78oC, c mi thm

c trng ca ru, d chy, chy vi ngn la mu xanh da tri, khng c khi,
ht m. Ha trn vi nc, cloroform v vi ether.
nh tnh; gii hn acid - kim; trong ca dung dch; aldehyd; benzen;
tp cht bay hi; cht khng bay hi; clorid v kim loi nng.
Phi tun theo cc yu cu v phng php th nh qui nh trong
chuyn lun ethanol 96%.
T trng biu kin
T 788,16 n 791,2 kg m-3 (Ph lc 5.15).
Bo qun
Trnh m, nhit t 8 n 15oC, d chy.
29-ETHANOL 96%
Ethanolum 96%
CH3 - CH2 - OH
C2H5OH
P.t.l: 46,07
Ethanol 96% l hn hp ethanol v nc, cha t 93,8% (kl/kl) n 94,7%

(kl/kl) hoc t 96,0% (tt/tt) n 96,6% (tt/tt) C2H5OH.
Tnh cht
Cht lng khng mu, trong sut, d bay hi, c mi c trng, d chy,
khi chy khng c khi v ngn la c mu xanh. Ho ln vi nc, cloroform,
ether v glycerin.
nh tnh
A. un nng 1 ml ch phm vi 1 ml acid acetic bng (TT) v thm vi
git dung dch acid sulfuric long (TT), s c mi ethyl acetat.
B. Thm 1 ml dung dch natri hydroxyd 1 M vo 5 ml dung dch ch phm

0,5% (tt/tt) trong nc, sau thm t t 2 ml dung dch trong nc c cha 2%
iod v 4% kali iodid. S c mi iodoform bay ln v c ta mu vng xut hin.
Gii hn acid - kim
Thm 0,25 ml dung dch phenolphtalein (CT) vo 20 ml ch phm. Dung
dch phi khng mu v phi chuyn sang mu hng khi thm khng c qu 0,2
ml dung dch natri hydroxyd 0,1 M.
trong ca dung dch
Pha long 5,0 ml ch phm thnh 100 ml bng nc, dung dch thu c
phi trong (Ph lc 5.12).
T trng biu kin
T 803,8 n 806,3 kg m-3 (Ph lc 5.15).
Aldehyd
Thm 5 ml nc, 1 ml dung dch fuchsin c kh mu (TT) vo 5,0 ml
ch phm. yn 30 pht. Bt k mu no xut hin trong dung dch th cng
khng c m hn mu ca dung dch i chiu c tin hnh trong cng iu
kin, cng thi gian, nhng thay 5 ml ch phm bng 5 ml dung dch c cha
0,001% acetaldehyd c ct li trong ethanol khng c aldehyd (TT).
Benzen
Hnh 1. Ph hp th t ngoi o hm bc hai in hnh ca ethanol 96%
cha khong 2 phn triu benzen.
Ghi ph t ngoi o hm bc hai (Ph lc 3.1) ca cc dung dch sau y
trong khong bc sng t 230 nm n 300 nm, dng cc o c di quang trnh
ti 4 cm. Dung dch (1) l ch phm. Dung dch (2) c cha 0,00020% (tt/tt)
benzen trong ch phm. Php th ch c gi tr khi bin Y trong hnh 1 trn ph
ca dung dch (2) ln hn 8 ln gi tr dao ng trung bnh ca hai pic k tip
nhau trong khong 280 nm n 300 nm. Trn ph ca dung dch (2), o bin
Y2. o bt k bin tng ng Y1 trn ph ca dung dch (1). Gi tr Y1 phi
khng c ln hn Y2 - Y1.
Tp cht bay hi
Tin hnh bng phng php sc k kh (Ph lc 4.2).
Dung dch chun ni: Cha 0,020% (tt/tt) butan-2-on.
Dung dch th (1) l ch phm.
Dung dch th (2) l ch phm c cha 0,020% (tt/tt) chun ni.
iu kin sc k:
Ct thu tinh (1,5 m x 4 mm) c nhi cc ht polymer xp (100 n 120
mesh) (Porapak N, Porapak Q v Chromosorb 102 l thch hp) v duy tr nhit
130oC.
Cch tin hnh:
Ghi sc k trong khong thi gian gp i thi gian lu ca chun ni.
Trong sc k ca dung dch th (2), din tch ca pic ph bt k no cng
khng c ln hn din tch pic ca dung dch chun ni v tng din tch ca
cc pic ph khng c ln hn hai ln din tch pc ca dung dch chun ni.
Cht khng bay hi
Khng c qu 0,005%.
Ly 100 ml ch phm lm bay hi trn cch thu n kh, sy cn 105oC
n khi lng khng i. Cn cn li khng c qu 5 mg.
Clorid
Thm 2 git dung dch acid nitric 10% (TT) v 2 git dung dch bc nitrat
2% (TT) vo 10 ml ch phm, yn 5 pht. Dung dch khng c c.
Kim loi nng
Ly chnh xc 20 ml ch phm cho vo cc v bc hi n kh trn cch
thu. Ho tan nng cn trong 20 ml nc v ngui. Ly 12 ml dung dch ny
tin hnh th theo phng php 1. Dng dung dch ch mu 1 phn triu chun
b mu i chiu.
Bo qun
Trnh m, nhit t 8 n 15oC, d chy.
30- ETHER M
Aether anaesthesicus
C4H10O
P.t.l: 74,1
Ether m l diethyl ether c cha mt lng thch hp cht chng oxy ho

khng bay hi ph hp.
Tnh cht
Cht lng trong sut, khng mu, rt linh ng, c mi c bit. D chy,
d bay hi. Hi ether ho ln mt t l nht nh vi khng kh, oxy hoc
nitrogen oxyd cho hn hp n. Tan trong 15 phn nc, tan theo bt c t l no
trong ethanol, benzen, cloroform, ether du ho, cc du bo v cc tinh du.
nh tnh
A. Ch phm phi t yu cu php th v t trng.
B. Ch phm phi t yu cu php th v khong chng ct.
T trng
0,714 n 0,716 (Ph lc 5.15).
Khong chng ct
Khng ct nu ch phm khng p ng php th peroxyd. Ch phm phi
c ct hon ton trong khong 34 - 35oC (Ph lc 5.20).
Ether m phi tun theo cc yu cu v phng php th tinh khit nh
"Ether thng", ngoi ra cn phi p ng cc yu cu sau:
Peroxyd
Cho 8,0 ml dung dch kali iodid - h tinh bt (TT) vo ng nghim nt mi
c dung tch khong 12 ml, ng knh 1,5 cm. Lm y bng ch phm v lc
mnh, yn ch ti 30 pht, khng c xut hin mu.
Cn sau khi bay hi
Khng c qu 0,002%.
Khng tin hnh php th ny nu nh ch phm khng t yu cu v
peroxyd. Ly chnh xc 50,0 ml ch phm v tin hnh nh "Ether thng". Cn
cn li khng c qu 1,0 mg.
Nc
Khng c qu 0,2% (kl/tt) (Ph lc 6.6).
Dng 20 ml ch phm.
Bo qun
Thuc c bng B. Trong l kn, trnh nh sng v ch mt (nhit
t 8 - 15oC), rt d chy.
Ghi ch: Khng c dng gy m nu l m qu 24 gi.
Sau thi hn 6 thng bo qun phi kim tra cht lng ca ch phm.
Nhn cn phi ghi loi, nng bt k cht chng oxy ho khng bay hi
c thm vo; ng thch hp cho vic s dng gy m.
Cng dng
Gy m.
31- Ether thng
Aether medicinalis
C4H10O
P.t.l: 74,1
Ether thng l diethyl ether cha t 96,0 n 98,0% C4H10O, c cha

mt t ethanol v nc.
Tnh cht
Cht lng trong sut, khng mu, rt linh ng, c mi c bit. D chy,
d bay hi. Hi ether ho ln mt t l nht nh vi khng kh, oxy hoc
nitrogen oxyd cho hn hp n. Tan trong 15 phn nc, tan theo bt c t l no
trong ethanol, benzen, cloroform, ether du ho, cc du bo v cc tinh du.
nh tnh
A. Ch phm phi t yu cu php th v t trng.
B. Ch phm phi t yu cu php th v khong chng ct.
T trng
0,714 n 0,718 (Ph lc 5.15).
Khong chng ct
Khng ct nu ch phm khng p ng php th peroxyd. Ch phm phi
c ct hon ton trong khong 34 - 36oC (Ph lc 5.20).
Gii hn acid
Ly 20,0 ml ethanol 96% (TT) cho vo bnh nn c nt mi dung tch 50

ml, thm 0,25 ml dung dch xanh bromothymol (CT) v nh dung dch natri
hydroxyd 0,02 M cho ti khi xut hin mu xanh bn vng trong 30 giy. Thm
25,0 ml ch phm, trn u v nh thm dung dch natri hydroxyd 0,02 M cho ti
khi mu xanh xut hin tr li bn vng trong 30 giy. Th tch dung dch natri
hydroxyd 0,02 M dng khng c ln hn 0,4 ml.
Peroxyd
Cho 8,0 ml dung dch kali iodid 10% (TT) vo ng nghim c nt mi,
dung tch khong 12 ml, ng knh 1,5 cm. Lm y bng ch phm v lc mnh,
yn ch ti 30 pht. Bt c mu vng no xut hin khng c m hn
mu ca dung dch gm 0,5 ml dung dch iod 0,0005 M c pha long vi 8,0 ml
dung dch kali iodid 10% (TT).
Hydrocarbur
Cho vo ng nghim c nt mi trng sch bng acid sulfuric (TT) 5,0
ml ch phm, ngm vo nc lnh v thm t t trong 5 pht 5,0 ml acid sulfuric
m c (TT), va cho va lc v lm lnh. ch ti 30 pht. Mu ca hn hp
khng c sm hn mu ca acid sulfuric m c (TT).
Aceton v aldehyd
Lc 10,0 ml ch phm vi 1 ml dung dch kali tetraiodomercurat kim (TT)
trong ng nghim c nt mi trong 10 giy v yn 5 pht trong bng ti. Ch
c xut hin c nh lp cht lng pha di.
Nu khng t c yu cu trn, ly 40,0 ml ch phm em ct n cn li
khong 5 ml, dch ct c hng vo bnh lm lnh trong nc . Th li vi
10,0 ml dch ct (qu trnh ct li ch p dng khi ch phm t yu cu v
peroxyd).
Mi l
Nh dn dn 10,0 ml ch phm ln mnh giy lc sch, khng mi, c din

tch khong 25 cm2, bay hi ngoi khng kh. Sau khi ether bay hi, giy
lc khng c mi l.
Cn sau khi bay hi
Khng tin hnh php th ny nu nh ch phm khng t yu cu v
peroxyd. Ly chnh xc 70,0 ml ch phm cho vo cc thu tinh cn b. Lm
bay hi trn cch thu. Cn cn li sau khi sy 100 - 105oC n khi lng
khng i, khng c qu 1,0 mg.
Bo qun
Thuc c bng B. Trong l kn, trnh nh sng, nhit khng qu
15oC v rt d chy.
Cng dng
Lm dung mi.
32- GLUCOSE KHAN
Glucosum anhydricum
Dextrose
C6H12O6
P.t.l: 180,2
Glucose khan l D-(+) - glucopyranose.

Tnh cht
Bt kt tinh trng, khng mi, v ngt.
D tan trong nc, hi tan trong ethanol 96%.

nh tnh
A. t mt t ch phm trong ng nghim, ch phm s chy, phng ln,
chy v c mi ng chy.
B. Ho tan 0,2 g ch phm vo 5 ml nc, thm 2 ml thuc th Fehling
(TT), un n si s hnh thnh ta nu.
C. Ch phm phi p ng php th gc quay cc ring.
Gc quay cc ring
T + 52,5 n + 53,3o, tnh theo ch phm khan (Ph lc 5.13).
Ho tan 10,0 g ch phm trong 80 ml nc, thm 0,2 ml dung dch amoniac
10% (TT), yn 30 pht v pha long n 100 ml bng nc o.
Dung dch cha 10,0 g ch phm trong 15 ml nc phi trong (Ph lc
5.12) v mu khng c m hn mu mu NV7 (Ph lc 5.17, phng php 2).
Gii hn acid
Ho tan 5,0 g ch phm trong 50 ml nc khng c carbon dioxyd (TT) ri
chun bng dung dch natri hydroxyd 0,02 N vi dung dch phenolphtalein
(CT) lm ch th. Mu ca dung dch phi chuyn sang hng khi dng khng qu
0,3 ml dung dch natri hydroxyd 0,02 N.
Arsen
Dng 1,0 g ch phm th theo phng php A.
Clorid
Khng c qu 0,0125% (Ph lc 7.4.5).
Dung dch S: Ho tan 10,0 g ch phm trong nc v pha long n 100 ml

bng nc.
Dng 4 ml dung dch S pha long thnh 15 ml vi nc v tin hnh th.
Sulfat
Khng c qu 0,02% (Ph lc 7.4.12).
Dng 7,5 ml dung dch S pha long thnh 15 ml vi nc v tin hnh th.
Kim loi nng
Ho tan 4,0 g ch phm trong 20 ml nc. Ly 12 ml dung dch ny th
theo phng php 1. Dng dung dch ch mu 1 phn triu chun b mu i
chiu.
ng t tan v dextrin
Ho tan 1,0 g ch phm trong 30 ml ethanol 90% bng cch un si.
ngui, dung dch thu c khng c c hn 30 ml ethanol 90%.
Tinh bt tan
Ho tan 2,5 g ch phm trong 25 ml nc, un si 1 pht, ngui ri thm
0,1 ml dung dch iod 0,1 N, mu xanh khng c xut hin.
Sulfit
Ho tan 2,5 g ch phm trong 25 ml nc, thm 0,1 ml dung dch iod 0,1 N
v vi git dung dch h tinh bt (CT), mu xanh phi xut hin.
Tro sulfat
Khng c qu 0,1%.
Ho tan 5,0 g ch phm trong 5 ml nc v thm 2 ml acid sulfuric (TT),

bc hi n kh trn cch thu v nung n khi lng khng i. Nu cn thit
lm nng li vi acid sulfuric (TT).
Nc
Bari
Thm 1 ml dung dch acid sulfuric 1 M vo 10 ml dung dch S. Kim tra
ngay v sau 1 gi, dung dch khng c c hn dung dch i chiu gm 10 ml
dung dch S v 1 ml nc.
Calci
Khng c qu 0,02% (Ph lc 7.4.3).
Ly 5,0 ml dung dch S pha long thnh 15 ml vi nc v tin hnh th.
Cht gy st
Nu ch phm d nh sn xut thuc tim di dng ng gi th tch
ln th phi p ng yu cu v cht gy st (Ph lc 10.5). Tim 10 ml dung dch
c cha 50 mg ch phm trong 1 ml nc pha thuc tim cho 1 kg th.
Bo qun
ng trong l kn.
Ch phm
Glucose tim truyn tnh mch; dung dch ung phi hp vi cc mui
b mt nc: Kali clorid v glucose tim truyn tnh mch: Kali clorid, natri v
glucose tim truyn tnh mch; natri clorid v glucose tim truyn tnh mch.
33-Glucose ngm mt phn t nc
Glucosum monohydricum
Dextrose ngm mt phn t nc
C6H12O6. H2O
P.t.l: 189,2
Glucose ngm mt phn t nc l D- (+) - glucopyranose ngm mt phn

t nc.
Tnh cht
Ch phm c tnh cht c m t trong chuyn lun "Glucose khan".
nh tnh
Ch phm c cc phn ng nh tnh ca chuyn lun "Glucose khan".
Ch phm phi p ng c cc yu cu ca chuyn lun "Glucose khan"
tr php th nc
Nc
T 7,0 n 10,0% (Ph lc 6.6).
Dng 0,500 g ch phm.
Bo qun
Xem chuyn lun "Glucose khan".
Ch phm
Xem chuyn lun "Glucose khan".
34-GLYCERIN
Glycerinum
Glycerol
CH2OH
CHOH
CH2OH
C3H8O3
P.t.l: 92,1
Glycerin l propan 1,2,3-triol, phi cha t 98,0 n 101,0% C3H8O3, tnh

theo ch phm khan.
Tnh cht
Cht lng snh, trong sut, khng mu, khng mi, v nng v ngt, ht m
mnh.
Trn ln c vi nc v ethanol 96%, kh tan trong aceton, thc t
khng tan trong benzen, cloroform, du bo, ether, ether du ho, tinh du.
nh tnh
Nhm I: A, D.
Nhm II: B, C, D.
A. Ly 5 ml ch phm, thm vo 1 ml nc, trn cn thn. Ph hng ngoi
(Ph lc 3.2) ca dung dch trn phi ph hp vi ph hng ngoi i chiu ca
glycerin 85%.
B. Trn 1 ml ch phm vi 0,5 ml acid nitric (TT) v thm 0,5 ml dung
dch kali dicromat 10%, mt vng xanh xut hin b mt phn cch gia hai lp.
yn 10 pht, vng xanh khng phn tn vo lp bn di.
C. un nng 1 ml ch phm vi 2 g kali hydrosulfat (TT) trong mt a
lm bay hi, hi ny c mi hc, lm chy nc mt v lm en giy tm dung
dch kali iodomercurat kim (TT).
D. Ch phm phi p ng php th ch s khc x.

Dung dch S: Pha long 50,0 g ch phm vi nc khng c carbon dioxyd
(TT) va 100 ml.
Dung dch S phi trong (Ph lc 5.12).
Pha long 10 ml dung dch S thnh 25 ml bng nc, dung dch thu c
phi khng mu (Ph lc 5.17, phng php 2).
Gii hn acid - kim
Ly 50 ml dung dch S, thm 0,5 ml dung dch phenolphtalein (CT), dung
dch khng mu. Thm dung dch natri hydroxyd 0,1 N cho n khi c mu hng.
Lng dung dch natri hydroxyd 0,1 N dng khng c qu 0,2 ml. Gi li dung
dch sau cng ny cho php th ester.
Ch s khc x
1,470 - 1,475 (Ph lc 5.7).
Clorid
Ly 1,0 ml dung dch S pha long vi nc thnh 15 ml v tin hnh th.
Dng 1 ml dung dch clorid mu 5 phn triu pha long thnh 15 ml bng nc
chun b mu i chiu.
Sulfat
Ly 10 ml dung dch S pha long thnh 15 ml bng nc th.
Kim loi nng
Pha long 6 ml dung dch S thnh 15 ml bng nc. Ly 12 ml dung dch

thu c th theo phng php 1. Dng dung dch ch mu 1 phn triu chun
b mu i chiu.
Arsen
Ly 1 ml dung dch S th theo phng php A.
St
Ly 2,5 g ch phm th.
Aldehyd v cc cht kh
Ly 7,5 ml dung dch S cho vo bnh nt mi, thm 7,5 ml nc v 1 ml
dung dch pararosanilin kh mu (TT). y np v yn trong mt gi. Mu
ca dung dch khng c m hn mu ca mu i chiu c tin hnh trong
cng iu kin v cng thi gian bng cch dng 7,5 ml dung dch formaldehyd
chun (c cha 5 phn triu CH2O) thay cho dung dch S. Kt qu ch c gi tr
khi mu i chiu c mu hng.
Ester
Thm 10 ml dung dch natri hydroxyd 0,1 M vo dung dch sau cng ca
php th gii hn acid - kim. un si hi lu trong 5 pht. Lm lnh. Thm 0,5
ml dung dch phenolphtalein (CT). Chun bng dung dch acid hydrocloric 0,1
N. Lng dung dch acid hydrocloric 0,1 N dng khng di 8,0 ml.
ng
Ly 10 ml dung dch S, thm 1 ml dung dch acid sulfuric 1 M, un nng
trn cch thu 5 pht. Thm vo 3 ml dung dch natri hydroxyd 2 M (khng c
carbonat) (TT). Trn u v thm tng git dung dch ng (II) sulfat 12,5% mi
pha. Dung dch s c mu xanh, trong sut. Tip tc un trn cch thu trong 5
pht. Mu ca dung dch vn phi xanh v khng c kt ta.
Cc hp cht halogen
Ly 10 ml dung dch S cho vo cc thu tinh 50 ml, thm 1 ml dung dch
natri hydroxyd 2 M (TT), 5 ml nc v 50 mg hp kim nhm - nickel (TT). un
trn cch thu trong 10 pht, lm lnh v lc. Ra cc v phu lc vi nc cho
n khi thu c 25 ml dch lc.
Ly 5 ml dch lc, thm 4 ml ethanol 96% (TT), 2,5 ml nc, 0,5 ml acid
nitric (TT) v 0,05 ml dung dch bc nitrat 1,7% (TT), khuy u. yn trong 2
pht. Dung dch khng c c hn dung dch i chiu c chun b trong
cng iu kin v cng thi gian.
Dung dch i chiu: Ly 7,0 ml dung dch clorid mu 5 phn triu, thm 4
ml ethanol 96% (TT), 0,5 ml nc, 0,5 ml acid nitric (TT) v 0,05 ml dung dch
bc nitrat 1,7% (TT).
Nc
Dng 1,500 g ch phm.
Tro sulfat
Dng 5,0 g ch phm.
nh lng
Ho tan 0,100 g ch phm trong 45 ml nc. Thm chnh xc 25,0 ml dung
dch natri periodat 2,14%. yn ch ti 15 pht, thm 5,0 ml dung dch ethan1,2-diol 50% trong nc. yn ch ti 20 pht v chun bng dung dch
natri hydroxyd 0,1 M, dng 0,5 ml dung dch phenolphtalein (CT) lm ch th.
Song song tin hnh lm mu trng.
1 ml dung dch natri hydroxyd 0,1 M tng ng vi 9,21 mg C3H8O3.
Bo qun
Trong l kn, trnh nh sng.
Ch phm
Dung dch tht trc trng, vin t hu mn.
Tc dng v cng dng
Nhun trng, ht m, dung mi ho tan, t dc.
35-IOD
Iodum
I2
P.t.l: 253,8
Iod phi cha t 99,5 n 100,5% I2.

Tnh cht
Phin nh hoc tinh th mn, mu tm en, c nh kim loi, mi kch ng
c bit. D bay hi nhit thng.
Rt kh tan trong nc, tan trong ethanol 96%, cloroform, kh tan trong
glycerin, d tan trong dung dch ca cc iodid.
nh tnh
A. t nh mt t ch phm trong ng nghim, s bay hi mu tm, hi ny
ngng t thnh nhng mui tinh th mu en nh xanh trn thnh ng.
B. Ly 10 ml dung dch bo ho ch phm, thm 0,5 ml dung dch h tinh
bt (CT), s hin mu lam. Mu s mt khi un nng, ngui mu lam xut hin
tr li.
Dung dch S: Nghin 1,5 g ch phm vi 10 ml nc, lc, ra phu lc

bng nc v pha long dch lc thnh 15 ml bng nc. Thm 0,5 g km bt (TT)
vo dung dch trn. Khi dung dch mt mu, lc v ra phu lc vi nc cho ti
khi thu c 20 ml dch lc.
Clorid v bromid
Khng c qu 0,025%.
Ly 5 ml dung dch S, thm 1,5 ml amoniac (TT) v 3 ml dung dch bc
nitrat 4% (TT). Lc, ra phu vi nc cho n khi thu c 10 ml dch lc, thm
vo 1,5 ml acid nitric (TT) v yn mt pht. Dung dch ny khng c c
hn dung dch i chiu pha ng thi vi dung dch th gm 10,75 ml nc; 0,25
ml dung dch acid hydrocloric 0,01 N; 0,2 ml dung dch acid nitric 13% (TT) v
0,3 ml dung dch bc nitrat 4% (TT).
Cyanid
Ly 5 ml dung dch S, thm 0,2 ml dung dch st (II) sulfat 1,5% (TT) v 1
ml dung dch natri hydroxyd 10% (TT). un nng trong vi pht. Acid ho bng
dung dch acid hydrocloric 10% (TT). Khng c xut hin mu lam hay lc.
Cn khng bay hi
Khng c qu 0,1%.
Cn chnh xc 1,00 g ch phm vo bt s cn b, un trn cch thu cho
n khi iod bay hi ht. Sy cn 100 - 105oC n khi lng khng i. Cn,
khi lng cn cn li khng c qu 1 mg.
nh lng
Trong mt bnh nn nt mi, ho tan 0,200 g ch phm trong 5 ml dung
dch kali iodid 20% (TT) v 1 ml dung dch acid acetic 2 M. Khi ch phm tan ht,
thm 50 ml nc. Chun bng dung dch natri thiosulfat 0,1 N, thm 1 ml dung
dch h tinh bt (CT) vo lc cui nh lng.
1 ml dung dch natri thiosulfat 0,1 N tng ng vi 12,69 mg iod.

Bo qun
Bng B, ng trong l thu tinh mu, c nt thy tinh kn, ni mt.
Cng dng
St khun.
Ch phm
Dung dch iod 1%, cn iod 1%, cn iod 5%.
36- ISONIAZID
Isoniazidum
C6H7N3O
P.t.l: 137,14
Isoniazid l 4 - pyridin carboxylic acid hydrazid, phi cha t 98,0 n

101,0% C6H7N3O, tnh theo ch phm lm kh.
Tnh cht
Bt kt tinh trng hay tinh th khng mu, khng mi.
D tan trong nc, hi tan trong ethanol 96%, kh tan trong cloroform, rt
kh tan trong ether.
nh tnh
Nhm I: B v C.
Nhm II: A v C.

ngoi ca isoniazid chun hoc ph hng ngoi i chiu ca isoniazid.
B. Ho tan 0,1 g ch phm trong 2 ml nc, thm dung dch nng ca 0,10
g vanilin (TT) trong 10 ml nc, yn v c thnh ng nghim bng mt a
thu tinh, s c ta vng, ta ny sau khi kt tinh li bng 5 ml ethanol 70% v sy
kh 100 - 105oC, c im chy t 226 - 231oC (Ph lc 5.19).
C. im chy: 170 - 174oC (Ph lc 5.19).
(TT) v pha long n 50 ml bng cng dung mi.
Dung dch S phi trong (Ph lc 5.12) v khng c c mu m hn mu
pH
Hydrazin v tp cht lin quan
Dung mi khai trin: Nc - aceton - methanol - ethyl acetat (10: 20: 20:
50).
Dung dch th: Ho tan 1,0 g ch phm trong hn hp ng th tch aceton
(TT) v nc c 10,0 ml.
Dung dch i chiu: Ho tan 50,0 mg hydrazin sulfat trong 50 ml nc v
thm aceton (TT) va 100,0 ml. Ly 10,0 ml dung dch ny, thm 0,2 ml dung
dch th v pha long thnh 100,0 ml bng hn hp ng th tch aceton (TT) v
nc.
Trin khai bn mng n khi dung mi i c 15 cm. kh bn mng trong
khng kh v quan st di nh sng t ngoi bc sng 254 nm. Bt k vt ph
no ngoi vt chnh ca dung dch th khng c m mu hn vt ca dung
dch i chiu (0,2%). Phun bn mng bng dung dch dimethylamino
benzaldehyd (TT1). Quan st di nh sng ban ngy. Dung dch i chiu xut
hin thm vt tng ng vi hydrazin. Vt tng ng vi hydrazin ca dung dch
th khng c m mu hn vt tng ng vi hydrazin ca dung dch i chiu
(0,05%).
Kim loi nng
Mt khi lng do lm kh
Khng c qu 0,5% (Ph lc 5.16).
(1,000 g; 100 - 105oC).
Tro sulfat
Dng 1,0 g ch phm.
nh lng
Cn chnh xc khong 0,250 g ch phm, ho tan trong nc va 100,0
ml. Ly 20,0 ml dung dch trn, thm vo 100 ml nc, 20 ml acid hydrocloric
(TT), 0,2 g kali bromid (TT) v 0,05 ml dung dch methyl (CT). nh lng t
t bng dung dch kali bromat 0,1 N, lc lin tc cho ti khi mu bin mt.
Song song tin hnh mu trng trong cng iu kin nh trn.
1 ml dung dch kali bromat 0,1 N tng ng vi 3,429 mg C6H7N3O.
Bo qun
Trong l thu tinh nt kn, trnh nh sng.
Cng dng
Phng v phi hp vi cc thuc khc iu tr lao.
Ch phm
Vin rimifon 150 mg, nang isoniazid thuc tim, siro.
37-KALI CLORID
Kalii chloridum
KCl
P.t.l: 74,6
Kali clorid phi cha t 99,0 n 100,5% KCl, tnh theo ch phm lm
kh.
Tnh cht
Tinh th khng mu hoc bt kt tinh trng, khng mi.
D tan trong nc, thc t khng tan trong ethanol.
nh tnh
(TT) v pha long va 100 ml.
Dung dch S cho cc phn ng c trng ca ion kali v clorid (Ph lc
7.1).
php 2).
Gii hn acid - kim
Ly 50,0 ml dung dch S, thm 0,1 ml dung dch xanh bromothymol (CT).
Dung dch phi chuyn mu khi thm khng qu 0,5 ml dung dch natri hydroxyd
0,01 N hoc 0,5 ml dung dch acid hydrocloric 0,01 N.
Sulfat
Khng c qu 0,03% (Ph lc 7.4.12).
Ly 5 ml dung dch S, thm nc va 15 ml v tin hnh th.
Iodid
Lm m 5,0 g ch phm bng cch thm tng git hn hp va mi pha
gm 25 ml dung dch h tinh bt khng c iodid (CT), 2,0 ml dung dch acid
sulfuric 0,5 M, 0,15 ml dung dch natri nitrit 10% v 25 ml nc. Sau 5 pht, quan
st di nh sng thng: Hn hp th nghim khng c c bt k tiu phn
hoc vt mu xanh no xut hin.
Bromid
Khng c qu 0,1%.
Pha long 1,0 ml dung dch S thnh 50 ml bng nc. Thm vo 5,0 ml
dung dch ny 2,0 ml dung dch phenol (CT) v 1,0 ml dung dch cloramin T
0,02%, trn u ngay. Sau ng 2 pht, thm 0,15 ml dung dch natri thiosulfat
0,1 M, trn u v pha long thnh 10,0 ml bng nc. hp th (Ph lc 3.1)
ca dung dch ny bc sng 590 nm, dng nc lm mu trng, khng c
ln hn hp th ca dung dch c chun b trong cng iu kin v cng thi
gian nhng thay 5,0 ml dung dch th bng 5,0 ml dung dch kali bromid chun
cha 3,0 mg/ ml.
Bari
Ly 5,0 ml dung dch S, thm vo 5,0 ml nc v 1,0 ml dung dch acid
sulfuric 1 M. Sau 15 pht, dung dch th khng c c hn mt hn hp gm
5,0 ml dung dch S v 6,0 ml nc.
Kim loi nng

Ly 12,0 ml dung dch S v tin hnh th theo phng php 1. Dng dung
St
Ly 5,0 ml dung dch S, thm nc va 10 ml v tin hnh th.
Magnesi v cc kim loi kim th
Khng c qu 0,02% (tnh theo calci) (Ph lc 7.4.14).
Dng 10,0 g ch phm th. Th tch dung dch natri edetat 0,01 M
dng khng c qu 5,0 ml.
Mt khi lng do lm kh
Khng c qu 1,0% (Ph lc 5.16).
(1,000 g; 100 - 105oC; 3 gi).
nh lng
Cn 1,300 g ch phm, ho tan vi nc v pha long thnh 100,0 ml. Ly
chnh xc 10,0 ml dung dch trn cho vo bnh nn, thm 50 ml nc, 5 ml dung
dch acid nitric 12,5% (TT), 25,0 ml dung dch bc nitrat 0,1 N v 2 ml dung dch
dibutylphtalat (hoc nitrobenzen) (TT). Lc u v chun bng dung dch
amoni thiocyanat 0,1 N. Dng 2 ml dung dch st (III) amoni sulfat 10% lm ch
th.
1 ml dung dch bc nitrat 0,1 N tng ng vi 7,46 mg KCl.
i vi ch phm d nh dng pha cc dung dch thm phn v cc dung
dch thuc tim, ngoi cc yu cu trn phi t yu cu v natri v nhm.
Natri
Khng c qu 0,1%.
Xc nh bng phng php quang ph pht x nguyn t (Ph lc 3.4,
phng php 1).
Dung dch th: Ho tan 1,00 g ch phm trong nc va 100,0 ml.
Dung dch chun: Ho tan trong nc 0,5084 g natri clorid c sy
100 - 105oC trong 3 gi v thm nc va 1000,0 ml (200 g Na/ ml), pha
long tip theo yu cu.
o cng pht x 589 nm.
Nhm
Dung dch th: Ho tan 4,0 g ch phm trong 100 ml nc, thm 10 ml
Dung dch i chiu: Trn ln 2,0 ml dung dch nhm mu 2 phn triu (2
g/ ml) vi 10 ml dung dch m acetat pH 6,0 v 98 ml nc.
Dung dch mu trng: Trn ln 10 ml dung dch m acetat pH 6,0 v 100
ml nc.
Bo qun
ng trong l nt kn ni kh ro, trnh nh sng.
Cng dng
B sung cht in gii.
Ch phm
Dung dch tim kali clorid; Dch truyn dextrose kali clorid v natri clorid;
Dch truyn dextrose v kali clorid; Hn hp mui pha dung dch ung b cht
in gii. Vin kali clorid tc dng ko di.
38-KALI IODID
Kalii iodidum
KI
P.t.l: 166,0
Kali iodid phi cha t 99,0 n 100,5% KI, tnh theo ch phm lm
kh.
Tnh cht
Tinh th khng mu hay bt kt tinh trng, khng mi, d chy khi tip xc
vi khng kh m.
Rt d tan trong nc, d tan trong glycerin, tan trong ethanol 96%.
nh tnh
(TT) v pha long va 100 ml.
Dung dch S cho phn ng c trng ca ion kali v iodid (Ph lc 7.1).
php 2).
Gii hn kim
Ly 10 ml dung dch S, thm 0,1 ml dung dch acid sulfuric 0,1 N v 1 git
dung dch phenolphtalein (CT), dung dch khng c c mu.
Iodat
Ly 10 ml dung dch S, thm 0,25 ml dung dch h tinh bt khng c iodid

(CT) v 0,2 ml dung dch acid sulfuric 10% (TT). yn trong ti 2 pht, hn hp
khng c c mu xanh lam.
Sulfat
Khng c qu 0,015% (Ph lc 7.4.12).
Ly 10 ml dung dch S pha long vi nc va 15 ml v tin hnh th.
Thiosulfat
Thm 0,1 ml dung dch h tinh bt (CT) v 0,1 ml dung dch iod 0,005 M
vo 10 ml dung dch S, mu xanh to thnh.
Kim loi nng
St
Mt khi lng do lm kh
Khng c qu 1,0% (Ph lc 5.16).
(1,000 g; 100 - 105oC; 3 gi).
nh lng
Ho tan 1,000 g ch phm trong nc v pha long va 100,0 ml. Ly
chnh xc 10,0 ml dung dch trn, thm 20 ml acid hydrocloric (TT) v 5,0 ml
cloroform (TT). Lc u v chun bng dung dch kali iodat 0,1 N cho ti khi
mu tm ca iod xut hin trong lp cloroform. Tip tc thm tng git dung
dch kali iodat 0,1 N v lc u hn hp cho n khi lp cloroform mt mu.

yn hn hp trong 5 pht, nu lp cloroform c mu tm, tip tc chun vi
dung dch kali iodat 0,1 N.
1 ml dung dch kali iodat 0,1 N tng ng vi 5,533 mg KI.
Bo qun
ng trong l kn, trnh nh sng.
Cng dng
Cht khng gip, khng nm, b sung iod, long m.
Ch phm
Dung dch ung kali iodid.
39-KALI PERMANGANAT
Kalii permanganas
KMnO4
P.t.l: 158,03
Kali permanganat phi cha t 99,0 n 100,5% KMnO4.

Tnh cht
Tinh th hnh lng tr mu tm sm hoc gn nh en, hoc bt dng ht,
mu tm sm hoc en nu, thng c nh kim, khng mi.
D b phn hu v gy n khi tip xc vi mt s cht hu c v cht d b
oxy ho. Tan trong nc lnh, d tan trong nc si.
Cn thn trng khi tin hnh th nghim vi kali permanganat v khi tip
xc trc tip cht ny vi mt s cht hu c hoc cht d b oxy ho khc n c
th gy n ngay c trng thi lng hoc rn.
nh tnh
A- Ho tan 0,05 g ch phm trong 5 ml dung dch acid sulfuric 10% (TT).
Thm dung dch hydrogen peroxyd long (TT) vo t t, dung dch th b mt
mu v c bt kh bay ln.
B- Ho tan 0,1 g ch phm trong 4 ml nc, thm 1 ml ethanol 96% (TT).
un si n khi dung dch mt mu. Lc. Dch lc cho phn ng c trng ca ion
kali (Ph lc 7.1).
Mu sc ca dung dch
Dung dch S: Ho tan 0,75 g ch phm trong 25 ml nc, thm 3 ml ethanol
96% (TT) v un si t 2 n 3 pht. ngui, thm nc va 30 ml v lc.
Dung dch S phi khng mu (Ph lc 5.17, Phng php 2).
Clorid
Khng c qu 0,02% (Ph lc 7.4.5).
Sulfat
Khng c qu 0,05% (Ph lc 7.4.12).
Ly 12 ml dung dch S pha long vi nc thnh 15 ml v tin hnh th.
Cc cht khng tan trong nc
Khng c qu 1,0%.
Ho tan 0,5 g ch phm trong 50 ml nc. un si, lc qua phu thu tinh
xp cn b trc (phu c c trung bnh). Ra cn trn phu cho n khi nc
ra khng mu. Sy cn nhit 100 - 105oC cho n khi lng khng i.
Khi lng cn cn li khng c qu 5 mg.
nh lng
Cn chnh xc khong 0,300 g ch phm, ho tan v pha long va 100
ml vi nc trong bnh nh mc. Ly 20,0 ml dung dch ny cho vo bnh nn c
nt mi, thm 20 ml nc, 1 g kali iodid (TT) v 10 ml dung dch acid hydrocloric
long (TT). Chun iod gii phng ra bng dung dch natri thiosulfat 0,1 N,
dng 1 ml dung dch h tinh bt (CT) lm ch th v c cho vo khi hn hp
nh lng nht mu.
1 ml dung dch natri thiosulfat 0,1 N tng ng vi 3,16 mg KMnO4.
Bo qun
Tc dng v cng dng
Cht st trng.
40-KAOLIN NANG
Kaolinum ponderosum
Kaolin nng l nhm silicat thin nhin ngm nc c loi tp cht,
c thnh phn khng n nh.
Tnh cht
Bt mn trng hoc trng ng, s c cm gic trn. Thc t khng tan trong
nc v cc dung mi hu c.
nh tnh
A. Thm 1 g kali nitrat (TT) v 3 g natri carbonat (TT) vo 0,5 g ch phm
trong chn kim loi v un nng cho n khi hn hp chy. ngui, thm vo
hn hp 20 ml nc si, trn u v lc. Ra cn vi 50 ml nc. Thm vo cn 1
ml acid hydrocloric (TT) v 5 ml nc. Lc, thm vo dch lc 1 ml dung dch
natri hydroxyd 42% v lc. Thm vo dch lc 3 ml dung dch amoni clorid
10,7%, ta keo trng xut hin.
B. Thm 2,0 g ch phm c chia thnh 20 phn vo 100 ml dung dch
natri lauryl sulfat 1,0% trong mt ng ong chia vch 100 ml c ng knh 30
mm. Sp xp th t thm vo sao cho khong cch gia cc ln thm vo ca mi

phn cch nhau 2 pht. yn 2 gi. Th tch quan st c ca phn cn lng
xung khng c ln hn 5 ml.
C. Ly 0,25 g ch phm th phn ng ca silicat (Ph lc 7.1).
Gii hn acid - kim
Thm 20 ml nc khng c carbon dioxyd (TT) vo 1,0 g ch phm, lc
trong 2 pht v lc. Thm vo 10 ml dch lc 0,1 ml dung dch phenolphtalein
(CT). Dung dch phi khng mu v phi chuyn sang mu hng khi thm khng
qu 0,25 ml dung dch natri hydroxyd 0,01 N.
Tp cht hu c
Nung n 0,3 g ch phm trong chn nung. Cn ch c php hi c
mu so vi ch phm ban u.
Kh nng hp ph
Thm 10,0 ml dung dch xanh methylen 0,37% vo 1,0 g ch phm trong
ng nghim c nt mi v lc trong 2 pht. lng. Ly tm v pha long dung
dch ny theo t l 1 thnh 100 bng nc. Dung dch thu c c mu khng
c m hn mu ca dung dch xanh methylen 0,003%.
Kh nng trng n
Nghin 2,0 g ch phm vi 2 ml nc. Hn hp thu c khng c chy.
Cc cht tan trong acid v c
Khng c qu 1,0%.
Thm 7,5 ml dung dch acid hydrocloric long (TT) v 27,5 ml nc vo
5,0 g ch phm, un si trong 5 pht v lc. Ra cn trn phu lc bng nc. Pha
long bng nc ton b dch lc v nc ra thnh 50,0 ml (gi mt phn dung
dch ny dng th kim loi nng). Thm 1,5 ml dung dch acid sulfuric 1 M
(TT) vo 10,0 ml dung dch trn. Bc hi trn cch thu n kh v nung. Khi
lng ca cn khng c qu 10 mg.
Clorid
Khng c qu 0,025% (Ph lc 7.4.5).
Dung dch S: Thm mt hn hp gm 6 ml acid acetic (TT) v 34 ml nc
vo 4 g ch phm. Lc trong mt pht v lc.
Ly 2 ml dung dch S pha long thnh 15 ml v tin hnh th.
Sulfat
Khng c qu 0,1% (Ph lc 7.4.12).
Ly 1,5 ml dung dch S pha long thnh 15 ml v tin hnh th.
Calci
Khng c qu 0,025% (Ph lc 7.4.3).
Ly 4 ml dung dch S pha long thnh 15 ml v tin hnh th.
Kim loi nng
Thm 5 ml nc, 10 ml acid hydrocloric (TT) v 25 ml methyl isobutyl
keton (TT) vo 5 ml dung dch c chun b th cc cht tan trong acid v c.
Lc trong 2 pht. yn cho tch lp. Bc hi lp nc n kh trn cch thu.
Ho tan cn trong 1 ml acid acetic (TT) v pha long thnh 25 ml bng nc, lc.
Ly 12 ml dch lc tin hnh th theo phng php 1. Dng dung dch ch mu 1
phn triu chun b mu i chiu.
nhim khun
Tng s vi khun hiu kh c th sng li c khng c qu 1000 trn
mt gam ch phm. Xc nh bng phng php a thch (Ph lc 10.7).
Khi kaolin nng c d nh dng sn xut cc thuc s dng bn

trong c th th phi p ng yu cu php th kim loi nng di y:
Kim loi nng
Thm 10 ml nc, 20 ml acid hydrocloric (TT) v 25 ml methyl isobutyl
keton (TT) vo 10 ml dung dch c chun b th cc cht tan trong acid v
c. Lc trong 2 pht. yn cho tch lp. Bc hi lp nc n kh trn cch
thu. Ho tan cn trong 1 ml acid acetic (TT) v pha long thnh 25 ml bng nc,
lc. Ly 12 ml dch lc tin hnh th theo phng php 1. Dng dung dch ch
Bo qun
Trong bao b kn.
Ch phm
Thuc p.
Nhn
Phi ghi r kh nng s dng ca ch phm, v d nh ch phm c ph
hp cho mc ch sn xut cc thuc dng bn trong c th khng.
41-KAOLIN NHE
Kaolinum leve
Kaolin nh l nhm silicat thin nhin ngm nc c loi hu ht cc
tp cht bng cch gn lc v sy kh. C cha tc nhn phn tn thch hp.
Tnh cht
Bt trng nh, khng c cc ht ct sn, khng mi hoc gn nh khng
mi, s c cm gic trn. Thc t khng tan trong nc v cc acid v c.
nh tnh
A. un chy 1 g ch phm vi 2 g natri carbonat khan (TT), lm m hn

hp vi 10 ml nc, lc v ra phu lc vi 5 ml nc (gi li cn th php
th sau). Tp hp dch lc v nc ra, sau thm 3 ml acid hydrocloric (TT) s
xut hin ta keo trng.
B. Ho tan cn gi li php th A trong 10 ml acid hydrocloric (TT).

Dung dch thu c phi cho phn ng c trng ca nhm (Ph lc 7.1).
C. Nghin 2 g ch phm vi 2 ml nc. Hn hp thu c s chy.
Tiu phn th
Chuyn 5 g ch phm vo ng ong c nt mi kch thc 16 cm x 35 mm,
thm 60 ml dung dch natri pyrophosphat 1%, lc k v yn 5 pht. Dng pipet
ht 50 ml v tr di b mt cht lng khong 5 cm. Thm 50 ml nc vo phn
cht lng cn li, lc v yn 5 pht, tin hnh ht 50 ml cht lng ging nh
trn. Nhc li thao tc ny trong cng iu kin nh trn n khi ht c tng s
hn dch l 400 ml. Chuyn phn cn li trong ng ong vo cc v bc hi n
kh trn cch thu. Cn thu c sau khi sy n khi lng khng i 105oC
khng c qu 25 mg.
Tiu phn mn
Phn tn 5 g ch phm trong 250 ml nc bng cch lc mnh trong 2 pht
trong bnh nn c nt mi, rt ngay vo ng ong thu tinh c ng knh 5 cm,
ng thi chuyn 20 ml hn dch trn bng pipet vo cc thu tinh v bc hi n
kh, sy n khi lng khng i 105oC. Phn cn li trong ng ong yn
trong 4 gi 20oC. Ht 20 ml hn dch bng pipet v tr di b mt cht lng
ng 5 cm v khng c lm c, chuyn vo cc thu tinh v bc hi n kh,
sy n khi lng khng i 105oC. Khi lng cn ca ln ht sau khng
c nh hn 70% khi lng cn ca ln ht trc.
Arsen

Ly 0,50 g ch phm, thm 25 ml nc v tin hnh th theo phng php
A.
Kim loi nng
un nng trn cch thu 6,0 g ch phm trong 15 pht di ng sinh hn
ngc vi hn hp gm 70 ml nc v 10 ml acid hydrocloric (TT), lc. Thm 0,5
ml acid nitric (TT) vo 40 ml dch lc v bc hi n khi c khi cn nho, sau
thm 20 ml nc, 2 g amoni clorid (TT), 2 g amoni thiocyanat (TT) v chit 2
ln, mi ln vi 10 ml hn hp ng th tch alcol amyl v ether. Thm vo lp
nc 2 g acid citric (TT) v nc va 60 ml. Ly 12 ml dung dch ny tin
mu i chiu.
Clorid
Khng c qu 0,033% (Ph lc 7.4.5).
un si 1,0 g ch phm vi 80 ml nc v 20 ml dung dch acid nitric 2 M
(TT) di ng sinh hn ngc trong 5 pht, ngui v lc. Ly 15 ml dch lc
tin hnh th.
Mt khi lng do lm kh
Khng c qu 1,5% (Ph lc 5.16).
(1,000 g; 105oC).
Mt khi lng do nung
Khng c qu 15,0%.
Nung 1,0 g ch phm 600oC n khi lng khng i.
Cht ho tan
un si 2 g ch phm trong 100 ml dung dch acid hydrocloric 0,2 M di

ng sinh hn ngc trong 5 pht, ngui v lc. Bc hi 50 ml dch lc n kh.
Cn thu c sau khi nung 600oC trong 30 pht, khng c qu 10 mg.
Bo qun
Trong bao b kn.
Ch phm
Hn hp kaolin, hn hp kaolin v morphin.
Tc dng
Chng a chy.
Ghi ch: Khi kaolin hoc kaolin nh c k n hoc yu cu th cp pht
kaolin nh, tr khi bit chc chn kaolin nh (thin nhin) c yu cu.
42-KAOLIN NH THIN NHIN
Kaolinum leve naturale
Kaolin nh (thin nhin) l nhm silicat thin nhin ngm nc c
loi hu ht cc tp cht bng cch gn lc v sy kh. Khng cha tc nhn phn
tn.
Tnh cht
Bt trng nh, khng c cc ht ct sn, khng mi hoc gn nh khng
mi, s c cm gic trn. Thc t khng tan trong nc v cc acid v c.
nh tnh
Php th A, B c tin hnh theo chuyn lun "Kaolin nh".
C. Nghin 2 g ch phm vi 2 ml nc. Hn hp thu c khng c
chy.
Tiu phn th, arsen, kim loi nng, clorid, mt khi lng do lm kh, mt
khi lng do nung v cht ho tan
c tin hnh th v phi p ng yu cu nh trong chuyn lun kaolin
nh.
Tiu phn mn
Phn tn 5 g ch phm trong 250 ml nc c cha 50 mg natri
pyrophosphat (TT) bng cch lc mnh trong 2 pht trong bnh nn c nt mi, rt
ngay vo ng ong thu tinh c ng knh 5 cm, ng thi chuyn 20 ml hn
dch trn bng pipet vo cc thu tinh v bc hi n kh, sy n khi lng
khng i 105oC. Phn cn li trong ng ong yn trong 4 gi 20oC. Ht
20 ml hn dch bng pipet v tr di b mt cht lng ng 5 cm v khng c
lm c, chuyn vo cc thu tinh v bc hi n kh, sy n khi lng khng
i 105oC. Khi lng cn ca ln ht sau khng c nh hn 70% khi lng
cn ca ln ht trc.
Bo qun
Trong bao b kn.
Ch phm
Hn hp kaolin, hn hp kaolin v morphin.
Tc dng
Chng a chy.
Ghi ch: Khi kaolin hoc kaolin nh c k n hoc yu cu th cp pht
kaolin nh, tr khi bit chc chn kaolin nh (thin nhin) c yu cu.
43-NATRI BENZOAT
Natrii benzoas
C7H5NaO2 P.t.l: 144,1

Natri benzoat l natri benzencarboxylat, phi cha t 99,0 n 100,5%
C7H5NaO2, tnh theo ch phm lm kh.
Tnh cht
Bt kt tinh hay ht hoc mnh mu trng. Hi ht m, d tan trong nc,
hi tan trong ethanol 90% (tt/tt).
nh tnh
A. Phi cho phn ng nh tnh B v C ca ion benzoat (Ph lc 7.1).
B. Phi cho phn ng nh tnh ca ion natri (Ph lc 7.1).
(TT) v pha long cho va 100 ml vi cng dung mi.
Gii hn acid - kim
Thm 10 ml nc khng c carbon dioxyd (TT) v 0,2 ml dung dch
phenolphtalein (CT) vo 10 ml dung dch S. Dung dch phi chuyn mu khi thm
khng c qu 0,2 ml dung dch natri hydroxyd 0,1 N hoc dung dch acid
hydrocloric 0,1 N.
Hp cht halogen
Tt c cc dng c thu tinh c dng phi khng c clorid v phi c
chun b bng cch ngm qua m trong dung dch acid nitric 50% (TT), c ra
sch v ngm trong nc. Phi c ch dn rng dng c thu tinh c dng cho
php th ny.
Dung dch th: Ly 20,0 ml dung dch S, thm 5 ml nc, pha long n
50,0 ml bng ethanol 96% (TT).
Xc nh clor b ion ho:
Khng c qu 0,02%.
Trong 3 bnh nh mc 25 ml, chun b cc dung dch sau:
Dung dch (1): Thm vo 4,0 ml dung dch th, 3 ml dung dch natri
hydroxyd long (TT) v 3 ml ethanol 96% (TT). Dung dch ny c dng
chun b dung dch A.
Dung dch (2): Thm vo 3 ml dung dch natri hydroxyd long (TT), 2 ml
nc v 5 ml ethanol 96% (TT). Dung dch ny c dng chun b dung dch
B.
Dung dch (3): Thm vo 4,0 ml dung dch clorid mu 8 phn triu, 6,0 ml
nc. Dung dch ny dng chun b dung dch C.
Trong bnh nh mc 25 ml th t cho vo 10,0 ml nc. Thm vo mi
bnh 5 ml dung dch st (III) amoni sulfat (CT), trn u v thm tng git, va
thm va lc, 2 ml acid nitric (TT) v 5 ml dung dch thu ngn (II) thiocyanat
(TT). Lc. Pha long dung dch trong mi bnh n 25,0 ml bng nc v cc
bnh trong chu nc 20oC trong 15 pht. o hp th ca dung dch A
bc sng 460 nm trong cc o 2 cm, ly dung dch B lm mu trng v ca dung
dch C dng dung dch trong bnh cha 10 ml nc lm mu trng. hp th ca
dung dch A khng c ln hn hp th ca dung dch C.
Xc nh clor ton phn:
Khng c qu 0,03%.
Dung dch (1): Thm 7,5 ml dung dch natri hydroxyd long (TT) v 0,125
g hp kim nhm nickel (TT) vo 10 ml dung dch th. un nng trn ni cch
thu 10 pht. ngui n nhit phng, lc vo bnh nh mc c dung tch 25
ml v ra phu lc 3 ln, mi ln vi 2 ml ethanol 96% (TT) (ta nh c th hnh

thnh ri bin mt khi acid ho). Pha long dch lc v nc ra thnh 25,0 ml
bng nc. Dung dch ny c dng chun b dung dch A.
Dung dch (2): Chun b nh dung dch (1), nhng thay 10,0 ml dung dch
th bng 10,0 ml hn hp ng th tch ethanol 96% (TT) v nc. Dung dch ny
dng chun b dung dch B.
Dung dch (3): Thm 4,0 ml nc vo 6,0 ml dung dch clorid mu 8 phn
triu. Dung dch ny dng chun b dung dch C.
Thm ring bit ln lt vo 4 bnh nh mc c dung tch 25 ml: 10 ml
dung dch (1), 10 ml dung dch (2), 10 ml dung dch (3) v 10 ml nc.
Thm vo mi bnh 5 ml dung dch st (III) amoni sulfat (CT), trn u v
thm tng git, va thm va lc 2 ml acid nitric (TT) v 5 ml dung dch thu
ngn (II) thiocyanat (TT), lc. Pha long dung dch trong mi bnh n 25 ml bng
nc v cc bnh trong chu nc 20oC trong 15 pht. o hp th (Ph
lc 3.1) bc sng 460 nm, trong cc o 2 cm ca dung dch A, dng dung dch
B lm mu trng v ca dung dch C, dng dung dch cha 10 ml nc lm mu
trng. hp th ca dung dch A khng c ln hn hp th ca dung dch
C.
Kim loi nng
Ly 2,0 g ch phm tin hnh th theo phng php 3. Dng 2 ml dung
Mt khi lng do lm kh
Khng c qu 2,0% (Ph lc 5.16).
(1,000 g; 100 - 105oC).
nh lng
Ho tan 0,250 g ch phm trong acid acetic khan (TT), lm nng n 50oC
(nu cn thit). ngui, dng 0,05 ml dung dch naphtholbenzein (CT) lm ch
th. Chun bng dung dch acid percloric 0,1 N n khi mu xanh lc xut hin.
C7H5NaO2.
Bo qun
Trong l kn.
44-NATRI BROMID
Natrii bromidum
NaBr P.t.l: 102,9
Natri bromid phi cha t 98,0 n 100,5% NaBr, tnh theo ch phm
lm kh.
Tnh cht
Bt cm mu trng hoc tinh th m c hay trong sut khng mu, hi ht
m. D tan trong nc, tan trong ethanol 96%.
nh tnh
A. Ch phm phi cho phn ng ca ion bromid (Ph lc 7.1).
B. Dung dch S phi cho phn ng ca ion natri (Ph lc 7.1).
(TT) va 100 ml.
php 2).
Gii hn acid - kim
Thm 0,1 ml dung dch xanh bromothymol (CT) vo 10 ml dung dch S.

Dung dch phi chuyn mu khi thm khng c qu 0,5 ml dung dch acid
hydrocloric 0,01 N hoc dung dch natri hydroxyd 0,01 N.
Bromat
Thm 1 ml dung dch h tinh bt (CT), 0,1 ml dung dch kali iodid 10%
(TT) v 0,25 ml dung dch acid sulfuric 0,5 M vo 10 ml dung dch S. yn ch
ti trong 5 pht. Khng c c mu xanh hoc tm xut hin.
Clorid
Khng c qu 0,6%.
Trong bnh nn, ho tan 1,000 g ch phm trong 20 ml acid nitric long
(TT). Thm 5 ml nc oxy gi m c (TT) v un nng trn cch thu n khi
dung dch mt mu hon ton. Ra thnh bnh bng mt t nc v lm nng trn
cch thu tip trong 15 pht. ngui, pha long n 50 ml bng nc v thm
5,0 ml dung dch bc nitrat 0,1 M v 1 ml dibutylphtalat (TT). Lc v chun
bng dung dch amoni thiocyanat 0,1 M, dng 5 ml dung dch st (III) amoni
sulfat 10% lm ch th. Th tch dung dch bc nitrat 0,1 M dng khng c
ln hn 1,7 ml.
Iodid
Thm 0,15 ml dung dch st (III) clorid 10,5% v 2 ml cloroform (TT) vo
5 ml dung dch S. Lc v tch lp. Lp cloroform khng c c mu (Ph lc
5.17. phng php 1).
Sulfat
Khng c qu 0,01% (Ph lc 7.4.12).
Bari
Thm 5 ml nc v 1 ml dung dch acid sulfuric 1 M vo 5 ml dung dch S.

Sau 15 pht, dung dch khng c c hn hn hp gm 5 ml dung dch S v 6
ml nc.
Kim loi nng
Ly 12 ml dung dch S th theo phng php 1. Dng dung dch ch mu 1
phn triu lm mu i chiu.
St
Ly 5 ml dung dch S pha long thnh 10 ml bng nc th.
Khng c qu 0,02% tnh theo Ca (Ph lc 7.4.14).
Ly 10,0 g ch phm tin hnh th. Th tch ca dung dch natri edetat 0,01
M dng khng uc qu 5,0 ml.
Mt khi lng do lm kh
Khng c qu 3,0% (Ph lc 5.16).
(1,000 g; 100 - 105oC; 3 gi).
nh lng
Ho tan 2,000 g ch phm trong nc v pha long n 100,0 ml bng cng
dung mi. Thm vo 10,0 ml dung dch trn 50 ml nc v 5 ml acid nitric long
(TT), 25,0 ml dung dch bc nitrat 0,1 M v 2 ml dibutylphtalat (TT). Lc, chun
bng dung dch amoni thiocyanat 0,1 M, dng 2 ml dung dch st (III) amoni
sulfat 10% lm ch th v lc mnh cho ti kt thc php nh lng. Cn hiu
chnh i vi lng clorid c mt, c xc nh mc clorid.
1 ml dung dch bc nitrat 0,1 M tng ng vi 10,29 mg NaBr.
Bo qun
45-NATRI CALCI EDETAT
Natrii calcii edetas
C10H12CaN2Na2O8. xH2O
P.t.l: 374,3
Natri calci edetat l dinatri [(ethylendinitrilo) tetra - acetato] calciat (2-) c

cha mt lng khng xc nh nc kt tinh, phi cha t 98,0 n 102,0%
C10H12CaN2Na2O8, tnh theo ch phm khan.
Tnh cht
Bt trng hoc hu nh trng, d ht m. D tan trong nc, thc t khng
tan trong ethanol 96% v ether.
nh tnh
ngoi ca natri calci edetat chun.
B. Ho tan 2 g ch phm trong 10 ml nc, thm 6 ml dung dch ch nitrat
(TT), lc v thm 3 ml dung dch kali iodid (TT), khng c c ta mu vng
xut hin. Kim ho dung dch trn bng cch thm dung dch amoniac 2 M (TT),
dng giy qu lm ch th v thm 3 ml dung dch amoni oxalat 4% (TT), s c
ta trng.
C. Ho tan 0,5 g ch phm trong 10 ml nc. Kim ha dung dch bng
cch thm dung dch amoniac 2 M (TT), dng giy qu lm ch th v thm 3
ml dung dch amoni oxalat 4% (TT). Ti a ch c ta nh hnh thnh.
D. Nung ch phm. Cn cho phn ng c trng ca ion calci v ion natri

(Ph lc 7.1).
Dung dch S: Ho tan 5,0 g ch phm trong nc v thm nc va 100
ml.
php 2).
pH
Ho tan 5,0 g ch phm trong nc khng c carbon dioxyd (TT) v thm
va 25 ml bng cng dung mi trn. pH ca dung dch t 6,5 n 8,0 (Ph lc
5.9).
Dinatri edetat
Khng c qu 1,0%.
Ho tan 5,0 g ch phm trong 250 ml nc. Thm 10 ml dung dch m
amoniac pH 10,0 v khong 50 mg hn hp en eriocrom T (CT). Lng dung
dch magnesi clorid 0,1 M khng c qu 1,5 ml lm thay i mu ca ch th
thnh mu tm.
Clorid
Khng c qu 0,1% (Ph lc 7.4.5).
Thm 30 ml acid nitric long (TT) vo 20 ml dung dch S, yn 30 pht
v lc. Ly 2,5 ml dch lc pha long vi nc thnh 15 ml tin hnh th.
Kim loi nng
St
Thm 0,25 g calci clorid (TT) vo mi ng trc khi thm acid mercaptoacetic
(TT).
Nc
T 5,0 n 13,0% (Ph lc 6.6).
nh lng
Ho tan 0,500 g ch phm trong 300 ml nc, thm 2 g
hexamethylentetramin (TT) v 2 ml dung dch acid hydrocloric long (TT). Chun
bng dung dch ch nitrat 0,1 M, dng khong 50 mg hn hp da cam xylenol
(CT) lm ch th.
1 ml dung dch ch nitrat 0,1 M tng ng vi 37,43 mg
C10H12CaN2Na2O8.
Bo qun
Trong l nt kn.
46-NATRI CAMPHOSULFONAT
Natrii camphosulfonas
C10H15O4SNa
P.t.l: 254,3
Natri camphosulfonat l mui natri ca acid 10 - camphosulfonic (acid 7,7 dimethyl - 2 - oxobicyclo - [2.2.1] heptan - 1 - methansulfonic), thu c bng
cch iu ch t camphor (thin nhin hay tng hp) vi acid sulfuric m c v
anhydrid acetic.
Tnh cht
Bt kt tinh trng, c mi long no nh, v hi ng. D b ht m, vn cc,
i mu vng.
Rt d tan trong nc; tan trong ethanol; t tan trong ether, benzen,
cyclohexan; khng tan trong carbon tetraclorid.
nh tnh
A. im chy: 283 n 286oC (Ph lc 5.19).
B. Gc quay cc ring
+17,25 n +19,25o (i vi natri camphosulfonat iu ch t camphor
thin nhin).
-1,5 n +1,5o (i vi natri camphosulfonat iu ch t camphor tng
hp, racemic).
Ho tan 1,0 g ch phm trong nc, pha long n 25 ml vi cng dung
mi v tin hnh o (Ph lc 5.13).
C. un nng khong 1 g ch phm vi vi vin natri hydroxyd (TT), s bc
mi c trng ca camphor.
Ho tan 2 g ch phm trong 10 ml nc. Dung dch phi trong (Ph lc
5.12) v khng c c mu m hn mu ca dung dch iod 0,00005 N.
pH
Ho tan 1 g ch phm trong 10 ml nc khng c carbon dioxyd (TT). pH
ca dung dch phi t 6,0 n 8,0 (Ph lc 5.9).
Bari
Ho tan 0,1 g ch phm trong 5 ml nc, thm 2 git dung dch acid
hydrocloric 10% (TT) v 2,5 ml dung dch bo ho calci sulfat (TT). Dung dch
thu c phi trong.
Clorid
Khng c qu 0,01% (Ph lc 7.4.5).
Ho tan 0,5 g ch phm trong nc va 15 ml v tin hnh th.
Sulfat
Khng c qu 0,05% (Ph lc 7.4.12).
Ho tan 0,3 g ch phm trong nc va 15 ml v tin hnh th.
Kim loi nng
Ho tan 2,0 g ch phm trong nc v pha long n 20 ml vi cng dung
mi. Ly 12 ml dung dch ny th theo phng php 1. Dng dung dch ch mu 2
Mt khi lng do lm kh
Khng c qu 2,7% (Ph lc 5.16).
(1,000 g; 100 - 105oC; 2 gi).
Bo qun
Ch phm
Dung dch tim natri camphosulfonat 10%; dung dch ung nh git.
Tc dng v cng dng
Kch thch thn kinh trung ng (u tin hnh no). Dng kch thch h hp
v tr tim.
47-NATRI CITRAT
Natrii citras
C6H5Na3O7. 2H2O P.t.l: 294,1

Natri citrat l trinatri 2 - hydroxypropan - 1, 2, 3 - tricarboxylat, phi cha
t 99,0 n 101,0% C6H5Na3O7, tnh theo ch phm khan.
Tnh cht
Bt kt tinh trng hoc tinh th dng ht trng, ht m nh trong khng kh
m. D tan trong nc, thc t khng tan trong ethanol 96%.
nh tnh
A. Thm vo 1 ml dung dch S 4 ml nc, dung dch thu c phi cho
phn ng ca ion citrat (Ph lc 7.1).
B. 1 ml dung dch S phi cho phn ng A ca ion natri (Ph lc 7.1).
(TT) va 100 ml.
php 2).
Gii hn acid - kim
Thm 0,1 ml dung dch phenolphtalein (CT) vo 10 ml dung dch S. Dung
dch phi chuyn mu khi thm khng qu 0,2 ml dung dch natri hydroxyd 0,1 N,
hoc dung dch acid hydrocloric 0,1 N.
Cht d carbon ho
Thm 10 ml acid sulfuric (TT) vo 0,20 g ch phm c nghin nh v

lm nng trong cch thu 90 1oC trong 60 pht. Lm lnh nhanh. Dung dch c
mu khng c m hn mu mu V2 hoc LV2 (Ph lc 5.17, phng php 2).
Clorid
Oxalat
Khng c qu 0,03%.
Ho tan 0,50 g ch phm trong 4 ml nc. Thm 3 ml acid hydrocloric
(TT) v 1 g km ht (TT) vo dung dch trn, un nng trn cch thu trong 1
pht. yn 2 pht, gn lp cht lng vo ng nghim c cha 0,25 ml dung dch
phenylhydrazin hydroclorid 1,0% v un nng n si. Lm ngui nhanh, chuyn
vo ng nghim c chia vch, thm mt lng th tch tng ng acid
hydrocloric (TT) v 0,25 ml dung dch kali fericyanid 5% (TT). Lc v yn 30
pht. Mu hng ca dung dch khng c m hn mu ca dung dch i chiu
c chun b tng t trong cng thi gian nhng dng 4 ml dung dch acid
oxalic 0,005% thay cho 0,50 g ch phm ho tan trong 4 ml nc.
Sulfat
Khng c qu 0,015% (Ph lc 7.4.12).
Thm 2 ml dung dch acid hydrocloric 25% vo 10 ml dung dch S, thm
nc va 15 ml v tin hnh th.
Kim loi nng
Ly 12 ml dung dch S tin hnh theo phng php 1. Dng dung dch ch
Nc
T 11,0 n 13,0% (Ph lc 6.6).
Dng 0,300 g ch phm. Sau khi thm ch phm, khuy trong 15 pht trc
khi chun .
Cht gy st
Nu ch phm c d nh dng sn xut dung dch tim vi th tch
ln th phi t php th ny.
Tim cho 1 kg th 10 ml dung dch va mi pha trong nc ct pha tim c
cha 10,0 mg ch phm v 7,5 mg calci clorid khng c cht gy st trong 1 ml
(Ph lc 10.5).
nh lng
Ho tan 0,150 g ch phm trong 20 ml acid acetic khan (TT), lm nng n
khong 50oC. ngui. Dng 0,25 ml dung dch naphtholbenzein (CT) lm ch
th v chun bng dung dch acid percloric 0,1 N n khi mu xanh xut hin.
C6H5Na3O7.
Bo qun
Trong l kn.
48-NATRI CLORID
Natrii chloridum
NaCl
P.t.l: 58,44
Natri clorid phi cha t 99,0 n 100,5% NaCl, tnh theo ch phm lm
kh.
Tnh cht
Bt kt tinh trng hoc tinh th khng mu. D tan trong nc, thc t
khng tan trong ethanol.
nh tnh
A. Phi cho phn ng ca ion clorid (Ph lc 7.1).
B. Phi cho phn ng ca ion natri (Ph lc 7.1).
(TT) v pha long va 100,0 ml bng cng dung mi.
php 2).
Gii hn acid - kim
Thm 0,1 ml dung dch xanh bromothymol (CT) vo 20 ml dung dch S.
Dung dch phi chuyn mu khi thm khng qu 0,5 ml dung dch acid
hydrocloric 0,01 N hoc dung dch natri hydroxyd 0,01 N.
Bromid
Thm vo 1,0 ml dung dch S, 4,0 ml nc, 2,0 ml dung dch phenol
(CT2) v 1,0 ml dung dch cloramin 0,01% (TT), trn u ngay. Sau ng 2 pht,
thm 0,15 ml dung dch natri thiosulfat 0,1 M, trn u v pha long thnh 10,0 ml
bng nc. o hp th (Ph lc 3.1) ca dung dch trn bc sng 590 nm,
dng nc lm mu trng. hp th ca dung dch trn khng c ln hn
hp th ca dung dch i chiu c chun b trong cng mt thi gian, cng
cch tin hnh, nhng thay 1,0 ml dung dch S v 4 ml nc bng 5,0 ml dung
dch kali bromid 0,0003%.
Ferocyanid
Ho tan 2,0 g ch phm trong 6 ml nc. Thm 0,5 ml hn hp gm 5 ml

dung dch st (III) amoni sulfat 1% trong dung dch acid sulfuric 0,25% v 95 ml
dung dch st (II) sulfat 1,0%. Mu xanh khng c xut hin trong vng 10
pht.
Iodid
Lm m 5,0 g ch phm bng cch thm tng git hn hp va mi pha
gm 0,15 ml dung dch natri nitrit 10% (TT), 2 ml dung dch acid sulfuric 0,5 M,
25 ml dung dch h tinh bt khng c iodid (CT) v 25 ml nc. Sau 5 pht, quan
st di nh sng ban ngy, hn hp cht th khng c c mu xanh.
Nitrit
Thm 10 ml nc vo 10 ml dung dch S. o hp th (Ph lc 3.1) ca
dung dch bc sng 354 nm. hp th thu c khng c ln hn 0,01.
Phosphat
Pha long 2,0 ml dung dch S thnh 100 ml bng nc v tin hnh th.
Sulfat
Khng c qu 0,02% (Ph lc 7.4.12).
Pha long 7,5 ml dung dch S thnh 30 ml bng nc v ly 15 ml dung
dch ny tin hnh th.
Nhm
Nu ch phm c d nh dng sn xut cc dung dch thm tch
mng bng, thm tch mu hoc lc mu, th phi p ng yu cu php th ny.
Dung dch th: Ho tan 20,0 g ch phm trong 100 ml nc v thm 10 ml
Dung dch i chiu: gm 2 ml dung dch nhm mu 2 phn triu, 98 ml

nc v 10 ml dung dch m acetat pH 6,0.
Dung dch mu trng: gm 10 ml dung dch m acetat pH 6,0 v 100 ml
nc.
Arsen
Dng 5 ml dung dch S v tin hnh th theo phng php A.
Bari
Thm vo 5 ml dung dch S, 5 ml nc v 2 ml dung dch acid sulfuric 1
M. Sau 2 gi, dung dch khng c c hn hn hp gm 5 ml dung dch S v 7
ml nc.
Kim loi nng
St
Ly 10 ml dung dch S v tin hnh th. Dng hn hp gm 4 ml dung dch
st mu 1 phn triu v 6 ml nc chun b mu i chiu.
Khng c qu 0,01% tnh theo Ca (Ph lc 7.4.14).
Dng 10,0 g ch phm.
Th tch ca dung dch natri edetat 0,01 M dng khng c qu 2,5 ml.
Kali
Khng c qu 0,05%.
Nu c d nh sn xut thuc tim c phn liu, hoc cc dung dch
thm tch mu, lc mu, thm tch mng bng, th ch phm phi p ng yu cu
php th ny.
Xc nh bng phng php quang ph pht x nguyn t (Ph lc 3.4,
Phng php 1).
Dung dch th: Ho tan 1,00 g ch phm trong nc v pha long va
100 ml bng cng dung mi.
Dung dch chun: Ho tan trong nc 1,144 g kali clorid (TT) c sy
100 - 105oC trong 3 gi v pha long thnh 1000,0 ml bng nc (dung dch
cha 600 g K/ ml). Pha long theo yu cu.
o cng pht x 768 nm.
Mt khi lng do lm kh
Khng c qu 0,5% (Ph lc 5.16).
(1,000 g; 100 - 105oC; 2 gi).
Ni c t vi khun
Khng c cha qu 5 EU ni c t trong 1 g ch phm (Ph lc 10.3).
Nu ch phm c d nh sn xut cc dng thuc tim m khng c
phng php hu hiu no khc loi ni c t th phi tin hnh php th ny.
nh lng
Ho tan 1,000 g ch phm trong nc v pha long thnh 100 ml vi cng
dung mi. Thm 50 ml nc, 5 ml acid nitric long (TT), 25,0 ml dung dch bc
nitrat 0,1 M v 2 ml dibutylphthalat (TT) vo 10,0 ml dung dch trn. Lc v
chun bng dung dch amoni thiocyanat 0,1 M, dng 2 ml dung dch st (III)
amoni sulfat 10% lm ch th v lc mnh cho ti khi kt thc php nh lng.
1 ml dung dch bc nitrat 0,1 M tng ng vi 5,844 mg NaCl.

Nhn
Nhn cn ghi r ch phm dng sn xut cc dng thuc tim phn liu
hoc khng c ni c t vi khun, hoc dng sn xut cc dung dch thm tch
mng bng, thm tch mu hoc lc mu.
49-NATRI HYDROCARBONAT
Natrii hydrocarbonas
NaHCO3
P.t.l: 84,0
Natri hydrocarbonat phi cha t 99,0 n 101,0% NaHCO3.

Tnh cht
Bt kt tinh trng. Tan trong nc, thc t khng tan trong ethanol 96%.
Khi un nng trng thi kh hoc trong dung dch, n chuyn dn thnh natri
carbonat.
nh tnh
A. Thm vo 5 ml dung dch S 0,1 ml dung dch phenolphtalein (CT), mu
hng nht xut hin. un nng, kh bay ln v dung dch c mu .
B. Phi cho phn ng ca carbonat v bicarbonat (Ph lc 7.1).
C. Dung dch S cho phn ng ca natri (Ph lc 7.1).
Dung dch S: Ho tan 5,0 g ch phm trong 90 ml nc khng c carbon
dioxyd (TT) v pha long thnh 100 ml bng cng dung mi.
php 2).
Carbonat
pH ca dung dch S va mi pha phi khng c ln hn 8,6 (Ph lc

5.9).
Clorid
Khng c qu 0,015% (Ph lc 7.4.5).
Thm vo 7 ml dung dch S, 2 ml acid nitric (TT), pha long thnh 15 ml
bng nc v tin hnh th.
Sulfat
Khng c qu 0,015% (Ph lc 7.4.12).
Thm acid hydrocloric (TT) vo hn dch cha 1,0 g ch phm trong 10 ml
nc n khi trung tnh v tha khong 1 ml ri pha long thnh 15 ml bng nc
v tin hnh th.
Amoni
Ly 10 ml dung dch S pha long thnh 15 ml bng nc v tin hnh th
theo phng php A. Dng hn hp gm 5 ml nc v 10 ml dung dch amoni
Arsen
Ly 0,5 g ch phm tin hnh th theo phng php A.
Calci
Khng c qu 0,01% (Ph lc 7.4.3).
Thm acid hydrocloric (TT) vo hn dch cha 1,0 g ch phm trong 10 ml
nc cho n khi trung tnh, pha long thnh 15 ml bng nc v tin hnh th.
Kim loi nng

Ho tan 2,0 g ch phm trong hn hp gm 2 ml acid hydrocloric (TT) v
18 ml nc. Ly 12 ml dung dch ny tin hnh th theo phng php 1. Dng
dung dch ch mu 1 phn triu lm mu i chiu.
St
Ha tan 0,5 g ch phm trong 5 ml dung dch acid hydrocloric long (TT),
pha long thnh 10 ml bng nc v tin hnh th.
nh lng
Ho tan 1,500 g ch phm trong 50 ml nc khng c carbon dioxyd (TT).
Chun bng dung dch acid hydrocloric 1 M, dng 0,2 ml dung dch da cam
methyl (CT) lm ch th.
1 ml dung dch acid hydrocloric 1 M tng ng vi 84,0 mg NaHCO3.
50-NATRI SALICYLAT
Natrii salicylas
C7H5NaO3 P.t.l: 160,1

Natri salicylat l natri 2 - hydroxybenzencarboxylat, phi cha t 99,0 n
101,0% C7H5NaO3, tnh theo ch phm lm kh.
Tnh cht
Bt kt tinh trng hoc tinh th khng mu hay hnh vy ng nh, khng
mi.
D tan trong nc, hi tan trong ethanol 96%, thc t khng tan trong
ether.
nh tnh
A. Ly vi ht ch phm a vo ngn la khng mu, ngn la s chuyn
thnh mu vng.
B. Ly khong 10 mg ch phm ho tan trong 10 ml nc, thm 1 git dung
dch st (III) clorid 3% (TT), s xut hin mu tm.
C. Ho tan khong 1,5 g ch phm trong khong 20 ml nc, thm 6 ml
dung dch acid nitric 16% (TT), s xut hin ta trng. Lc, ra ta bng nc v
sy kh trong bnh ht m vi acid sulfuric (TT), im chy ca acid salicylic thu
c t 158 n 161oC (Ph lc 5.19).
(TT), thm va 50,0 ml vi cng dung mi.
Gii hn acid
Ht 20 ml dung dch S, thm 0,1 ml dung dch phenol (CT), dung dch
c mu vng. Mu ca dung dch phi chuyn sang mu tm khi thm khng
qu 2,0 ml dung dch natri hydroxyd 0,01 M.
Clorid
Khng c qu 0,02% (Ph lc 7.4.5).
Ly 5 ml dung dch S, thm 5 ml nc v 10 ml acid nitric long (TT), lc.
Ht 10 ml dch lc, pha long thnh 15 ml vi nc v tin hnh th.
Sulfat
Khng c qu 0,06% (Ph lc 7.4.12).

Ly 2,5 ml dung dch S, pha long thnh 15 ml vi nc v tin hnh th.
Kim loi nng
Ho tan 1,50 g ch phm trong 15 ml hn hp gm 5 th tch nc v 10
th tch ethanol 96% (TT). Ly 12 ml dung dch tin hnh th theo phng php 2.
Dng 10 ml dung dch ch mu 2 phn triu thu c bng cch pha long t dung
dch ch mu 100 phn triu vi hn hp gm 5 th tch nc v 10 th tch
ethanol 96% (TT), chun b mu i chiu.
Mt khi lng do lm kh
Khng c qu 0,5% (Ph lc 5.16).
(1,000 g; 100 - 105oC).
nh lng
Cn chnh xc khong 0,130 g ch phm, ho tan trong 30 ml acid acetic
khan (TT). Chun bng dung dch acid percloric 0,1 N. Xc nh im kt thc
bng phng php o in th (Ph lc 6.12).
C7H5NaO3.
Bo qun
ng trong chai l kn, trnh nh sng.
51-NATRI SULFAT
Natrii sulfas
Na2SO4. 10H2O
P.t.l: 322,2
Natri sulfat ngm 10 phn t nc phi cha t 99,0 n 100,5% Na2SO4,

tnh theo ch phm lm kh.
Tnh cht
Bt kt tinh mu trng, hoc tinh th trong sut khng mu.
D tan trong nc, thc t khng tan trong ethanol 96%. Tan mt phn
trong nc kt tinh ca chnh n khong 33oC.
nh tnh
Ch phm phi cho phn ng ca ion natri v sulfat (Ph lc 7.1).
Dung dch S: Ho tan 5,0 g ch phm trong nc v pha long bng nc
va 100 ml.
php 2).
Gii hn acid - kim
Thm vo 10 ml dung dch S 0,1 ml dung dch xanh bromothymol (CT).
lm chuyn mu dung dch ny, khng c dng qu 0,5 ml dung dch acid
hydrocloric 0,01 M hoc dung dch natri hydroxyd 0,01 M.
Clorid
Khng c qu 0,02% (Ph lc 7.4.5).
Ly 5 ml dung dch S pha long vi nc thnh 15 ml v tin hnh th.
Arsen
Ly 10 ml dung dch S v tin hnh th theo phng php A.
Calci
Khng c qu 0,02% (Ph lc 7.4.3).

Ly 10 ml dung dch S, pha long vi nc thnh 15 ml v tin hnh th.
Kim loi nng
Ly 12 ml dung dch S, tin hnh th theo phng php 1. Dng dung dch
St
Magnesi
Khng c qu 0,01%.
Thm vo 10 ml dung dch S 1 ml glycerin 85% (TT), 0,15 ml dung dch
vng titan (CT), 0,25 ml dung dch amoni oxalat 4% (TT) v 5 ml dung dch natri
hydroxyd 2 M (TT), lc u. Dung dch ny nu c bt k mu hng no cng
khng c m hn mu ca dung dch i chiu c chun b ng thi trong
cng mt iu kin, nhng thay dung dch S bng hn hp 5 ml dung dch
magnesi mu 10 phn triu v 5 ml nc.
Mt khi lng do lm kh
T 52,0 n 57,0% (Ph lc 5.16).
(1,000 g; 30oC; 1 gi; sau 130oC).
nh lng
Ho tan 3,00 g ch phm trong 50 ml nc. Cho dung dch ny i qua mt
ct cha nha trao i ion acid mnh (TT) vi tc chy khong 4 ml mt pht.
Ra ct vi nc (khong 300 ml) cho ti khi dng khng qu 0,05 ml dung dch
natri hydroxyd 0,1 M trung ho 50 ml dch hng c. Chun dch hng
c bng dung dch natri hydroxyd 1 M, dng 0,1 ml dung dch da cam methyl
(CT) lm ch th.
1 ml dung dch natri hydroxyd 1 M tng ng vi 71,0 mg Na2SO4.
Bo qun
ng trong chai,l kn.
52-NATRI SULFAT KHAN
Natrii sulfas exsiccatus
Na2SO4
P.t.l: 142,0
Natri sulfat khan phi cha t 99,0 n 100,5% Na2SO4, tnh theo ch
phm lm kh.
Tnh cht
Bt trng, d ht m. D tan trong nc.
nh tnh
Ch phm phi cho phn ng ca ion natri v sulfat (Ph lc 7.1).
Dung dch S: Ho tan 2,2 g ch phm trong nc ri thm nc va 100
ml.
php 2).
Gii hn acid - kim
Thm vo 10 ml dung dch S 0,1 ml dung dch xanh bromothymol (CT).
lm chuyn mu dung dch ny, khng c dng qu 0,5 ml dung dch natri
hydroxyd 0,01 M hoc dung dch acid hydrocloric 0,01 M.
Clorid
Khng c qu 0,045% (Ph lc 7.4.5).

Arsen
Ly 10 ml dung dch S v tin hnh th theo phng php A.
Calci
Khng c qu 0,045% (Ph lc 7.4.3).
Kim loi nng
Ly 12 ml dung dch S, tin hnh th theo phng php 1. Dng dung dch
St
Magnesi
Khng c qu 0,02%.
Thm vo 10 ml dung dch S 1 ml glycerin 85% (TT), 0,15 ml dung dch
vng titan (CT), 0,25 ml dung dch amoni oxalat 4% (TT) v 5 ml dung dch natri
hydroxyd 2 M (TT), lc u. Dung dch ny nu c mu hng th khng c m
hn mu ca dung dch i chiu c chun b ng thi trong cng iu kin,
nhng thay dung dch S bng hn hp 5 ml dung dch magnesi mu 10 phn triu
v 5 ml nc.
Mt khi lng do lm kh
Khng c qu 5,0% (Ph lc 5.16).

(1,000 g; 130oC).
nh lng
Ho tan 1,30 g ch phm trong 50 ml nc. Cho dung dch ny i qua mt
ct cha nha trao i ion acid mnh (TT) vi tc chy khong 4 ml trong mt
pht. Ra ct vi nc (khong 300 ml) cho n khi dng khng qu 0,05 ml
dung dch natri hydroxyd 0,1 M trung ho 50 ml dch hng c. Chun
dch hng c vi dung dch natri hydroxyd 1 M, dng 0,1 ml dung dch da cam
methyl (CT) lm ch th.
1 ml dung dch natri hydroxyd 1 M tng ng vi 71,0 mg Na2SO4.
Bo qun
ng trong chai, l kn, trnh ht m.
53-NATRI THIOPENTAL V NATRI CARBONAT

Thiopentalum natricum et natrii carbonas
C11H17N2NaO2S P.t.l: 264,3

Natri thiopental l hn hp ca natri (RS) - 5 - ethyl - 5 - (1 - methylbutyl) 2 - thiobarbiturat v natri carbonat khan, phi cha t 84,0 n 87,0%
C11H18N2O2S v t 10,2 n 11,2% Na, c hai u tnh theo ch phm lm
kh.
Tnh cht
Bt trng hi ng, c mi ging nh ti, ht m.
D tan trong nc, tan mt phn trong ethanol 96%, thc t khng tan trong
ether.
nh tnh
Nhm I: A, B, E.
Nhm II: A, C, D v E.
A. Acid ho 10 ml dung dch S bng dung dch acid hydrocloric long
(TT), dung dch si bt. Cho 20 ml ether (TT) vo dung dch, lc. Tch ly lp
ether, ra vi 10 ml nc, lm khan bng natri sulfat khan (TT), lc, lm bay hi
dch lc n kh v sy cn 100 - 105oC. Xc nh im chy (Ph lc 5.19) ca
cn. Trn ng lng cn ny vi thiopental chun v xc nh im chy ca hn
hp. im chy ca cn v ca hn hp phi khong 160oC. S khc bit v im
chy ca 2 mu trn khng c qu 2oC.
B. Ph hng ngoi (Ph lc 3.2) ca cn thu c php th A phi ph
hp vi ph hng ngoi ca thiopental chun.
Dung mi khai trin: Amoniac m c - ethanol 96% - cloroform (5: 15:
80).
Dung dch th: Ho tan 0,1 g ch phm trong nc v thm va 100 ml
bng cng dung mi.
Dung dch i chiu: Ho tan 85 mg thiopental chun trong 10 ml dung
dch natri hydroxyd long (TT) v pha long n 100 ml bng nc.
Trin khai sc k n khi dung mi i c 18 cm. Quan st bn mng di nh
sng t ngoi bc sng 254 nm. Vt chnh trn sc k ca dung dch th
phi ging v v tr v kch thc vi vt chnh trn sc k ca dung dch i

chiu.
D. Phn ng c trng ca barbiturat c hydro nhm NH khng b thay
th (Ph lc 7.1).
E. Phn ng c trng ca natri (Ph lc 7.1).
(TT) v b sung n 50,0 ml bng cng dung mi.
mu LV3 (Ph lc 5.17, phng php 2).
Clorid
Khng c qu 0,033% (Ph lc 7.4.5).
Ly 5 ml dung dch S, thm 35 ml nc v 10 ml dung dch acid nitric 2 M.
Lc vi ether 3 ln, mi ln vi 25 ml. B lp ether, un cch thu lp nc
loi hon ton ether. Dng 15 ml lp nc ny th.
Tp cht lin quan
Khng c qu 0,5%.
Xc nh bng phng php sc k lp mng (Ph lc 4.4).
Dung mi khai trin: Amoniac m c - ethanol 96%: cloroform (5: 15:
80).
Dung dch th: Ho tan 1,0 g ch phm trong nc v pha long bng nc
n 100,0 ml, lc b ta nu c.
Dung dch i chiu: Pha long 0,5 ml dung dch th thnh 100,0 ml vi
nc.
Trin khai sc k n khi dung mi i c khong 15 cm. Quan st bn mng
di nh sng t ngoi bc sng 254 nm. Bt c vt ph no trn sc k thu
c t dung dch th khng c m mu hn vt trn sc k thu c t
dung dch i chiu. Khng k n nhng vt vch xut pht.
Mt khi lng do lm kh
Khng c qu 2,0% (Ph lc 5.16).
(0,500 g; 80oC; 4 gi).
nh lng
Natri: Ho tan 0,400 g ch phm trong 30 ml nc. Chun bng dung
dch acid hydrocloric 0,1 N v dng 0,1 ml dung dch methyl (CT) lm ch th,
n khi mu ca dung dch chuyn sang . un si nh 2 pht, lm ngui, nu
cn th tip tc chun vi dung dch acid hydrocloric 0,1 N n mu nh c.
1 ml dung dch acid hydrocloric 0,1 N tng ng vi 2,299 mg natri.
Thiopental: Ho tan 0,150 g ch phm trong 5 ml nc, thm 2 ml dung
dch acid sulfuric 1 M ri chit vi cloroform (TT) 4 ln, mi ln 10 ml. Gp cc
dch chit cloroform li, lc, ra phu lc bng cloroform, gp dch lc, lm bay
hi dch lc n kh trn cch thu. Ho tan cn trong 30 ml dimethylformamid
(TT) c trung ho trc bng dung dch lithi methoxyd 0,1 M v 0,1 ml dung
dch xanh thymol 0,2% trong methanol. Chun ngay bng dung dch lithi
methoxyd 0,1 M n khi dung dch chuyn sang mu xanh dng, trnh dung
dch tip xc vi carbon dioxyd ca khng kh trong sut qu trnh nh lng.
1 ml lithi methoxyd 0,1 M tng ng vi 24,23 mg C11H18N2O2S.
Bo qun
Trong chai l kn v trnh nh sng.
Ch phm
Dung dch tim thiopental.

Tc dng v cng dng
Gy m tng qut.
54-NATRI THIOSULFAT
Natrii thiosulfas
Natri hyposulfit
Na2S2O3. 5H2O
P.t.l: 248,2
Natri thiosulfat phi cha t 99,0 n 101,0% Na2S2O3. 5H2O.

Tnh cht
Tinh th trong, khng mu, ln hoa trong khng kh kh.
Rt tan trong nc, thc t khng tan trong ethanol 96%, tan trong nc kt
tinh ca n khong 49oC.
nh tnh
(TT) va 100 ml.
A. Ly 1 ml dung dch S, thm vi git dung dch iod 0,1 N, dung dch mt
mu.
B. Ly 1 ml dung dch S, thm 1 ml acid hydrocloric (TT), s xut hin ta
lu hunh v c mi ca lu hunh dioxyd.
C. Ly 1 ml dung dch S, thm 2 ml dung dch bc nitrat 0,1 N, c ta trng
chuyn nhanh sang vng ri dn dn sang en.
D. Dung dch S cho phn ng A ca ion natri (Ph lc 7.1).
php 2).
pH
Dung dch S phi c pH t 6,0 n 8,4 (Ph lc 5.9).
Clorid
Khng c qu 0,02% (Ph lc 7.4.5).
Ly 5 ml dung dch S, thm 15 ml dung dch acid nitric 2 M, un si nh
trong 3 - 4 pht. ngui, lc, pha long dch lc bng nc thnh 25 ml. Ly
12,5 ml dung dch thu c, pha long thnh 15 ml vi nc v tin hnh th.
Sulfat v sulfit
Khng c qu 0,2%.
Ly 2,5 ml dung dch S, pha long vi nc thnh 10 ml. Ht 3 ml dung
dch thu c, thm 2 ml dung dch iod 0,1 N, thm tip tng git dung dch iod
0,1 N cho n khi c mu vng rt nht bn vng, ri pha long vi nc thnh 15
ml, tin hnh th gii hn sulfat (Ph lc 7.4.12).
Sulfid
Ly 10 ml dung dch S, thm 0,5 ml dung dch natri nitroprusiat 0,5% mi
pha, khng c c mu tm.
Kim loi nng
Ly 10,0 ml dung dch S, thm 0,05 ml dung dch natri sulfid (TT), yn
2 pht. Dung dch ny khng c c mu m hn mu ca dung dch gm 10
ml dung dch ch mu 1 phn triu v 0,05 ml dung dch natri sulfid (TT).
nh lng
Ho tan 0,500 g ch phm trong 20 ml nc v chun bng dung dch

iod 0,1 N. Vo lc cui chun , thm 1 ml dung dch h tinh bt (CT).
1 ml dung dch iod 0,1 N tng ng vi 24,82 mg Na2S2O3. 5H2O.
Bo qun
ng trong l kn.
55-NHM HYDROXYD KH
Aluminii hydroxydum siccum
Nhm hydroxyd kh l nhm oxyd ngm nc, phi cha t 47,0 n
60,0% Al2O3 (P.t.l: 102,0).
Tnh cht
Bt trng v nh hnh.
Thc t khng tan trong nc, tan trong cc acid v c long v trong cc
dung dch hydroxyd kim.
nh tnh
Dung dch S: Ho tan 1,25 g ch phm trong 7,5 ml acid hydrocloric (TT)
bng cch un nng trn cch thy v pha long vi nc thnh 50 ml.
Dung dch S phi c phn ng ca ion nhm (Ph lc 7.1).
Dung dch S khng c c hn c mu S2 (Ph lc 5.12) v mu
khng c m hn mu mu LV6 (Ph lc 5.17, phng php 2).
Gii hn kim
Lc 1,0 g ch phm vi 20 ml nc khng c carbon dioxyd (TT) trong
mt pht v lc. Thm vo 10 ml dch lc, 0,1 ml dung dch phenolphtalein (TT).
Dung dch nu c bt k mu hng no cng phi mt mu khi cho thm 0,3 ml

dung dch acid hydrocloric 0,1 M.
Kh nng trung ho
Tin hnh php th 37oC.
Ho tan 0,5 g ch phm trong 100 ml nc, un nng, thm 100,0 ml dung
dch acid hydrocloric 0,1 M c lm nng trc v khuy lin tc. pH ca
dung dch sau 10 pht, 15 pht v 20 pht khng c di 1,8; 2,3 v 3,0 v
bt k thi im no cng khng c qu 4,5. Thm 10,0 ml dung dch acid
hydrocloric 0,5 M c lm nng trc, khuy lin tc trong mt gi v chun
bng dung dch natri hydroxyd 0,1 M n pH 3,5. Lng dung dch natri
hydroxyd 0,1 M dng khng c qu 35,0 ml.
Clorid
Khng c qu 1% (Ph lc 7.4.5).
Ho tan 0,1 g ch phm trong 10 ml dung dch acid nitric long (TT) bng
cch lm nng v pha long vi nc thnh 100 ml. Ly 5 ml dung dch ny, pha
long vi nc thnh 15 ml v tin hnh th.
Sulfat
Khng c qu 1% (Ph lc 7.4.12).
Pha long 4 ml dung dch S vi nc thnh 100 ml. Ly 15 ml dung dch
ny tin hnh th.
Arsen
Ly 10 ml dung dch S tin hnh th theo phng php A.
Kim loi nng
Trung ho 10 ml dung dch S bng amoniac m c (TT), dng dung dch

vng metanil (CT) lm ch th ngoi. Lc nu cn ri pha long vi nc thnh 15
ml. Ly 12 ml dung dch ny tin hnh th theo phng php 1. Dng 10 ml dung
nhim khun
Tng s vi khun hiu kh sng li c khng c qu 1000 trong mt
gam ch phm. Xc nh bng phng php a thch (Ph lc 10.7).
Ch phm phi t cc yu cu v Enterobacteria v cc vi khun Gram m
khc; v Escherichia coli (Ph lc 10.7).
nh lng
Ho tan 0,800 g ch phm trong 10 ml dung dch acid hydrocloric 25%
bng cch un nng trn cch thu. ngui v pha long vi nc thnh 50,0
ml. Thm vo 10,0 ml dung dch ny dung dch amoniac 6 M cho ti khi bt u
xut hin ta. Thm mt lng ti thiu dung dch acid hydrocloric long (TT) cn
thit ho tan ta v pha long vi nc thnh 20 ml. Tin hnh chun nhm
theo phng php chun complexon (Ph lc 6.11).
1 ml dung dch natri edetat 0,1 M tng ng vi 5,098 mg Al2O3.
Bo qun
Trong ng kn, nhit di 30oC.
56-NHM PHOSPHAT KH
Aluminii phosphas siccum
AlPO4
P.t.l: 121,95
Nhm phosphat kh ch yu l nhm phosphat hydrat ho, phi cha

khng t hn 80,0% AlPO4.
Sn xut
Ch phm c iu ch bng cch sy kh trong iu kin thch hp, sn

phm ca phn ng gia dung dch nc ca mui nhm vi kim phosphat nh
natri phosphat.
Tnh cht
Bt mu trng c cha cc b vn d nghin. Tan trong acid v c long,
thc t khng tan trong ethanol 96%, trong nc v cc dung dch kim hydroxyd.
nh tnh
Dung dch ch phm trong dung dch acid hydrocloric 2 M cho phn ng
c trng ca ion nhm v ion phosphat (Ph lc 7.1).
pH
Hn dch ch phm 4% trong nc khng c carbon dioxyd (TT) c pH t
5,5 n 6,5 (Ph lc 5.9).
Kh nng trung ho
Ry ch phm (nghin nu cn thit) qua ry c mt ry c 75 m. Cn 0,5 g
ch phm ry trn, thm 30 ml dung dch acid hydrocloric 0,1 M 37oC v
duy tr nhit 37oC trong 20 pht, khuy lin tc, pH ca hn hp ny phi t
2,0 n 2,5 (Ph lc 5.9).
Arsen
Ha tan 0,40 g ch phm trong 18 ml acid hydrocloric brom ho (TT) v
pha long vi nc va 50 ml. Ly 25 ml dung dch thu c tin hnh th
theo phng php A.
Kim loi nng
Ho tan 1,43 g ch phm trong 20 ml dung dch acid hydrocloric 1 M v 10

ml nc, thm 0,5 ml acid nitric (TT) v un si 30 giy. ngui, thm 2 g
amoni clorid (TT) v 2 g amoni thiocyanat (TT) v chit hai ln, mi ln vi 10 ml
hn hp ng th tch amyl alcol v ether. Thm 2 g acid citric (TT) vo lp nc
v pha long vi nc thnh 50 ml. Ly 12 ml dung dch thu c th theo
phng php 1. Dng dung dch ch mu 2 phn triu chun b mu i chiu.
Clorid
Khng c qu 1,4% (Ph lc 7.4.5).
Ho tan 0,24 g ch phm trong 10 ml dung dch acid nitric 2 M, un si,
ngui, pha long thnh 1000 ml bng nc v lc. Ly 15 ml dch lc tin hnh
th.
Sulfat
Khng c qu 0,6% (Ph lc 7.4.12).
Ho tan 0,17 g ch phm trong 10 ml dung dch acid hydrocloric 2 M, un
si, ngui, pha long vi nc thnh 100 ml, lc. Ly 15 ml dch lc, thm 2
ml dung dch acid hydrocloric 2 M v tin hnh th.
Phosphat tan
Khng c qu 1,0% tnh theo PO4.
Lc 5,0 g ch phm vi 150 ml nc trong hai gi, lc n khi c dch
lc trong, ra phu lc bng 50 ml nc. Tp trung dch lc v nc ra, thm
nc va 250 ml, trn u, pha long 10 ml dung dch ny vi nc thnh 100
ml. Ly 5 ml dung dch thu c, thm 4 ml dung dch acid sulfuric 1 M, 1 ml
dung dch amoni molybdat - acid sulfuric (TT), 2 ml thuc th
methylaminophenol - sulfit (TT) v 5 ml nc. Trn u, yn trong 15 pht v
thm nc va 25 ml. yn tip 15 pht v o hp th (Ph lc 3.1) ca
dung dch bc sng 730 nm trong cc o dy 2 cm.
Tnh hm lng phosphat tan t ng cong chun c thit lp bi cc

dung dch kali dihydrophosphat 0,00286% c x l ging nh mu th bt u
t cu "thm 4 ml dung dch acid sulfuric 1 M..."
Dung dch kali dihydrophosphat 0,00286% tng ng vi 0,00100%
PO4.
nh lng
Ho tan 0,800 g ch phm trong 15 ml dung dch acid hydrocloric 2 M, lm
nng nu cn ho tan ht ch phm, ngui v thm dung dch acid
hydrocloric 2 M va 100 ml. Ly 10 ml dung dch thu c, thm 25 ml dung
dch natri edetat 0,05 M, nh tng git amoniac 13,5 M (TT) n khi c phn ng
kim vi giy qu. un si nh 5 pht, ngui v thm 10 ml dung dch c
pha nh sau: Ho tan 7,7 g amoni acetat (TT) trong 50 ml nc, thm 6 ml acid
acetic bng (TT), thm nc va 100 ml. Chnh pH n 4,5 bng acid acetic
bng (TT), thm 2 ml dung dch dithizon 0,025% trong ethanol 96%. Thm
ethanol 96% c th tch gp i v chun bng dung dch km clorid 0,05
M n khi mu chuyn sang .
Song song lm mu trng. Hiu gia mu trng v mu th l lng natri
edetat tiu th.
1 ml dung dch natri edetat 0,05 M tng ng vi 6,098 mg AlPO4.
Bo qun
Trong ng kn, nhit khng qu 30oC.
57-NIKETHAMID
Nikethamidum
C10H14N2O P.t.l: 178,2

Nikethamid l N, N - diethylpyridin - 3 - carboxamid, phi cha t 99,0 n
101,0% C10H14N2O, tnh theo ch phm khan.
Tnh cht
Cht lng snh nh du hoc khi kt tinh khng mu hoc mu hi nh
vng. C th trn ln vi nc, cloroform, ethanol 96% v ether bt k t l no.
nh tnh
Nhm I: A, B.
Nhm II: A, C, D.
A. Ph t ngoi (Ph lc 3.1) trong khong t 230 n 350 nm trong cc o
dy 2 cm ca dung dch 0,0015% trong dung dch acid hydrocloric 0,01 M ch c
mt cc i hp th 263 nm v A (1%, 1 cm) bc sng 263 nm khong 285.
ngoi ca nikethamid chun.
C. un nng 0,1 g ch phm vi 1 ml dung dch natri hydroxyd 2 M.
Diethylamin c to ra c th nhn bit bng mi c trng v bng s chuyn
mu giy qu thnh xanh.
D. Thm 2 ml dung dch cyanogen bromid (TT) v 3 ml dung dch anilin
2,5% vo 2 ml dung dch ch phm 0,1% v lc, mu vng xut hin.
pH
pH ca dung dch 25% t 6,0 n 7,8 (Ph lc 5.9).
Ch phm dng lng hoc c lm lng bng cch un nng nh phi

trong (Ph lc 5.12) v khng c m mu hn mu ca mu mu V5 (Ph lc
5.17, phng php 2).
Ch s khc x
T 1,524 n 1,526 (Ph lc 5.7).
Tp cht lin quan
Dung mi khai trin: Propanol - cloroform (25: 75).
Dung dch th: Ho tan 0,4 g ch phm trong methanol (TT) v pha long
vi methanol (TT) va 10,0 ml.
Dung dch i chiu (1): Ho tan 40 mg ethylnicotinamid chun trong
methanol (TT) v thm methanol (TT) va 100,0 ml.
Dung dch i chiu (2): Ht chnh xc 1,0 ml dung dch i chiu (1) pha
thnh 10,0 ml bng methanol (TT).
Cch tin hnh: Chm ring bit ln bn mng 10 l cc dung dch trn.
Trin khai sc k n khi dung mi i c 15 cm, ly ra kh ngoi khng kh.
Quan st di nh sng t ngoi bc sng 254 nm. Bt k vt no tng ng
vi ethylnicotinamid trn sc k ca dung dch th khng c m mu hn
vt trn sc k ca dung dch i chiu (1) v bt k vt ph khc ngoi vt
chnh v vt tng ng vi ethylnicotinamid khng c m mu hn vt trn
sc k ca dung dch i chiu (2).
Kim loi nng
Ly 12 ml dung dch ch phm 10% trong nc tin hnh th theo phng

php 1. Dng dung dch ch mu 1 phn triu chun b mu i chiu.
Nc
Dng 2,000 g ch phm.
Tro sulfat
Dng 1,0 g ch phm.
nh lng
Ho tan 0,150 g ch phm trong hn hp gm 20 ml acid acetic khan (TT)
v 5 ml anhydrid acetic (TT). Chun bng dung dch acid percloric 0,1 N. Xc
nh im kt thc bng phng php chun o in th (Ph lc 6.12).
C10H14N2O.
Bo qun
58-PARACETAMOL
Paracetamolum
C8H9NO2
P.t.l: 151,2
Paracetamol l N - (4 - hydroxyphenyl) acetamid, phi cha t 99,0 n

101,0% C8H9NO2, tnh theo ch phm lm kh.
Tnh cht
Bt kt tinh trng, khng mi. Hi tan trong nc, rt kh tan trong
cloroform, ether, d tan trong dung dch kim, ethanol 96%.
nh tnh
Nhm I: A v E.
Nhm II: B, C, D v E.
ngoi ca paracetamol chun.
B. Ho tan 50 mg ch phm trong methanol (TT) va 100,0 ml. Ly 1,0
ml dung dch, thm 0,5 ml dung dch acid hydrocloric 0,1 M (TT), thm methanol
(TT) va 100,0 ml. Bo qun dung dch ny trnh nh sng v em o hp
th (Ph lc 3.1) ngay tc khc bc sng 249 nm. A (1%, 1 cm) phi trong
khong 860 - 980.
C. un nng 0,1 g ch phm trong 1 ml acid hydrocloric (TT) trong 3 pht,
thm 10 ml nc, lm lnh, khng c ta to thnh. Thm 0,05 ml dung dch kali
dicromat 5% (TT), xut hin mu tm v khng chuyn sang mu .
D. Ch phm phi c phn ng ca nhm acetyl (Ph lc 7.1). Thc hin
phn ng bng cch un trc tip trn la.
E. im chy: 168 - 172oC (Ph lc 5.19).
Clorid
Khng c qu 0,010% (Ph lc 7.4.5).
Dung dch S: Lc 3,0 g ch phm vi 30 ml nc, lc.
Ly 5 ml dung dch S, thm nc va 15 ml v tin hnh th.
Sulfat
Khng c qu 0,020% (Ph lc 7.4.12).

Ly 7,5 ml dung dch S, thm nc va 15 ml v tin hnh th.
Kim loi nng
Ho tan 1,0 g ch phm trong hn hp gm 15 th tch nc v 85 th tch
aceton (TT) ri pha long vi cng dung mi va 20 ml. Ly 12 ml dung dch
ny th theo phng php 2. Dng dung dch ch mu 1 phn triu thu c bng
cch pha long dung dch ch mu 100 phn triu vi hn hp dung mi trn
chun b mu i chiu.
4 - Aminophenol
Ho tan 0,50 g ch phm trong hn hp methanol (TT) - nc (50: 50) va
10,0 ml. Thm 0,2 ml dung dch c cha natri nitroprusiat (TT) 10 g/l v natri
carbonat khan (TT) 10 g/l mi pha. Trn u v yn 30 pht. Song song chun
b mu i chiu trong cng iu kin, tin hnh vi 10,0 ml hn hp methanol
(TT) - nc (50 : 50) cha 0,50 g paracetamol khng c 4 - aminophenol v 0,5
ml dung dch 4 - aminophenol 0,05 g/l trong hn hp methanol (TT) - nc (50 :
50). Mu xanh ca dung dch th khng c m hn mu ca dung dch i
chiu.
Tp cht lin quan
Bn mng: Silicagel HF254.
Dung mi khai trin: Methanol - 1,1,1-tricloroethan - diisopropyl ether (10:
40: 50).
Dung dch th (1): Cho 1,0 g ch phm nghin mn vo ng ly tm bng

thy tinh hay polytetra-fluoroethylen, thm 5 ml ether khng c peroxyd (TT), lc
30 pht, ly tm 15 pht hay cho n khi thu c lp dung dch trn trong sut.
Dung dch th (2): Ho tan 0,10 g ch phm trong methanol (TT) va 4
ml.
Dung dch i chiu (1): Ho tan 50 mg cloroacetanilid trong methanol
(TT) va 10,0 ml. Ly 2,0 ml dung dch ny pha long thnh 100 ml vi
methanol (TT).
Dung dch i chiu (2): Pha long 5,0 ml dung dch i chiu (1) thnh 8
ml bng methanol (TT).
Dung dch i chiu (3): Ho tan 0,25 g cloroacetanilid v 0,1 g ch phm
trong methanol (TT) va 100 ml.
Cch tin hnh: Chm ring bit ln bn mng 20 l mi dung dch trn,
ring dung dch th (1) chm 200 l. Trin khai sc k ngay tc khc trong bnh
khng bo ho, n khi dung mi i c 10 cm. kh bn mng ngoi khng
kh. Quan st di nh sng t ngoi bc sng 254 nm, bt c vt no tng
ng vi cloroacetanilid trong sc k ca dung dch th (1) khng c m
mu hn vt thu c t sc k ca dung dch i chiu (1) (0,05%), bt c vt
no trong sc k ca dung dch th (2), ngoi vt chnh v vt tng ng vi
cloroacetanilid, khng c m mu hn vt thu c t sc k ca dung dch
i chiu (2) (0,25%). Php th ch c gi tr khi sc k thu c t dung dch
i chiu (3) c 2 vt r rng ring bit.
Mt khi lng do lm kh
Khng c qu 0,5% (Ph lc 5.16).
(1,000 g; 100 - 105oC).
Tro sulfat

Dng 1,0 g ch phm.
nh lng
Ho tan 0,300 g ch phm trong hn hp gm 10 ml nc v 30 ml dung
dch acid sulfuric long (TT). un si hi lu trong 1 gi, lm lnh v pha long
vi nc va 100,0 ml. Ly 20,0 ml dung dch, thm 40 ml nc, 40 g nc ,
15 ml dung dch acid hydrocloric long (TT) v 0,1 ml dung dch feroin (CT).
nh lng bng dung dch amoni ceri sulfat 0,1 M cho n khi xut hin mu
vng. Song song tin hnh mu trng trong cng iu kin.
1 ml dung dch amoni ceri sulfat 0,1 M tng ng vi 7,56 mg
C8H9NO2.
Bo qun
Ch phm
Vin nn, vin bao phim, hn dch ung, dung dch ung, vin nn si bt.
Cng dng
H nhit, gim au
59-PEPSIN
Pepsinum
Pepsin l ch phm cha men tiu protein, ly t nim mc cn ti ca d
dy ln, tru, b hoc cu, tc dng trong mi trng acid (pH t 1 n 5), phi c
hot lc khng t hn 0,5 n v trong 1 mg, tnh theo ch phm lm kh.
Pepsin c iu ch trong nhng iu kin nht nh, hn ch ti a
nhim khun.
Tnh cht
Bt kt tinh hoc v nh hnh, trng hay vng nht, ht m.

Ch phm tan trong nc cho mt dung dch c l v c phn ng acid
yu, thc t khng tan trong ethanol 96% v ether.
nh tnh
Cho 1 ml fibrin congo ln mt giy lc v ra bng mt dung dch c
iu ch bng cch pha long 30 ml dung dch acid hydrocloric 1 M vi nc
c 1000 ml v iu chnh pH n gia 1,5 v 1,7, n khi nc ra khng cn
mu. Chc thng giy lc v trng fibrin congo qua l thng bng 20 ml dung
dch acid hydrocloric trn. Lc hn hp ny trc khi dng. Ho tan mt lng
ch phm khng t hn 20 n v hot lc trong 2 ml dung dch acid hydrocloric
trn v iu chnh pH n gia 1,5 v 1,7 (Dung dch th). Cho vo hai ng
nghim, mi ng 4 ml hn dch fibrin congo. Thm vo mt ng 1 ml dung
dch th v ng cn li 1 ml nc (mu trng). Trn u cc ng v cho vo ni
cch thu 25oC, lc nh trong 15 pht. Dung dch mu trng khng c mu v
dung dch th phi c mu xanh tm.
Mt khi lng do lm kh
Khng c qu 5,0% (Ph lc 5.16).
(0,500 g; phosphor pentoxyd; p sut khng qu 0,7 kPa; 60oC; 4 gi).
Gii hn vi khun
1,0 g ch phm khng c c Escherichia coli v 10 g ch phm khng
c c Salmonella (Ph lc 10.7).
nh lng
Hot lc ca pepsin c xc nh bng phng php sinh hc, bng cch
so snh lng peptid khng b kt ta bi dung dch acid tricloroacetic 4,0%, c
gii phng t mt c cht l hemoglobin bi tc dng ca ch phm v tc dng
ca cht chun trong cng mt thi gian v iu kin. Cc peptid c gii

phng ny c nh lng bng thuc th phosphomo-libdotungstic.
Ch trnh lc v lm si bt cc dung dch th v dung dch chun trong
qu trnh nh lng.
Cch tin hnh:
Dung dch chun cha 0,5 n v hot lc trong 1 ml dung dch c iu
ch bng cch pha long 30 ml dung dch acid hydrocloric 1 M thnh 1000 ml vi
nc v iu chnh pH n gia 1,5 v 1,7. Nu cn thit iu chnh pH ca dung
dch cui n gia 1,5 v 1,7 bng dung dch acid hydrocloric 1 M. Dung dch ny
ch c dng trong vng 15 pht.
Dung dch th cha ch phm c nng v cch pha tng t nh dung
dch chun. Dng ngay sau khi pha.
Chun b 12 ng nghim c sn que khuy. nh du cc ng S1, S2, S3
cho dung dch chun; T1,T2, T3 cho dung dch th v BS1, BS2, BS3, BT1, BT2,
BT3 cho dung dch mu trng tng ng.
Cho tng 1 ml dung dch chun vo cc ng S1, S2, S3, BS1, BS2, BS3, v
tng 1 ml dung dch th vo cc ng T1, T2, T3, BT1, BT2, BT3.
vo cch thu cho cc dung dch t c nhit tng ng vi nhit
ni cch thu 24,9 n 25,10C th thm vo cc ng mu trng BS1, BS2,
BS3, BT1, BT2, BT3 mi ng 10 ml dung dch acid tricloroacetic 4,0 % c
lm m nhit 24,9 n 25,10C.
Ln lt cch nhau 30 giy, thm tng 5 ml dung dch hemoglobin (TT)
c lm m trong ni cch thu n gia 24,9 v 25,1oC vo cc ng S1, S2, S3,
T1, T2, T3, BS1, BS2, BS3 , BT1, BT2, BT3, khuy trn nh nhng tng ng.
ng 10 pht sau khi thm dung dch hemoglobin th ln lt cch nhau 30 giy
thm tng 10 ml dung dch acid tricloroacetic 4,0 % c lm m trong ni
cch thu n gia 24,9 v 25,1oC vo cc ng S1, S2, S3, T1,, T2, T3 v trn
u.
Mt giy lc thch hp t php th sau: Lc 5 ml dung dch acid
tricloroacetic 5% qua mt giy lc trng, trn 7 cm. hp th (Ph lc 3.1) ca
dch lc o 275 nm, dng dung dch acid tricloroacetic 5% cha lc lm mu
trng, phi t hn 0,04.
Lc dung dch trong mi ng 2 ln qua giy lc c ra trc bng
dung dch acid tricloroacetic 5%, sau bng nc v lm kh. B i 5 ml mi
dung dch lc u. Chuyn 3,0 ml cc dung dch lc sau vo mi ng cha sn 20
ml nc. Trn u v thm 1,0 ml dung dch natri hydroxyd 20,0% v 1,0 ml
thuc th phosphomolybdotungstic (TT). Tin hnh theo trnh t cc ng BS1,
BS2, BS3 trc cc ng S1,S2, S3 v cc ng BT1, BT2, BT3 trc cc ng T1,,
T2, T3 v trn u.
Sau t nht 15 pht, o hp th (Ph lc 3.1) ca cc dung dch S1, S2,
S3, T1,, T2, T3 540 nm, so vi mi dung dch mu trng tng ng.
Php th ch c gi tr khi cc hp th o c nm gia 0,30 v
0,40.Tnh hp th trung bnh ca cc dung dch chun S1, S2, S3 v ca cc
dung dch th T1, T2, T3.
Bo qun
ng trong l kn, trnh nh sng v nhit t 2 n 80C.
60-PETHIDIN HYDROCLORID
Pethidini hydrochloridum
C15H21NO2.HCl
P.t.l: 283,8
Pethidin hydroclorid l ethyl - 1 - methyl - 4 - phenyl - piperidin - 4 carboxylat hydroclorid, phi cha t 99,0 n 101,0% C15H21NO2.HCl, tnh theo
ch phm lm kh.
Tnh cht
Bt kt tinh trng
Rt d tan trong nc, d tan trong ethanol 96%, thc t khng tan trong
ether.
nh tnh
Nhm I: B v D.
Nhm II: A,C v D.
A. im chy ca ch phm phi t 187 n 190oC (Ph lc 5.19).
ngoi i chiu ca pethidin hydroclorid.
C. Ho tan 0,1 g ch phm trong 10 ml ethanol (TT) v thm 10 ml dung
dch acid picric 1%. Ta tinh th thu c sau khi ra vi nc v sy kh 100
n 105oC chy trong khong 186 n 193oC. Trn u ng lng ta thu c
v ch phm, xc nh im chy ca hn hp. im chy ca hn hp phi thp
hn im chy ca ta t nht l 20oC (Ph lc 5.19).
D. Thm 5 ml nc vo 5 ml dung dch S. Dung dch ny cho phn ng A
ca ion clorid (Ph lc 7.1).
(TT) v pha long thnh 25 ml vi cng dung mi.
php 2).
Gii hn acid - kim
Thm 0,2 ml dung dch methyl (CT) v 0,2 ml dung dch natri hydroxyd
0,01 M vo 10 ml dung dch S. Dung dch ny mu vng. Thm 0,3 ml dung dch
acid hydrocloric 0,01 M, dung dch chuyn sang .
Tp cht lin quan
Khng c qu 1,0%.
Bn mng: Kieselguhr G c hot ho bng cch t bn mng vo bnh
sc k c cha mt lng thch hp hn hp dung mi gm: 10 th tch
phenoxyethanol v 90 th tch aceton sao cho bn mng ngp trong dung mi 5
mm. Khi dung mi i c t nht l 15 cm, ly bn mng ra v lm kh trong
lung kh, bn mng phi dng ngay. Tin hnh sc k cng mt chiu nh khi
hot ho.
Dung mi khai trin: Dng lp trn ca hn hp Diethylamin phenoxyethanol - ether du ho (1: 8: 100).
Dung dch th: Ho tan 0,1 g ch phm trong 5 ml nc, thm 0,5 ml dung
dch natri hydroxyd 10 M v 2 ml ether, lc. tch lp. Dng lp trn lm dung
dch th.
Dung dch i chiu: Pha long 0,5 ml dung dch th thnh 50 ml bng
ether (TT).
Cch tin hnh: Chm ring bit 5l mi dung dch trn ln bn mng.
Trin khai n khi dung mi i c 12 cm. kh bn mng trong khng kh 10
pht v chy nhc li. kh bn mng trong khng kh 10 pht v phun dung
dch diclorofluorescein 0,2% trong methanol (TT). bn mng 5 pht v phun
nc n khi bn mng mu trng hay vng nht. Quan st di nh sng ban

ngy, trn bn mng c nhng vt mu hay da cam. Bt k vt ph no ca
dung dch th khng c m mu hn vt ca dung dch i chiu. Quan st
ngay di nh sng t ngoi bc sng 365 nm, trn bn mng c nhng vt
pht quang mu vng m. Bt k vt ph no ca dung dch th khng c m
mu hn vt ca dung dch i chiu.
Mt khi lng do lm kh
Khng c qu 0,5% (Ph lc 5.16).
(1,000 g; 100 - 105oC).
Tro sulfat
Dng 1,0 g ch phm.
nh lng
dung dch thu ngn (II) acetat (TT). Chun bng dung dch acid percloric 0,1
N, dng 0,1 ml dung dch tm tinh th (CT) lm ch th, n khi mu chuyn t
xanh tm sang xanh lc.
C15H21NO2.HCl.
Bo qun
Thuc gy nghin. ng trong ng kn, trnh nh sng.
61-PHENOBARBITAL
Phenobarbitalum
C12H12N2O3
P.t.l: 232,2
Phenobarbital l acid 5- ethyl - 5 - phenylbarbituric, phi cha t 99,0 n

101,0% C12H12N2O3, tnh theo ch phm lm kh.
Tnh cht
Tinh th khng mu hay bt kt tinh trng, khng mi.
Rt kh tan trong nc, hi tan trong cloroform, tan trong ether, d tan
trong ethanol 96%. To thnh hp cht tan trong nc vi hydroxyd, carbonat
kim v vi amoniac.
nh tnh
Nhm I: A v B.
Nhm II: B,C v D.
A. Xc nh im chy (Ph lc 5.19) ca ch phm v ca hn hp ng
lng ch phm vi phenobarbital chun. im chy ca ch phm v ca hn
hp phi khong 176oC. S khc bit v im chy ca 2 mu trn khng c
qu 2oC.
ngoi ca phenobarbital chun.
Dung mi khai trin: l lp di ca hn hp gm Amoniac m c ethanol 96% - cloroform (5: 15: 80).
Dung dch th: Ho tan 0,1 g ch phm trong ethanol 96% (TT) c
100 ml.
Dung dch i chiu: Ho tan 0,1 g phenobarbital chun trong ethanol 96%
(TT) c 100 ml.
Trin khai sc k ti khi dung mi i c khong 18 cm. Quan st ngay bn
mng di nh sng t ngoi bc sng 254 nm. Vt chnh ca sc k thu
c t dung dch th phi ging nhau v v tr v kch thc vi vt chnh ca
sc k thu c t dung dch i chiu.
D. Phn ng c trng ca barbiturat c hydro nhm NH khng b thay
th (Ph lc 7.1).
Ho tan 1,0 g ch phm trong hn hp gm 4 ml dung dch natri hydroxyd
2 M v 6 ml nc. Dung dch phi trong (Ph lc 5.12) v mu khng c m
hn mu mu V6 (Ph lc 5.17, phng php 2).
Gii hn acid
un si 1,0 g ch phm vi 50 ml nc trong 2 pht, ngui ri lc.
Thm 0,15 ml dung dch methyl (CT) vo 10,0 ml dch lc, dung dch c mu
vng cam. chuyn sang mu vng, th tch dung dch natri hydroxyd 0,1 N s
dng khng c qu 0,1 ml.
Tp cht lin quan
Khng c qu 0,5%.
Dung mi khai trin: L lp di ca hn hp gm Amoniac m c ethanol 96% - cloroform (5: 15: 80).
Dung dch th: Ho tan 1,0 g ch phm trong ethanol 96% (TT) v pha
long n 100 ml bng cng dung mi.
ethanol 96% (TT).
Trin khai sc k ti khi dung mi i c khong 15 cm. Quan st ngay bn
mng di nh sng t ngoi bc sng 254 nm, phun thuc th
diphenylcarbazon thu ngn (TT). kh bn mng ngoi khng kh, phun dung
dch kali hydroxyd trong ethanol (TT) va mi pha. Sy bn mng 100 - 105oC
trong 5 pht, quan st ngay tc khc. Khi quan st di nh sng t ngoi hoc
sau khi phun thuc th, bt c vt ph no trn sc k thu c t dung dch
th khng c m mu hn vt trn sc k thu c t dung dch i chiu.
Mt khi lng do lm kh
Khng c qu 1,0% (Ph lc 5.16).
(1,000 g; 100 - 105oC; 2 gi).
Tro sulfat
Dng 1,0 g ch phm.
nh lng
Ho tan 0,100 g ch phm trong 5 ml pyridin (TT), thm 0,5 ml dung dch
thymolphtalein (CT) v 10 ml dung dch bc nitrat 8,5% trong pyridin. Chun
bng dung dch natri hydroxyd 0,1 N trong ethanol n khi c mu xanh. Song
song lm mu trng.
1 ml dung dch natri hydroxyd 0,1 N trong ethanol tng ng vi 11,61
mg C12H12N2O3.
Bo qun
Trong chai l kn.
Ch phm
Cn thuc phenobarbital. Vin nn phenobarbital.
Tc dng v cng dng
An thn, chng co git.
62- PHENOL
Phenolum
C6H6O
P.t.l: 94,1
Phenol phi cha t 99,0 n 100,5% C6H6O.

Tnh cht
Tinh th hoc khi kt tinh khng mu hay mu hng nht, c mi c
trng, d chy lng.
Tan trong nc, rt tan trong dicloromethan, ethanol 96% v glycerin.
nh tnh
A. Ho tan 0,5 g ch phm trong 2 ml dung dch amoniac 13,5 M (TT),
phi tan hon ton. Pha long vi nc thnh 100 ml. Ly 2 ml dung dch ny,
thm 0,05 ml dung dch natri hypoclorit (3% Cl) xut hin mu xanh v mu ny
m dn.
B. Ly 1 ml dung dch S, thm 10 ml nc v 0,1 ml dung dch st (III)
clorid 10,5%, xut hin mu tm v mu ny mt i khi thm 5 ml propan-2-ol.
C. Ly 1 ml dung dch S, thm 10 ml nc v 1 ml nc brom (TT) s c

ta mu vng nht.
Dung dch S: Ho tan 1,0 g ch phm trong nc va c 15 ml.
mu N6 (Ph lc 5.17, Phng php 2).
Gii hn acid
Thm 0,05 ml dung dch da cam methyl (CT) vo 2 ml dung dch S. Dung
dch phi c mu vng.
im ng c
Khng c di 39,5oC (Ph lc 5.18).
Cn sau khi bay hi
Khng c qu 0,05%.
Ly 5,000 g ch phm lm bay hi n kh trn cch thu v sy 100 105oC trong 1 gi.
nh lng
Ho tan 2,000 g ch phm trong nc c 1000,0 ml. Chuyn 25,0 ml
dung dch ny vo 1 bnh thu tinh c nt mi. Thm 50,0 ml dung dch brom 0,1
N v 5 ml acid hydrocloric (TT). y bnh v 30 pht (thnh thong lc), sau
yn 15 pht na. Thm 5 ml dung dch kali iodid 20%, lc v chun bng
dung dch natri thiosulfat 0,1 N cho n mu vng nht. Thm 0,5 ml dung dch h
tinh bt (CT) v 10 ml cloroform (TT), tip tc va chun va lc mnh.
Song song lm mu trng.
1 ml dung dch brom 0,1 N tng ng vi 1,569 mg C6H6O.
Bo qun

Tc dng v cng dng
St trng.
63- PHENYTOIN
Phenytoinum
C15H12N2O2
P.t.l: 252,3
Phenytoin l 5,5-diphenylimidazolidin-2, 4-dion, phi cha t 99,0 n

101,0% C15H12N2O2, tnh theo ch phm lm kh.
Tnh cht
Bt kt tinh trng hoc gn nh trng, khng mi hoc gn nh khng mi.
Thc t khng tan trong nc, hi tan trong ethanol 96%, kh tan trong
cloroform v ether. Rt kh tan trong methylen clorid. Tan trong cc dung dch
hydroxyd kim long.
nh tnh
Nhm I: A.
Nhm II: B, C v D.
ngoi ca phenytoin chun.
B. Trong mc th "Tp cht lin quan", vt chnh trong sc k thu c
ca dung dch th (2) phi c v tr v kch thc ging vi vt chnh trong sc k
thu c ca dung dch i chiu (1).
C. Cho vo 10 mg ch phm 1 ml nc v 0,05 ml amoniac (TT). un n

si, thm 0,05 ml dung dch ng sulfat 5% trong dung dch amoniac 2 M (TT) v
lc u. Ta kt tinh mu hng xut hin.
Dung dch ca 1,0 g ch phm trong hn hp gm 20 ml nc v 5 ml dung
dch natri hydroxyd 1 M phi trong (Ph lc 5.12) v khng c c mu m hn
mu ca mu mu NV6 (Ph lc 5.17, phng php 2).
Gii hn acid - kim
Thm 45 ml nc vo 1,0 g ch phm, un si khong 2 pht, ngui v
lc. Ra phu lc bng nc khng c carbon dioxyd (TT). Pha long dch lc v
nc ra phu lc bng nc khng c carbon dioxyd (TT) thnh 50 ml. Ly 10
ml dung dch thu c v thm 0,15 ml dung dch methyl (CT), mu ca ch th
phi chuyn sang mu khi thm khng qu 0,5 ml dung dch acid hydrocloric
0,01 M. Ly 10 ml dung dch thu c v thm 0,15 ml dung dch xanh
bromothymol (CT), mu ca ch th phi chuyn sang mu xanh lam khi thm
khng qu 0,5 ml dung dch natri hydroxyd 0,01 M.
Kim loi nng
Tp cht lin quan
Bn mng: Silicagel GF254. Trc khi dng, ra bn mng bng hn hp
gm 30 ml dioxan (TT) v 75 ml hexan (TT). bn mng kh ngoi khng kh.
Dung mi khai trin: Dioxan - hexan (30: 75).
Dung mi ho tan mu: Hn hp gm aceton (TT) v methanol (TT) ng

th tch.
Dung dch th (1): Ho tan 0,40 g ch phm trong dung mi ho tan mu
c 10 ml.
Dung dch th (2): Pha long 1 ml dung dch th (1) thnh 20 ml bng dung
mi ho tan mu.
Dung dch i chiu (1): Ho tan 20 mg phenytoin chun trong dung mi
ho tan mu c 10 ml.
Dung dch i chiu (2): Ho tan 8 mg benzophenon trong dung mi ho
tan mu c 100 ml.
Dung dch i chiu (3): Ho tan 8 mg benzil trong dung mi ho tan mu
c 100 ml.
Dung dch i chiu (4): Pha long 1 ml dung dch th (1) thnh 100 ml
bng dung mi ho tan mu.
Dung dch i chiu (5): Trn u 1 ml dung dch i chiu (2) v 1 ml
Cch tin hnh:
Chm ring bit ln bn mng 10 l mi dung dch trn, dng lung kh
lnh lm kh bn mng trong khong 2 pht. Trin khai sc k n khi dung
mi i c 15 cm. bn mng kh ngoi khng kh v quan st di nh sng
t ngoi bc sng 254 nm. Trn sc k ca dung dch th (1) cc vt tng
ng vi vt ca benzophenon v benzil khng c m mu hn vt thu c
trn sc k ca dung dch i chiu (2) v (3) (0,2%), cc vt ph khc tr vt
chnh v vt tng ng vi benzophenon v benzil khng c m mu hn vt
thu c trn sc k ca dung dch i chiu (4) (1%). Php th ch c gi tr
khi sc k thu c ca dung dch i chiu (5) cho thy 2 vt tch r rng.
Mt khi lng do lm kh
Khng c qu 0,5% (Ph lc 5.16).
(1,000 g; 105oC).
Tro sulfat
Dng 1,0 g ch phm.
nh lng
Ho tan 0,200 g ch phm trong 50 ml dimethyl-formamid (TT). Chun
bng dung dch natri methoxyd 0,1 M. Xc nh im kt thc bng phng php
chun o in th (Ph lc 6.12).
1 ml dung dch natri methoxyd 0,1 M tng ng vi 25,23 mg
C15H12N2O2.
Bo qun
ng trong bnh kn.
64-PHYTOMENADION
Phytomenadionum
Vitamin K1
C31H46O2 P.t.l: 450,71

Phytomenadion l 2 - methyl - 3 - [(2E, 7R, 11R) - 3,7,11,15 - tetramethyl 2 - hexadecanyl] - 1,4 - naphtoquinon, phi cha t 97,0 n 102,0% C31H46O2.
Tnh cht
Cht lng nht, trong, mu vng hoc vng cam, khng mi.
D tan trong ether, isooctan, cloroform v du bo.
Hi tan trong ethanol v methanol, thc t khng tan trong nc. N b
phn hu dn dn v b sm mu do nh sng. T trng khong 0,967.
nh tnh
A. Ho tan 0,05 g ch phm trong 10 ml ethanol (TT) v thm 1 ml dung
dch kali hydroxyd trong ethanol (TT) (1: 10), xut hin mu xanh, chuyn sang
ta, lu chuyn thnh nu.
B. Ho tan 0,05 g ch phm trong 10 ml hn hp methanol v ether (1: 1).
Thm mt dung dch mi pha ca 0,75 g natri hydrosulfit (TT) trong 2 ml nc
m v lc mnh, mu vng mt ngay.
C. Ph hp th t ngoi (Ph lc 3.1) ca dung dch ch phm trong
isooctan (1: 100.000) c cc cc i hp th trong khong 242,0 nm v 244,0 nm,
khong 247,5 nm v 249,5 nm, khong 260,0 nm v 262,0 nm, khong 269,0 nm
v 271,0 nm. Ph hp th t ngoi ca dung dch ch phm trong isooctan (1:
10.000) c 1 cc i hp th trong khong 324,0 nm v 327,0 nm.
Ch s khc x
1,525 - 1,529 (Ph lc 5.7).
Ho tan 1,0 g ch phm trong 10 ml isooctan (TT). Dung dch thu c
phi trong (Ph lc 5.12) v cho mu vng.
Gii hn acid - kim
Ho tan 1,0 g ch phm trong 20 ml ethanol (TT). Dung dch ny phi
trung tnh i vi giy qu.
T l ca cc hp th nh sng
Xc nh hp th nh sng A1, A2, A3 ca dung dch ch phm trong
isooctan (1: 100.000) 248,5 nm, 253,5 nm v 269,5 nm; t l A2/A1 phi gia
0,69 v 0,73; t l A2/A3 gia 0,74 v 0,78. Xc nh hp th A4 v A5 ca
dung dch ch phm trong isooctan (1: 10.000) 284,5 nm v 326,0 nm, t l
A4/A5 phi gia 0,28 v 0,34.
Tp cht lin quan
Xc nh bng phng php sc k lp mng (Ph lc 4.4). (Tin hnh
di nh sng du).
Dung mi khai trin: Cyclohexan - ether - methanol (80: 20: 1).
Dung dch th: Dung dch ch phm 0,50% trong isooctan (TT).
Dung dch i chiu: Dung dch menadion 0,0050% trong isooctan (TT).
Cch tin hnh:
Chm ring bit ln bn mng 10 l mi dung dch trn. Trin khai sc k
n khi dung mi i c khong 15 cm, ly bn mng ra, kh ngoi khng kh
v quan st di nh sng t ngoi bc sng 254 nm. Bt c vt ph no trn
sc k ca dung dch th khng c m mu hn vt trn sc k ca dung
dch i chiu.
Tro sulfat
Dng 1,0 g ch phm.
nh lng
Tin hnh trong nh sng du.
Ho tan 0,100 g ch phm trong isooctan (TT) v thm cng dung mi va

100,0 ml. Ly chnh xc 10,0 ml dung dch ny v cho isooctan (TT) va
100,0 ml. Ly chnh xc 10,0 ml dung dch sau v cho cng dung mi cho va
100,0 ml. o hp th (Ph lc 3.1) ca dung dch ny bc sng cc i 249
nm, rng ca khe ph l 1,0 nm. Tnh hm lng ca C31H4602 theo A (1%, 1
cm), ly 410 l gi tr ca A (1%, 1 cm) bc sng 249 nm.
Bo qun
ng trong chai tht kn v trnh nh sng.
65- PILOCARPIN NITRAT
Pilocarpini nitras
C11H16N2O2. HNO3
P.t.l: 271,3
Pilocarpin
(3S,4R)-3-ethyl-4-[(1-methyl-1H-imidazol-5-yl)
nitrat
methyl]-dihydro-3H-furan-2-on
nitrat,
phi
cha
98,5
101,0%
C11H16N2O2. HNO3, tnh theo ch phm lm kh.

Tnh cht
Bt kt tinh trng hoc tinh th khng mu, khng mi hoc mi nh, v
ng. Chu tc ng ca nh sng v m. Ngay ni thiu nh sng, ch phm
cng b phn hu t t khi tip xc vi khng kh m. S phn hu xy ra nhanh
hn nhit cao.
D tan trong nc, hi tan trong ethanol 96%, thc t khng tan trong
cloroform v ether. Dung dch pilocarpin nitrat kh bn vng pH t 4 n 5.
Chy khong 174oC km theo phn hu.

nh tnh
Nhm I: A, B, E.
Nhm II: A, C, D, E.
A. Gc quay cc ring:
T + 80,0 n + 83,0o (Ph lc 5.13). Th trn dung dch S v tnh theo
ch phm lm kh.
ngoi ca pilocarpin nitrat chun.
C. Quan st sc k thu c trong phn th "Tp cht lin quan": vt
chnh ca dung dch th (2) phi tng t v v tr, mu sc v kch thc so vi
vt chnh ca dung dch i chiu (1).
D. Pha long 0,2 ml dung dch S bng nc va 2 ml. Thm 0,05 ml
dung dch kali dicromat 5% (TT), 1 ml dung dch hydrogen peroxyd long (TT), 2
ml cloroform (TT) v lc. Mu tm s xut hin trong lp cloroform.
E. Ch phm cho phn ng ca nitrat (Ph lc 7.1).
(TT) v pha long n 50,0 ml vi cng dung mi. Pha ngay trc khi dng.
pH
Tp cht lin quan

Khng c qu 1,0%,.
Dung mi khai trin: Amoniac m c - methanol - cloroform (1: 14: 85).
Dung dch th (1): Ho tan 0,3 g ch phm trong nc va 10 ml
Dung dch th (2): Pha long 0,5 ml dung dch th (1) vi nc va 15
ml.
Dung dch i chiu (1): Ho tan 10 mg pilocarpin nitrat chun trong nc
v pha long n 10 ml bng cng dung mi.
Dung dch i chiu (2): Pha long 3 ml dung dch i chiu (1) vi nc
va 10 ml.
Trin khai trong bnh sc k n khi dung mi i c khong 15 cm, ly bn
mng ra sy kh 100 n 105oC trong 10 pht. ngui v phun dung dch kali
iodobismuthat (TT).
Trn sc k , ngoi vt chnh, bt k vt ph no ca dung dch th (1)
khng c m mu hn vt ca dung dch i chiu (2).
Clorid
St
Khng qu 10 phn triu (Ph lc 7.4.11).
Ly 10 ml dung dch S tin hnh th, dng 5 ml dung dch st mu 1 phn

triu v 5 ml nc chun b mu i chiu.
Mt khi lng do lm kh
Khng c qu 0,5% (Ph lc 5.16).
(1,000 g; 100 - 105oC).
Tro sulfat
Dng 0,5 g ch phm.
nh lng
Ho tan 0,250 g ch phm trong 30 ml acid acetic khan (TT). Chun
bng dung dch acid percloric 0,1 N C. Xc nh im kt thc bng phng
php chun o in th (Ph lc 6.12) hoc bng ch th tm tinh th (CT)
im tng ng c mu xanh l. Song song lm mu trng v tin hnh nhng
hiu chnh cn thit.
C11H16N2O2. HNO3.
Bo qun
Trong chai l nt kn, trnh nh sng. Thuc c bng A.
Ch phm
Dung dch nh mt pilocarpin nitrat.
Tc dng v cng dng
Cht cng i giao cm. Thuc nh mt lm co ng t, h nhn p, tr
glaucom.
Ghi ch
Dng mui pilocarpin hydroclorid c cng tc dng v cng dng nh

pilocarpin nitrat.
66-PIPERAZIN ADIPAT
Piperazini adipas
C4Hl0N2. C6H10O4
P.t.l: 232,3
Piperazin adipat phi cha t 98,0 n 10l,0% C4H10N2. C6H10O4, tnh

theo ch phm khan.
Tnh cht
Bt kt tinh trng, chy khong 250oC km theo phn hy. Tan trong
nc, thc t khng tan trong ethanol 96%.
nh tnh
Nhm I: B v C.
Nhm II: A.
ngoi ca piperazin adipat chun.
B. Trong php th "Tp cht lin quan", sau khi phun cc dung dch
ninhydrin th vt chnh trn sc k thu c t dung dch th (2) phi tng t
v mu sc, v tr, kch thc vi vt chnh trn sc k thu t dung dch i
chiu (1).
C. Ly l0 ml dung dch S, thm 5 ml acid hydrocloric (TT) v chit 3 ln,
mi ln vi l0 ml ether (TT). Gp dch chit v bc hi cho ti kh. Ra cn vi 5
ml nc v sy kh 100 - l05OC. im chy (Ph lc 5.19) ca cn l 150 154oC.

Dung dch S: Ho tan 2,5 g ch phm trong nc c 50 ml.
Dung dch S phi trong (Ph lc 5.12) v khng m mu hn mu mu N8
(Ph lc 5.17, phng php 2).
Kim loi nng
Tp cht lin quan
Dung mi khai trin: Amoniac m c - aceton (20: 80) va mi pha.
Dung mi ho tan: Ethanol - amoniac m c (2: 3).
Dung dch th (1): Ho tan 1,0 g ch phm trong 6 ml amoniac m c
(TT) v pha long bng ethanol thnh 10 ml.
Dung dch th (2): Pha long 1 ml dung dch th (1) bng dung mi ho tan
thnh 10 ml.
Dung dch i chiu (1): Ho tan 0,1 g piperazin adipat chun trong dung
mi ho tan c 10 ml.
Dung dch i chiu (2): Ho tan 25 mg ethylendiamin trong dung mi ho
tan c 100 ml.
Dung dch i chiu (3): Ho tan 25 mg triethylendiamin trong dung mi
ho tan c 100 ml.
Dung dch i chiu (4): Ho tan 12,5 mg triethylendiamin trong 5,0 ml

dung dch th (1) v pha long bng dung mi ho tan thnh 50 ml.
Trin khai sc k n khi dung mi i c 15 cm. Sy bn mng 1050C v
phun ln lt dung dch ninhydrin 0,3% trong hn hp acid acetic khan v butanol
(3 : 100), dung dch ninhydrin 0,15% trong ethanol. Sy bn mng 1050C
trong10 pht.
Trn sc k bt k vt ph no ca dung dch th (1) khng c m
mu hn vt ca dung dch i chiu (2) (0,25%).
Phun ln bn mng dung dch iod 0,1 N v khong 10 pht. Vt tng
ng vi triethylendiamin ca dung dch th (1) khng c m mu hn vt ca
dung dch i chiu (3). Php th ch c gi tr khi dung dch i chiu (4) cho 2
vt tch r rng.
Tro sulfat
Khng c qu 0,l% (Ph lc 7.7, phng php 2).
Dng l,0 g ch phm.
Nc
Dng l,00 g ch phm.
nh lng
Ha tan 0,l00 g ch phm trong l0 ml acid acetic khan (TT) bng cch un
nng nh v pha long ti 70 ml bng cng dung mi. Chun bng dung dch
acid percloric 0,1 N (C) dng 0,25 ml dung dch 1 - naphtholbenzein (CT) lm
ch th, n khi mu chuyn t vng nu sang xanh l.
l ml dung dch acid percloric 0,lN tng ng vi 11,61 mg C4H10N2.
C6H10O4.
Bo qun
Trong chai l nt kn.
Tc dng
Tr giun sn.
67-PIPERAZIN CITRAT
Piperazini citras
(C4H10N2)3. 2C6H8O7
P.t.l: 643,0
Piperazin citrat phi cha t 98,0 n 101,0% (C4H10N2)3. 2C6H8O7,

tnh theo ch phm khan.
Tnh cht
Bt cm mu trng, sau khi sy kh 100- 1050C chy khong 1900C.
D tan trong nc, thc t khng tan trong ethanol 96% v ether.
nh tnh
Nhm I: B v C.
Nhm II: A.
ngoi ca piperazin citrat chun. Sy kh ch phm v chun 1200C trong 5 gi,
trnh m v o ph hng ngoi ngay.
B. Trong php th "Tp cht lin quan", sau khi phun cc dung dch
ninhydrin th vt chnh trn sc k thu c t dung dch th (2) phi tng t
v mu sc, v tr, kch thc vi vt chnh trn sc k thu c t dung dch
i chiu (1).
C. Ho tan 0,5 g ch phm trong 5 ml nc, dung dch ny cho phn ng

c trng ca citrat (Ph lc 7.1).
Dung dch S: Ho tan 1,25 g ch phm trong nc c 25 ml.
Dung dch S phi trong (Ph lc 5.12) v khng m mu hn mu ca
mu mu N8 (Ph lc 5.17, phng php 2).
Kim loi nng
Tp cht lin quan
Tin hnh th nh m t chuyn lun piperazin adipat trong thay
piperazin adipat chun bng piperazin citrat chun pha dung dch i chiu (1).
Tro sulfat
Dng 1,0 g ch phm.
Nc
T 10,0 n 14,0% (Ph lc 6.6).
Dng 0,300 g ch phm.
nh lng
Ho tan 0,100 g ch phm trong 10 ml acid acetic khan (TT) bng cch un
nng nh v pha long ti 70 ml bng cng dung mi. Chun bng dung dch
acid percloric 0,1 N (C) dng 0,25 ml dung dch 1 - naphtholbenzein (CT) lm
ch th, n khi mu chuyn t vng nu sang xanh l.

(C4H10N2)3. 2C6H8O7.
Bo qun
Trong chai l nt kn.
Tc dng
Tr giun sn.
68-PIPERAZIN HYDRAT
Piperazini hydras
C4H10N2.6H2O
P.t.l: 194,2
Piperazin hydrat phi cha t 98,0 n 101,0% C4H10N2. 6H2O.

Tnh cht
Tinh th khng mu, d chy nc.
D tan trong nc v ethanol 96%, rt kh tan trong ether.
Chy khong 430C.
nh tnh
Nhm I: A.
Nhm II: B v C.
ngoi ca piperazin hydrat chun. Sy ch phm v chun trn phosphor pentoxyd,
trong chn khng, trong 48 gi. Nghin thnh bt, trnh ht nc, p a v ghi
ph ngay.
B. Trong mc th "Tp cht lin quan", quan st bn mng sau khi phun
cc dung dch ninhydrin. Vt chnh ca dung dch th (2) phi c v tr, mu sc v
kch thc tng ng vi vt chnh ca dung dch i chiu (1).
C. Ho tan 0,5 g ch phm trong 5 ml dung dch natri hydroxyd long (TT),
thm 0,2 ml benzoyl clorid (TT) trn u. Tip tc thm tng phn 0,2 ml benzoyl
clorid (TT) n khi khng cn ta to thnh. Lc v ra ta bng tng lng nh
ca 10 ml nc. Ho tan ta trong 2 ml ethanol 96% (TT) nng, dung dch ny
vo 5 ml nc. yn 4 gi, lc, ra tinh th bng nc v sy kh 100 n
1050C. Tinh th chy 191 n 1960C (Ph lc 5.19).
(TT) c 20 ml.
Dung dch S phi trong (Ph lc 5.12) v c mu khng c thm hn
mu mu N8 (Ph lc 5.17, Phng php 2).
pH
Dung dch S c pH t 10,5 n 12,0 (Ph lc 5.9).
Tp cht lin quan
Tin hnh th nh m t chuyn lun piperazin adipat trong thay
piperazin adipat chun bng piperazin hydrat chun pha dung dch i chiu
(1).
Kim loi nng
Ly 12 ml dung dch S tin hnh th theo phng php 1. Dng dung dch
Tro sulfat

Dng 1,0 g ch phm.
nh lng
Ho tan 80,0 mg ch phm trong 10 ml acid acetic khan (TT) bng cch
un nng nh v pha long thnh 70 ml bng cng dung mi. Chun bng dung
dch acid percloric 0,1 N (C) vi ch th l 0,25 ml dung dch 1 - naphthol
benzein (CT) n khi mu chuyn t vng nu sang xanh lc.
1 ml dung dch acid percloric 0,1 N tng ng vi 9,705 mg C4H10N2.
6H2O.
Bo qun
Trong l kn v trnh nh sng.
69-PIPERAZIN PHOSPHAT
Piperazini phosphas
C4H10N2. H3PO4. H2O
P.t.l: 202,1
Piperazin phosphat phi cha t 98,5 n 100,5% C4H10N2. H3PO4, tnh

theo ch phm khan.
Tnh cht
Bt kt tinh trng, khng mi hoc gn nh khng mi.
Hi tan trong nc, thc t khng tan trong ethanol 96%.
nh tnh
A. Ho tan 0,1 g ch phm trong 5 ml nc, thm 0,5 g natri hydrocarbonat

(TT), 0,5 ml dung dch kali fericyanid 5% (TT) v 0,1 ml thu ngn (TT). Lc
mnh 1 pht v yn 20 pht. Mu dn dn xut hin.
B. Ho tan 0,2 g ch phm trong 5 ml dung dch acid hydrocloric 2 M (TT),
va khuy va thm 1 ml dung dch natri nitrit 50% (kl/tt) v lm lnh trong nc
15 pht, khuy nu cn thit to ta kt tinh. im chy (Ph lc 5.19) ca
tinh th (sau khi ra bng 10 ml nc v sy kh 105oC) khong 159oC.
C. Dung dch ca ch phm cho phn ng c trng ca ion phosphat (Ph
lc 7.1).
pH
Dung dch ch phm 1% c pH t 6,0 n 6,5 (Ph lc 5.9).
Kim loi nng
Ho tan 2,0 g ch phm trong 20 ml dung dch acid acetic 2 M (TT). Ly
12 ml dung dch ny th theo phng php 1. Dng dung dch ch mu 2 phn
triu chun b mu i chiu.
Nc
T 8,0 n 9,5% (Ph lc 6.6).
Dng 0,250 g ch phm.
nh lng
Ho tan 0,200 g ch phm trong hn hp gm 3,5 ml dung dch acid
sulfuric 0,5 M (TT) v 10 ml nc. Thm 100 ml dung dch acid picric (TT), un
nng trn cch thu 15 pht v yn 1 gi. Lc qua phu xp G4 v ra ta mi
ln bng 10 ml hn hp ng th tch ca dung dch bo ho acid picric (TT) v
nc, n khi nc ra khng cn phn ng ca ion sulfat. Ra ta 5 ln, mi ln
vi 10 ml ethanol (TT) v sy n khi lng khng i 100 n 105oC.
1 g cn tng ng vi 338,2 mg C4H10N2. H3PO4.

Bo qun
Trong l kn.
70-PRIMAQUIN DIPHOSPHAT
Primaquini diphosphas
C15H27N3O9P2
P.t.l: 455,3
Primaquin diphosphat l (RS) - 8 - (4 - amino - 1- methylbutylamino) - 6 methoxyquinolin diphosphat, phi cha t 98,5 n 101,5% C15H27N3O9P2, tnh
theo ch phm lm kh.
Tnh cht
Bt kt tinh mu da cam.
Tan trong nc, thc t khng tan trong ethanol 96% v trong ether.
Chy khong 2000C km theo phn hu.
nh tnh
Nhm I: A, C v D.
Nhm II: B v D.
A. Ho tan 15 mg ch phm trong dung dch acid hydrocloric 0,01 M (TT)
v pha long n 100,0 ml vi cng dung mi. Ph hp th nh sng (Ph lc 3.1)
ca dung dch thu c trong khong bc sng t 310 nm n 450 nm phi cho 2
cc i hp th 332 nm v 415 nm. hp th ring cc cc i ny ln lt

l t 45 n 52 v t 27 n 35. Pha long 5,0 ml dung dch ny n 50,0 ml bng
dung dch acid hydrocloric 0,01 M. Ph hp th t ngoi ca dung dch pha long
ny trong khong bc sng t 215 nm n 310 nm phi cho 3 cc i hp th
225 nm, 265 nm v 282 nm. hp th ring cc cc i ny ln lt l t 495
n 515, t 335 n 350 v t 330 n 345.
ngoi ca primaquin diphosphat chun. Chun b a mu o nh sau: Ho tan
ring bit 0,1 g ch phm v 0,1 g cht chun trong 5 ml nc, thm 2 ml dung
dch amoniac 2 M (TT), 5 ml cloroform (TT) v lc. Lm khan lp cloroform bng
cch lc qua 0,5 g natri sulfat khan (TT). Chun b a mu trng dng 0,3 g kali
bromid (TT). Nh tng git mt 0,1 ml lp cloroform ln a, cloroform bc
hi ht gia cc ln nh, ri lm kh a 500C trong 2 pht.
Dung mi khai trin: Amoniac m c - methanol - cloroform (1: 40: 60).
Php th c tin hnh cng nhanh cng tt trong iu kin trnh nh
sng. Dung dch th v chun ch pha trc khi dng.
Dung dch th: Ho tan 0,20 g ch phm trong 5 ml nc v pha long n
10 ml bng methanol (TT). Pha long 1 ml dung dch thu c n 10 ml vi mt
hn hp ng th tch nc v methanol (TT).
Dung dch i chiu: Ho tan 20 mg primaquin diphosphat chun trong 5
ml nc v pha long n 10 ml vi methanol (TT).
Cch tin hnh: Ra bn mng trc bng dung mi khai trin. bn
mng kh ngoi khng kh. Chm ring bit ln bn mng 5 l mi dung dch trn
v trin khai sc k n khi dung mi i c khong 15 cm. Ly bn mng ra
kh ngoi khng kh v quan st di nh sng t ngoi bc sng 254 nm. Vt
chnh trn sc k ca dung dch th phi tng ng v v tr v kch thc vi

vt chnh trn sc k ca dung dch i chiu.
D. Ho tan 50 mg ch phm trong 5 ml nc, thm 2 ml dung dch natri
hydroxyd long (TT) v chit 2 ln, mi ln vi 5 ml cloroform (TT). Lp nc,
sau khi acid ho bng acid nitric (TT), phi cho phn ng B ca phosphat (Ph
lc 7.1).
Tp cht lin quan
Tin hnh sc k lng (Ph lc 4.3).
Pha ng: Amoniac m c - methanol - cloroform - hexan (0,1: 10: 45:
45).
Dung dch th: Ho tan 50 mg ch phm trong nc v pha long n 5,0
ml vi cng dung mi. Thm 0,2 ml amoniac m c (TT) vo 1,0 ml dung dch
ny v lc vi 10,0 ml pha ng. Dng lp trong pha di.
Dung dch i chiu (1): Ho tan 50 mg primaquin diphosphat chun trong
nc v pha long n 5,0 ml vi cng dung mi. Thm 0,2 ml amoniac m c
(TT) vo 1,0 ml dung dch ny v lc vi 10,0 ml pha ng. Dng lp trong pha
di.
Dung dch i chiu (2): Pha long 3,0 ml dung dch th n 100,0 ml bng
pha ng.
Dung dch i chiu (3): Pha long 1,0 ml dung dch th n 10,0 ml bng
pha ng. Pha long tip 1,0 ml dung dch ny n 50,0 ml bng pha ng.
iu kin sc k:
Ct (20 cm x 4,6 mm) nhi silicagel dng cho sc k (10 m).
Tc dng 3,0 ml/pht.
Th tch tim: 20 l.
Cch tin hnh: Tim mi dung dch trn v ghi li sc k trong thi
gian ti thiu l gp i thi gian lu ca primaquin. Trong sc k thu c t
dung dch th, tng din tch ca tt c cc pic ph tr pic chnh, khng c ln
hn din tch pic chnh trong sc k thu c t dung dch i chiu (2) (3,0%)
- loi b pic ca dung mi v cc pic c din tch nh hn din tch pic chnh trong
sc k thu c t dung dch i chiu (3). Php th ch c gi tr khi: trong
sc k thu c t dung dch i chiu (1), ngay trc pic chnh l mt pic c
din tch pic vo khong 6% ca din tch pic chnh v phn gii gia hai pic
ny khng nh hn 2,0; trong sc k thu c t dung dch i chiu (3), t s
gia tn hiu ca pic chnh v nhiu ng nn khng nh hn 5.
Mt khi lng do lm kh
Khng c qu 0,5% (Ph lc 5.16).
(1,000 g; 100 - 1050C).
nh lng
Ho tan 0,200 g ch phm trong 40 ml acid acetic khan (TT), un nng nh.
Chun bng dung dch acid percloric 0,1 N (C). Xc nh im kt thc bng
phng php chun o in th (Ph lc 6.12).
C15H27N3O9P2.
Bo qun
Thuc c bng B. Bo qun trnh nh sng.
71-PROCAIN HYDROCLORID
Procaini hydrochloridum
C13H20N2O2. HCl P.t.l: 272,8

Procain hydroclorid l 2 - diethylaminoethyl 4 - aminobenzoat hydroclorid,
phi cha t 99,0 n 101,0% C13H20N2O2. HCl, tnh theo ch phm lm
kh.
Tnh cht
Tinh th khng mu hay bt kt tinh trng, khng mi.
Rt d tan trong nc, tan trong ethanol 96%, hi tan trong cloroform, thc
t khng tan trong ether.
nh tnh
Nhm I: A, C, D, E v F.
Nhm II: A, B v E.
A. im chy: 154 n 1580C (Ph lc 5.19).
ngoi ca procain hydroclorid chun.
C. Ly khong 5 mg ch phm, thm 0,5 ml acid nitric bc khi (TT), bc
hi cho ti kh trn cch thu. ngui ri ho tan cn trong 5 ml aceton (TT),
thm 1 ml dung dch kali hydroxyd 0,1 M trong ethanol (TT). Ch c mu nu
xut hin.
D. Ly 0,2 ml dung dch S, thm 2 ml nc, 0,5 ml dung dch acid sulfuric
1 M (TT), lc v thm 1 ml dung dch kali permanganat 0,1%. Mu bin mt.
E. Ch phm cho phn ng A ca clorid (Ph lc 7.1).
F. Pha long 1 ml dung dch S ti 100 ml bng nc. 2 ml dung dch ny
cho phn ng c trng ca amin thm bc nht (Ph lc 7.1).

(TT) c 50 ml.
php 2).
pH
Pha long 4 ml dung dch S ti 10 ml bng nc khng c carbon dioxyd
(TT). pH ca dung dch ny t 5,0 - 6,5 (Ph lc 5.9).
Kim loi nng
Ho tan 1,0 g ch phm trong nc c 25,0 ml, lc. Ly 10 ml dch
lc tin hnh theo phng php 5. Dng 2 ml dung dch ch mu 1 phn triu
chun b mu i chiu.
Tp cht lin quan
Tin hnh bng sc k lp mng (Ph lc 4.4).
Dung mi khai trin: Dibutyl ether - hexan - acid acetic bng (80: 16: 4).
Dung dch th: Ho tan 1,0 g ch phm trong nc c 10 ml.
Dung dch i chiu: Ho tan 50 mg acid 4 - aminobenzoic trong nc
c 100 ml. Pha long 1 ml dung dch ny thnh 10 ml bng nc.
Trin khai sc k n khi dung mi i c 10 cm, ly bn mng ra v lm kh
1050C trong 10 pht, quan st bn mng di nh sng t ngoi bc sng 254
nm. Bt k vt ph no trn sc k ca dung dch th khng c sm mu hn
vt trn sc k ca dung dch i chiu. Vt chnh ca dung dch th nm trn
ng xut pht.
Mt khi lng do lm kh
Khng c qu 0,5% (Ph lc 5.16).
(1,000 g; 100 - 1050C).
Tro sulfat
Dng 1,0 g ch phm.
nh lng
Ho tan 0,400 g ch phm trong 50 ml dung dch acid hydrocloric 2 M
(TT), thm 3 g kali bromid (TT). Lm lnh trong nc v chun chm bng
dung dch natri nitrit 0,1 M (C). Xc nh im kt thc bng phng php
chun o ampe (Ph lc 6.9).
1 ml dung dch natri nitrit 0,1 M tng ng vi 27,28 mg C13H20N2O2.
HCl.
Bo qun
Thuc c bng B. Ch phm c bo qun trong chai l nt kn, trnh
nh sng.
Tc dng
Gy t cc b
72-PROCAINAMID HYDROCLORID
Procainamidi hydrochloridum
C13H21N3O. HCl P.t.l: 271,8
Procainamid hydroclorid l 4 - amino - N - [2 - (diethylamino) ethyl] benzamid hydroclorid, phi cha t 98,0 n 101,0% C13H21N3O. HCl, tnh theo
ch phm lm kh.
Tnh cht
Bt kt tinh mu trng hay vng rt nht, d ht m.
Rt tan trong nc, d tan trong ethanol 96%, kh tan trong aceton, thc t
khng tan trong ether.
nh tnh
Nhm I: C v D.
Nhm II: A, B, D v E.
A. im chy: 166 n 1700C (Ph lc 5.19).
B. Ho tan 10,0 mg ch phm trong dung dch natri hydroxyd 0,1 M (TT)
c 100,0 ml. Pha long 10,0 ml dung dch ny bng dung dch natri
hydroxyd 0,1 M thnh 100,0 ml. Ph hp th t ngoi (Ph lc 3.1) ca dung dch
ny t 220 n 350 nm cho mt cc i hp th bc sng 273 nm. A (1%, 1
cm) bc sng cc i phi t 580 n 610.
C. Ph hng ngoi (Ph lc 3.2) ca ch phm phi ph hp vi ph hng
ngoi ca procainamid hydroclorid chun.
D. Pha long 1 ml dung dch S thnh 5 ml bng nc. Dung dch ny cho
phn ng A ca ion clorid (Ph lc 7.1).
E. Pha long 1 ml dung dch S thnh 2 ml bng nc, 1 ml dung dch ny
cho phn ng ca amin thm bc nht (Ph lc 7.1).

(TT) c 25,0 ml.
Dung dch S phi trong (Ph lc 5.12) v c mu khng c m hn mu
mu N6 (Ph lc 5.17, Phng php 2).
pH
Dung dch S phi c pH t 5,6 n 6,3 (Ph lc 5.9).
Tp cht lin quan
Khng c qu 0,5%.
Dung mi khai trin: Acid acetic bng - nc - butanol (15: 30: 60).
Dung dch th: Ho tan 0,10 g ch phm trong ethanol 96% (TT) v pha
long thnh 10 ml bng cng dung mi.
Dung dch i chiu: Pha long 1 ml dung dch th thnh 200 ml bng
ethanol 96% (TT).
Trin khai n khi dung mi i c 12 cm. kh bn mng trong lung kh
lnh. Quan st di nh sng t ngoi bc sng 254 nm.
Trn sc k , bt k vt ph no ca dung dch th cng khng c m
mu hn vt ca dung dch i chiu.
Kim loi nng
Cn 1,0 g ch phm v tin hnh theo phng php 3. Dng 2 ml dung dch
Mt khi lng do lm kh
Khng c qu 0,5% (Ph lc 5.16).
(1,000 g; 100 - 1050C).
Tro sulfat
Dng 1,0 g ch phm.
nh lng
Ho tan 0,250 g ch phm trong 50 ml dung dch acid hydrocloric 2 M
(TT), thm 3 g kali bromid (TT), lm lnh trong nc v chun chm bng
dung dch natri nitrit 0,1 M (C). Xc nh im kt thc bng phng php
chun o ampe (Ph lc 6.9).
1 ml dung dch natri nitrit 0,1 M tng ng vi 27,18 mg C13H21N3O.
HCl.
Bo qun
ng trong ng kn, trnh nh sng.
73-QUININ BISULFAT
Quinini bisulfas
C20H24N2O2. H2SO4. 7H2O
P.t.l: 548,6
Quinin bisulfat l (8S, 9R) - 6' - methoxycinchonan - 9 - ol hydrosulfat

heptahydrat, phi cha t 98,5 n 101,5% C20H24N2O2.. H2 SO4, tnh theo ch
phm khan.
Tnh cht
Tinh th khng mu hay bt kt tinh trng, khng mi, v ng, ln hoa
ngoi khng kh kh. D tan trong nc, hi tan trong ethanol 96%.
nh tnh
A. Phng php sc k lp mng (Ph lc 4.4).
Dung mi khai trin: Diethylamin - ether - toluen (15: 36: 60).
Dung dch th: Dung dch ch phm 1,0% trong methanol (TT).
Dung dch i chiu (1): Dung dch quinin sulfat chun 1,0% trong
methanol (TT).
Dung dch i chiu (2): Dung dch cha 1,0% ca mi quinidin sulfat
chun v quinin sulfat chun trong methanol (TT).
Cch tin hnh: Chm ring r ln bn mng 4 l ca mi dung dch trn.
Sau khi trin khai sc k, ly bn mng ra kh ngoi khng kh 15 pht v chy
sc k nhc li. Sau sy kh bn mng 105oC trong 30 pht, ngui v
phun thuc th iodoplatinat (TT). Vt chnh trn sc k thu c ca dung dch
th phi ging v v tr, mu sc v kch thc vi vt trn sc k thu c ca
dung dch i chiu (1). Php th ch c gi tr khi sc k ca dung dch i
chiu (2) cho 2 vt tch r rng.
B. p ng php th "pH".
C. Ch phm cho phn ng c trng ca sulfat (Ph lc 7.1).
pH
pH ca dung dch ch phm 1%: 2,8 - 3,4 (Ph lc 5.9).
Gc quay cc ring
T - 208 n - 216o, tnh theo ch phm khan (Ph lc 5.13).
Dng dung dch ch phm 3% trong dung dch acid hydrocloric 0,1 M
(TT) o.
Cc alcaloid cinchona khc
Tin hnh phng php sc k lng (Ph lc 4.3).
Pha ng: Ho tan 6,8 g kali dihydrophosphat v 3,0 g hexylamin trong 700
ml nc, iu chnh pH ti 2,8 bng dung dch acid phosphoric 1 M, thm 60 ml
acetonitril v pha long thnh 1000 ml bng nc.
Dung dch th: Ho tan 20 mg ch phm trong 5 ml pha ng, un nng
nh nu cn thit, pha long thnh 10 ml bng pha ng.
Dung dch i chiu (1) v dung dch i chiu (2) c chun b tng t
nh dung dch th nhng thay ch phm bng quinin sulfat chun v quinidin
sulfat chun.
Dung dch i chiu (3): Pha long 1,0 ml dung dch i chiu (1) thnh
10,0 ml bng pha ng. Pha long 1,0 ml dung dch thu c thnh 50,0 ml bng
pha ng.
Dung dch i chiu (4): Ho tan 10 mg thioure trong pha ng c 10
ml.
Dung dch phn gii: Hn hp ng th tch ca dung dch i chiu (1) v
iu kin sc k:
Ct thp khng g (15 - 25 cm x 4,6 mm) c nhi pha tnh C (5 m hoc
10 m) (Hypersil ODS 5 m l thch hp).
Detector quang ph hp th t ngoi bc sng 250 nm cho sc k
ca dung dch i chiu (4) v 316 nm cho sc k ca cc dung dch khc.
Tc dng: 1,5 ml/pht.
Th tch tim: 10 l.
Cch tin hnh:
Tim dung dch i chiu (2) v (4), nu cn thit iu chnh nng ca
acetonitril trong pha ng sc k thu c ca dung dch i chiu (2) c h
s dung lng ca pic quinidin l 3,5 n 4,5, to c tnh t pic ca thioure trong
sc k ca dung dch i chiu (4).
Tim dung dch i chiu (1), (2), (3) v dung dch phn gii. Sc k
ca dung dch i chiu (1) cho 1 pic chnh ca quinin v 1 pic ca dihydroquinin
c thi gian lu tng i so vi quinin l khong 1,4. Sc k ca dung dch
i chiu (2) cho 1 pic chnh ca quinidin v 1 pic ca dihydroquinidin c thi
gian lu tng i so vi quinin l khong 1,2. Sc k ca dung dch phn gii
cho 4 pic: quinin, dihydroquinin, quinidin, dihydroquinidin c nhn bit khi so
snh thi gian lu ca chng vi cc pic tng ng ca chng trong sc k ca
dung dch i chiu (1) v (2).
Php th ch c gi tr khi sc k ca dung dch phn gii c phn
gii gia pic ca quinin v quinidin t nht l 1,5 v phn gii gia pic ca
dihydroquinidin v quinin t nht l 1,0 v t s tn hiu v nhiu nn ca pic
chnh trong sc k ca dung dch i chiu (3) t nht l 5.
Tim dung dch th. Tin hnh sc k trong khong thi gian gp 2,5 ln
thi gian lu ca pic chnh. Tnh hm lng phn trm ca tp cht lin quan bng
phng php chun ho, b qua bt k pic no c din tch nh hn din tch ca
pic trong sc k ca dung dch i chiu (3) (0,2%). Hm lng ca
dihydroquinin khng c qu 10%, hm lng ca bt k tp cht lin quan no
ra gii trc quinin khng c qu 5% v hm lng ca bt k tp cht lin
quan no khc khng c qu 2,5%.
Tro sulfat
Nc
T 19,0 n 25,0% (Ph lc 6.6).
Dng 0,20 g ch phm.
Cation chun c
Phi t 75,3 n 79,6%, tnh theo ch phm khan, c xc nh bng
phng php sau: Thm vo dung dch nc thu c mc nh lng 0,1 ml
dung dch phenolphtalein (CT) v nh lng bng dung dch acid hydrocloric 0,1
N (C).
1 ml dung dch natri hydroxyd 0,1 N tng ng vi 16,32 mg
C20H26N2O2 2+
nh lng
Ho tan 0,450 g ch phm trong 15 ml nc. Thm 25 ml dung dch natri
hydroxyd 0,1 M (TT) v chit bng cloroform 3 ln, mi ln 25 ml. Tp trung dch
chit cloroform v ra bng 20 ml nc. Gp cc dung dch nc thu c em
th cation chun c. Lm khan dch chit cloroform bng natri sulfat khan
(TT), bc hi ti kh p sut 2kPa, ho tan cn cn li trong 50 ml acid acetic
khan (TT). Tin hnh chun trong mi trng khan (Ph lc 6.13. Phng php
1), dng dung dch tm tinh th (CT) lm ch th.
C20H24N2O2. H2SO4.
Bo qun
74-QUININ HYDROCLORID
Quinini hydrochloridum
C20H24N2O2. HCl. 2H2O P.t.l: 396,9

Quinin hydroclorid l (8S, 9R) - 6'- methoxycinchonan - 9 - ol hydroclorid
dihydrat, phi cha t 99,0 n 101,0% C20H24N2O2. HCl, tnh theo ch phm
lm kh.
Tnh cht
Tinh th hnh kim khng mu hay bt kt tinh trng, khng mi, v rt ng
Tan trong nc lnh, d tan trong nc nng, ethanol 96% v cloroform,
rt kh tan trong ether. Dung dch trong cloroform c th khng trong sut do to
thnh cc git nc.
nh tnh
A. Tin hnh phng php sc k lp mng (Ph lc 4.4).
Dung dch th: Ho tan 0,10 g ch phm trong methanol (TT) c 10
ml.
Dung dch i chiu: Ho tan 0,10 g quinin sulfat chun trong methanol
(TT) c 10 ml.
Trin khai sc k n khi dung mi i c 15 cm. Lm kh bn mng bng
lung kh trong 15 pht v chy sc k nhc li. Sy bn mng 105oC trong 30
pht, ngui v phun thuc th iodoplatinat (TT). Vt chnh ca dung dch th
phi tng t v v tr, mu sc v kch thc vi vt chnh ca dung dch i
chiu.
B. Ho tan 10 mg ch phm trong nc c 10 ml. Ly 5 ml dung dch

ny, thm 0,2 ml nc brom (TT) v 1 ml dung dch amoniac 2 M (TT), mu xanh
lc xut hin.
C. Ho tan 0,10 g ch phm trong 3 ml dung dch acid sulfuric 1 M (TT) v
thm nc va 100 ml, xut hin hunh quang xanh lam, hunh quang ny s
bin mt hu nh hon ton khi thm 1 ml acid hydrocloric (TT).
D. Ch phm phi cho phn ng ca ion clorid (Ph lc 7.1).
(TT) va 50 ml.
ca mu mu V6 (Ph lc 5.17, Phng php 2).
pH
Pha long 10 ml dung dch S thnh 20 ml bng nc khng c carbon
dioxyd (TT).
Dung dch thu c phi c pH t 6,0 n 6,8 (Ph lc 5.9).
Gc quay cc ring
T - 245 n - 2580, tnh theo ch phm lm kh (Ph lc 5.13).
Ho tan 0,50 g ch phm trong dung dch acid hydrocloric 0,1 M (TT) va
25,0 ml th.
Bari
Ly 15 ml dung dch S, thm vo 1 ml dung dch acid sulfuric 1 M (TT),
yn 15 pht, dung dch thu c khng c c hn hn hp gm 15 ml dung
dch S v 1 ml nc.
Sulfat
Khng c qu 0,05% (Ph lc 7.4.12).

Ly 15 ml dung dch S tin hnh th.
Yu cu v tin hnh th theo php th "Cc alcaloid cinchona khc" trong
chuyn lun "Quinin bisulfat" ch khc l: Php th ch c gi tr khi sc k ca
dung dch phn gii c phn gii gia pic ca quinin v quinidin t nht l 3,0
v phn gii gia pic ca dihydroquinidin v quinin t nht l 2,0.
Mt khi lng do lm kh
T 6,0 n 10,0% (Ph lc 5.16).
(1,000 g; 100 - 1050C).
Tro sulfat
Dng 1,0 g ch phm.
nh lng
Ho tan 0,300 g ch phm trong hn hp gm 50 ml acid acetic khan (TT)
v 20 ml anhydrid acetic (TT), thm 5 ml dung dch thu ngn (II) acetat (TT).
nh lng bng dung dch acid percloric 0,1 N (C), dng dung dch tm tinh th
(CT) lm ch th hoc c th xc nh im kt thc bng phng php chun
o in th (Ph lc 6.12). Song song tin hnh lm mt mu trng trong cng
iu kin.
C20H24N2O2. HCl.
Bo qun
Ch phm
Vin nn
Tc dng v cng dng
Tr st rt
75-QUININ SULFAT
Quinini sulfas
(C20H24N2O2)2. H2SO4. 2H2O
P.t.l:783,0
Quinin sulfat l (8S, 9R) - 6' - methoxycinchonan - 9 - ol sulfat dihydrat,

phi cha t 99,0 n 101,0% (C20H24N2O2)2. H2SO4, tnh theo ch phm
lm kh.
Tnh cht
Bt kt tinh trng hoc gn nh trng, hoc tinh th hnh kim khng mu,
mn. Kh tan trong nc, hi tan trong nc si v ethanol 96%, thc t khng tan
trong ether.
nh tnh
A. Tin hnh phng php sc k lp mng (Ph lc 4.4).
Dung dch th: Ho tan 0,10 g ch phm trong methanol (TT) v pha long
thnh 10 ml bng cng dung mi.
Dung dch i chiu: Ho tan 0,10 g quinin sulfat chun trong methanol
(TT) v pha long thnh 10 ml vi cng dung mi.
Trin khai sc k n khi dung mi i c 15 cm, ly bn mng lm kh trong
lung khng kh 15 pht v chy sc k nhc li. Sau lm kh bn mng
105oC trong 30 pht, ngui v phun thuc th iodoplatinat (TT). Vt chnh thu
c trn sc k ca dung dch th phi ging v v tr, mu sc v kch thc
vi vt chnh trn sc k ca dung dch i chiu.
B. Ho tan khong 5 mg ch phm trong 5 ml nc. Thm 0,2 ml nc
brom (TT) v 1 ml dung dch amoniac 2 M (TT), mu xanh lc xut hin.
C. Ho tan 0,1 g ch phm trong 3 ml dung dch acid sulfuric 1 M (TT) v
pha long thnh 100 ml bng nc. Hunh quang mu xanh m xut hin v bin
mt khi thm 1 ml acid hydrocloric (TT).
D. Ho tan khong 45 mg ch phm trong 5 ml dung dch acid hydrocloric
long (TT). Dung dch thu c cho phn ng A ca sulfat (Ph lc 7.1).
Dung dch S: Ho tan 0,500 g ch phm trong dung dch acid hydrocloric
0,1 M (TT) v pha long thnh 25,0 ml vi cng dung mi.
mu LV6 (Ph lc 5.17, phng php 2).
pH
pH ca hn dch ch phm 10 g/l trong nc t 5,7 n 6,6 (Ph lc 5.9).
Gc quay cc ring
Xc nh trn dung dch S.
Yu cu v tin hnh th theo php th "Cc alcaloid cinchona khc" trong

chuyn lun "Quinin hydroclorid".
Mt khi lng do lm kh
T 3,0 n 5,0% (Ph lc 5.16).
(1,000 g; 105oC).
Tro sulfat
Dng 1,0 g ch phm.
nh lng
Ho tan 0,300 g ch phm trong hn hp gm 10 ml cloroform (TT) v 20
ml anhydrid acetic (TT). Chun bng dung dch acid percloric 0,1 N (C). Xc
nh im kt thc bng phng php chun o in th (Ph lc 6.12).
(C20H24N2O2)2. H2SO4.
Bo qun
76- SORBITOL
Sorbitolum
C6H14O6
P.t.l: 182,2
Sorbitol l D - glucitol, phi cha t 98,0 n 101,0% C6H14O6, tnh theo

ch phm khan.
Tnh cht
Bt kt tinh mu trng, khng mi.
Rt d tan trong nc, hi tan trong ethanol 96%, thc t khng tan trong
ether.
nh tnh
A. Ha tan 0,5 g ch phm trong hn hp gm 5 ml anhydrid acetic (TT) v
0,5 ml pyridin (TT) bng cch lm nng, yn 10 pht. hn hp trn vo 25
ml nc, yn trong nc 2 gi v lc. Ly ta, kt tinh li trong mt lng
nh ethanol 96% (TT) v sy kh trong chn khng, im chy phi khong
1000C (Ph lc 5.19).
B. Phng php sc k lp mng (Ph lc 4.4).
Dung mi khai trin: Propanol - ethyl acetat - nc (70: 20: 10).
Dung dch th: Ho tan 50 mg ch phm trong nc c 20 ml.
Dung dch i chiu: Ho tan 50 mg sorbitol chun trong nc c 20
ml.
Trin khai bn mng trong bnh dung mi n khi dung mi i c khong 17
cm. Ly bn mng ra, kh ngoi khng kh v phun dung dch acid 4 aminobenzoic (TT). kh bn mng trong lung kh lnh n khi aceton bay
ht. Sy bn mng 1000C trong 15 pht. ngui v phun dung dch natri
periodat 0,2%, kh bn mng trong lung kh lnh. Sy bn mng 1000C
trong 15 pht.
Trn sc k , vt chnh ca dung dch th phi c v tr, mu sc v kch
thc tng ng vi vt chnh ca dung dch i chiu.
C. Ly 3 ml dung dch pyrocatechol 10% mi pha, lm lnh trong nuc ,
thm 6 ml acid sulfuric (TT). Thm 0,3 ml dung dch S vo 3 ml hn hp trn, un
nng nh 30 giy, c mu hng xut hin.
(TT) c 50,0 ml.
php 2).
Gii hn acid kim
Ly 10 ml dung dch S, thm 10 ml nc khng c carbon dioxyd (TT)
(dung dch A).
Ly 10 ml dung dch A, thm 0,05 ml dung dch phenolphtalein (CT).
Lng dung dch natri hydroxyd 0,01 N (C) dng chuyn mu ca dung dch
trn sang mu hng khng c qu 0,2 ml.
Ly 10 ml dung dch A, thm 0,05 ml dung dch methyl (CT). Lng
dung dch acid hydrocloric 0,01 N (C) dng chuyn mu ca dung dch trn
sang mu khng c qu 0,3 ml.
Gc quay cc ring
T + 4,0 n + 7,00, tnh theo ch phm khan (Ph lc 5.13).
Ha tan 5,00 g ch phm v 6,4 g natri tetraborat (TT) trong 40 ml nc,
yn 1 gi, thnh thong lc, thm nc va 50,0 ml, lc nu cn.
ng kh
Ha tan 5,0 g ch phm trong 3 ml nc bng cch un nng nh, ngui,
thm 20 ml dung dch ng citrat (TT) v vi vin bi thu tinh. un nng sao cho
sau 4 pht th si v un si tip 3 pht. Lm ngui nhanh v thm 100 ml dung
dch acid acetic 2,4% (tt/tt), 20,0 ml dung dch iod 0,05 N (C). Va lc va thm
25 ml hn hp gm acid hydrocloric (TT) v nc (6: 94). Khi ta tan ht, chun
iod tha bng dung dch natri thiosulfat 0,05 N (C) dng 1 ml dung dch h
tinh bt (CT) lm ch th, cho vo cui php chun . Lng dung dch natri
thiosulfat 0,05 N tiu th khng c t hn 12,8 ml.
Ch
Nickel
Clorid
Ly 10 ml dung dch S pha long bng nc thnh 15 ml th.
Sulfat
Khng c qu 0,01% (Ph lc 7.4.12).
Ly 15 ml dung dch S th.
Tro sulfat
Dng 2,0 g ch phm.
Nc
Dng 1,0 g ch phm.

nh lng
Ho tan 0,400 g ch phm trong nc c 100,0 ml. Ly 10,0 ml dung
dch ny, thm 20,0 ml dung dch natri periodat 2,14% v 2 ml dung dch acid
sulfuric 1 M (TT), un nng trn cch thu ng 15 pht. ngui, thm 3 g natri
hydrocarbonat (TT) bng cch thm tng lng nh v 25,0 ml dung dch natri
arsenit 0,1 M, lc u v thm 5 ml dung dch kali iodid 20% (TT), yn 15
pht. Chun bng dung dch iod 0,1 N n mu vng. Song song lm mu
trng.
1 ml dung dch iod 0,1 N tng ng vi 1,822 mg C6H14O6.
Cht gy st
Nu sorbitol d nh dng pha ch thuc tim th phi p ng yu cu
ca php th ny (Ph lc 10.5). Tim 10 ml dung dch cha 50 mg ch phm
trong 1 ml nc ct khng c cht gy st cho 1 kg th.
Bo qun
Trong ng kn.
77- STRYCHNIN SULFAT
Strychnini sulfas
(C21H22N2O2)2. H2SO4. 5H2O P.t.l: 857,0

Strychnin sulfat l strychnidin - 10 on sulfat penta-hydrat, chit t ht cy
Strychnos nux - vomica L. v cc loi Strychnos sp. khc, h Loganiaceae, phi
cha t 97,0 n 100,5% (C21H22N2O2)2.H2SO4, tnh theo ch phm khan.
Tnh cht
Tinh th hnh kim khng mu hay bt kt tinh trng, khng mi.
D tan trong nc si, hi tan trong ethanol v nc lnh, kh tan trong

cloroform v khng tan trong ether.
nh tnh
Nhm I: B, C v D.
Nhm II: A v D.
ngoi ca strychnin sulfat chun.
B. Trong php th "Tp cht lin quan": vt chnh ca dung dch th phi
ging v v tr, mu sc v kch thc so vi vt chnh ca dung dch i chiu (1).
C. Ho tan 50 mg ch phm trong 5 ml nc, thm 0,1 ml amoniac m c
(TT) v chit bng 5 ml cloroform (TT). Bc hi dch chit cloroform n cn trn
cch thu. Thm vo cn 0,1 ml acid sulfuric m c (TT) v 1 tinh th kali
dicromat (TT), xung quanh tinh th c mu tm, mu , mu vng khi lc.
D. Ch phm cho phn ng ca ion sulfat (Ph lc 7.1).
(TT) c 50,0 ml.
php 2).
Gii hn acid - kim
Ly 25 ml dung dch S, cho 0,1 ml dung dch methyl (CT), dung dch c
mu . Khi thm khng qu 0,5 ml dung dch natri hydroxyd 0,02 N (C) dung
dch phi chuyn sang mu vng.
Gc quay cc ring
T - 25 n - 29o, tnh theo ch phm khan (Ph lc 5.13).

Dng dung dch S o.
Brucin
Ly 0,1 g ch phm, thm 1 ml acid nitric (TT) v 0,2 ml nc, lc cho tan
hon ton. Nu dung dch thu c c mu hay da cam th khng c m
hn mu ca dung dch i chiu gm 1 ml acid nitric (TT) v 0,2 ml dung dch
brucin 0,054%.
Tp cht lin quan
Dung mi khai trin: Diethylamin - ethyl acetat -cyclohexan (15: 25: 60).
Dung dch th: Ho tan 0,1 g ch phm trong methanol (TT) v thm 10
ml vi cng dung mi.
Dung dch i chiu (1): Ho tan 0,1 g strychnin sulfat chun trong
methanol (TT) v thm 10 ml vi cng dung mi.
Dung dch i chiu (2): Ly 0,5 ml dung dch i chiu (1) v thm
methanol (TT) cho 100 ml.
Trin khai sc k n khi dung mi i c khong 15 cm, ly ra sy kh bn
mng 100 - 105oC trong 15 pht, ngui. Phun dung dch kali iodobismuthat
(TT) cho n khi cc vt cam xut hin. Ngoi vt chnh, bt k vt ph no
trn sc k ca dung dch th, khng c m mu hn vt chnh ca dung
dch i chiu (2).
Nc
T 10,0 n 13,0% (Ph lc 6.6).
Dng 0,10 g ch phm.

Tro sulfat
Dng 1,0 g ch phm.
nh lng
anhydrid acetic (TT). nh lng bng dung dch acid percloric 0,1 N (C). Xc
nh im kt thc bng phng php chun o in th (Ph lc 6.12) hoc
bng ch th xanh malachit (CT).
(C21H22N2O2)2. H2SO4.
Bo qun
Thuc c bng A. ng trong l kn, trnh nh sng.
Ch phm
Thuc tim strychnin sulfat.
Tc dng v cng dng
Kch thch thn kinh trung ng v tu sng, kch thch tiu ho.
78 -TERPIN HYDRAT
Terpinum hydratum
C10H20O2. H2O
P.t.l: 190,3
Terpin hydrat l cyclohexa nmethanol, 4 - hydroxy - , , 4 - trimethyl

monohydrat hay p - menthan 1, 8 - diol monohydrat, phi cha t 98,0 n
100,5% C10H20O2, tnh theo ch phm khan.
Tnh cht
Tinh th trong sut, khng mu hay bt kt tinh trng, khng mi. Sy cn
thn 100oC, ch phm s thng hoa v to thnh nhng tinh th hnh kim.
khng kh nng v kh, ch phm s dn dn b mt nc kt tinh v nhit
nng chy gim. Hi tan trong nc, tan trong nc nng v ethanol 96%, d tan
trong ethanol 96% nng, hi tan trong ether, cloroform.
nh tnh
Nhm I: A, D.
Nhm II: B, C, D, E.
ngoi ca terpin hydrat chun.
B. im chy: 115 - 1170C (Ph lc 5.19). un nng dng c ti 1100C
ri mi cho ng mao qun vo v tip tc un nng vi tc 4 - 60C trong 1
pht.
C. Trn sc k thu c trong php th "Tp cht lin quan": Vt chnh
ca dung dch th phi ging v v tr, mu sc v kch thc vi vt ca dung
dch i chiu (1).
D. Ly 5 ml dung dch ch phm (1/50), un nng ri cho thm vi git
acid sulfuric m c (TT). Dung dch s b vn c v c mi thm ca terpineol.
E. Nh vo 0,01 g ch phm khong 5 git dung dch st (III) clorid trong
ethanol (TT), em bc hi n kh trong chn s, s thy xut hin cng mt lc
cc ch khc nhau trong chn nhng mu son, tm v lc.

Dung dch S: Ho tan 2,50 g ch phm trong ethanol 96% (TT), thm
ethanol 96% va 50 ml.
php 2).
Gii hn acid - kim
Ly 10 ml dung dch S, thm 0,1 ml dung dch xanh bromothymol (CT).
Khng c dng qu 0,2 ml dung dch acid hydrocloric 0,02 N (C) hoc dung
dch natri hydroxyd 0,02 N (C) lm chuyn mu ca ch th.
Tp cht lin quan
Dung mi khai trin: Cloroform - ethyl acetat (1: 9).
Dung dch th: Ho tan 0,25 g ch phm trong methanol (TT), thm
methanol (TT) va 5 ml.
Dung dch i chiu (1): Ho tan 0,25 g terpin hydrat chun trong methanol
(TT) v thm methanol (TT) va 5 ml.
Dung dch i chiu (2): Ly 1 ml dung dch i chiu (1) v thm
methanol (TT) va 100 ml.
Trin khai sc k n khi dung mi i c khong 15 cm. Sy bn mng nhit
100 - 1050C trong 5 pht. ngui bn mng sau khi sy, phun dung dch
vanilin 1% trong acid sulfuric (TT). Nu trn sc k ca dung dch th c xut
hin cc vt khc vi vt chnh th cc vt ny khng c c mu m hn mu
ca vt chnh trn sc k ca dung dch i chiu (2).
Nc
T 8,0% - 10,0% (Ph lc 6.6).
Dng 0,20 g ch phm.
Tro sulfat
Dng 1,0 g ch phm.
nh lng
Bng phng php sc k kh (Ph lc 4.2).
Dung dch chun ni: Ho tan mt lng chnh xc biphenyl trong
cloroform (TT) c dung dch cha khong 20 mg/ ml.
Dung dch chun: Cn chnh xc khong 170 mg terpin hydrat chun, ho
tan bng 5 ml ethanol 96% (TT) trong bnh nh mc 100 ml, thm 5,0 ml dung
dch chun ni v thm cloroform (TT) n vch.
Dung dch th: Cn chnh xc khong 170 mg ch phm, tin hnh nh
cch chun b dung dch chun, bt u t "ho tan bng 5 ml...".
iu kin sc k:
Ct thp khng g hoc thu tinh (1,2 m x 3,5 mm) c nhi t diatomit
ra acid n trung tnh v silan ho (chromosorb AW - 80 - 100 mesh) vi
6% cht hp ph dimethylpolysiloxan dng cho sc k kh.
Kh mang l nitrogen dng cho sc k kh vi lu lng cn thit t
c thi gian lu ca terpin khong 7 pht v ca biphenyl khong 11 pht.
Nhit ct 1200C, nhit ca bung tim v ca detector 2600C.
Th tch tim: 1 l.
Cch tin hnh:

Tim dung dch chun. phn gii gia pic terpin v biphenyl khng
c nh hn 2,0 v lch chun tng i gia cc ln tim nhc li khng
c ln hn 2,0%.
Tim dung dch th. Tnh hm lng C10H20O2 theo t l din tch gia
pic ca terpin v chun ni c c t sc k ca dung dch th v dung dch
chun.
Bo qun
ng trong l nt kn, trnh nh sng.
Cng dng
Tng tit dch kh qun (long m).
Ch phm
Thng c kt hp trong cc ch phm tr ho nh:
Vin ung terpinbenzoat, vin ung terpincodein.
79-THAN HOT TNH
Carbo activatus
Than hot tnh l cht c kh nng hp ph cao, thu c t qu trnh than
ho thch hp cc cht c ngun gc thc vt.
Tnh cht
Bt nh, mu en, rt xp, thc t khng tan trong cc dung mi thng
thng.
nh tnh
A. Khi t n nng , ch phm chy chm v khng thnh ngn la.
B. Ch phm phi p ng php th "Kh nng hp ph".
Dung dch S: Thm vo 2,0 g ch phm trong mt bnh nn nt mi 50 ml

dung dch acid hydrocloric long (TT). un si nh di ng sinh hn hi lu
trong 1 gi, lc v ra phu lc bng dung dch acid hydrocloric long (TT). Gp
dch lc v nc ra ri bc hi n kh trn cch thu, ho tan cn trong dung
dch acid hydrocloric 0,1 M v pha long thnh 50,0 ml bng dung dch acid
hydrocloric 0,1 M.
Gii hn acid - kim
Thm vo 2,0 g ch phm 40 ml nc v un si trong 5 pht. ngui,
hon li th tch ban u bng nc khng c carbon dioxyd (TT) v lc. B 20 ml
dch lc u. Thm vo 10 ml dch lc 0,25 ml dung dch xanh bromothymol (CT)
v 0,25 ml dung dch natri hydroxyd 0,02 M, dung dch phi c mu xanh. Mu
ca ch th phi chuyn sang vng khi thm khng qu 0,75 ml dung dch acid
hydrocloric 0,02 M.
Cht tan trong acid
Khng c qu 3%.
Thm vo 1,0 g ch phm 25 ml dung dch acid nitric long (TT) v un si
trong 5 pht. Lc nng qua phu lc thu tinh xp s 10 v ra bng 10 ml nc
nng. Gp dch chit v nc ra, bc hi n kh trn cch thu, thm vo cn 1
ml acid hydrocloric (TT), bc hi li n kh v sy cn n khi lng khng i
100 n 105 C. Khi lng cn khng c qu 30 mg.
Cht mu tan trong kim
Thm vo 0,25 g ch phm, 10 ml dung dch natri hydroxyd long (TT) v
un si trong mt pht. ngui, lc v pha long dch lc thnh 10 ml bng
nc. Dung dch khng c c mu m hn mu mu LV4 (Ph lc 5.17,
phng php 2).
Cht tan trong ethanol 96%
Khng c qu 0,5%.
Thm vo 2,0 g ch phm 50 ml ethanol 96% (TT) v un si di ng
sinh hn hi lu trong 10 pht. Lc ngay, ngui v pha long thnh 50 ml bng
ethanol 96% (TT). Dch lc ny khng c c mu m hn mu mu V6 hoc
NV6 (Ph lc 5.17, phng php 2). Bc hi 40 ml dch lc n kh v sy cn
n khi lng khng i 100 n 105 C. Khi lng cn khng c qu 8 mg.
Cht hunh quang
Chit 10,0 g ch phm vi 100 ml cyclohexan (TT1) trong 2 gi trong b
chit Soxhlet. Ly phn dung dch v pha long thnh 100 ml bng cyclohexan
(TT1). Quan st di nh sng t ngoi bc sng 365 nm. Hunh quang ca
dung dch ny khng c m hn dung dch ca 83 g quinin trong 1000 ml
dung dch acid sulfuric 0,005 M c quan st trong cng iu kin.
Sulfid
Thm vo 1,0 g ch phm trong mt bnh nn, 5 ml dung dch acid
hydrocloric 25% v 20 ml nc. un n si. Kh gii phng ra khng c lm
giy ch acetat (TT) chuyn thnh mu nu.
ng
Xc nh bng phng php quang ph hp th nguyn t (Ph lc 3.4,
phng php 1).
Dung dch th: S dng dung dch S.
Dung dch i chiu: Chun b cc dung dch i chiu bng cch pha
long dung dch ng mu 0,1% bng dung dch acid hydrocloric 0,1 M.
o hp th 325,0 nm, s dng n cathod rng ng lm ngun bc
x v ngn la khng kh - acetylen.
Ch

phng php 1).
long dung dch ch mu 100 phn triu bng dung dch acid hydrocloric 0,1 M.
o hp th 283,3 nm, s dng n cathod rng ch lm ngun bc x
v ngn la khng kh - acetylen. Tu thuc vo my, c th s dng vch 217,0
nm.
Km
phng php 1).
long dung dch km mu 100 phn triu bng dung dch acid hydrocloric 0,1 M.
o hp th 214,0 nm, s dng n cathod rng km lm ngun bc x
v ngn la khng kh - acetylen.
Mt khi lng do lm kh
(1,00 g; 120 C; 4 gi).
Tro sulfat
Dng 1,0 g ch phm.
Kh nng hp ph
Thm vo 0,300 g ch phm trong mt bnh nn nt mi dung tch 100 ml,
25,0 ml dung dch mi pha ca 0,5 g phenazon trong 50 ml nc. Lc k trong 15
pht. Lc v b 5 ml dch lc u. Thm vo 10,0 ml dch lc 1,0 g kali bromid
(TT) v 20 ml dung dch acid hydrocloric long (TT). Dng 0,1 ml dung dch
ethoxycrysoidin (CT) lm ch th, chun bng dung dch kali bromat 0,1 N n
khi mu chuyn t hng sang hng vng. Gn im kt thc chun , chun
chm (1 git trong 15 giy). Song song tin hnh lm mu trng vi 10,0 ml
dung dch phenazon trn.
Tnh khi lng phenazon c hp ph bi 100 g than hot tnh theo
cng thc:
a: S mililit dung dch kali bromat 0,1 N dng cho mu trng.

b: S mililit dung dch kali bromat 0,1 N dng cho mu th.
m: Khi lng ch phm tnh ra gam.
Khng c di 40 g phenazon c hp ph bi 100 g than hot tnh,
tnh theo ch phm lm kh.
nhim khun
Tng s vi khun hiu kh sng li c khng c qu 1000 trong 1,0 g
ch phm, xc nh bng phng php a thch (Ph lc 10.7).
Bo qun
Trong chai l kn.
80 -THEOPHYLIN
Theophyllinum
C7H8N4O2 P.t.l.: 180,2

C7H8N4O2.H2O
P.t.l.: 198,2
Theophylin l 1,3 - dimethylpurin - 2,6 (3H, 1H) - dion, ngm mt phn t

nc hoc khan, phi cha t 99,0 n 101,0% C7H8N4O2, tnh theo ch phm
lm kh.
Tnh cht
Bt tinh th trng, khng mi. Kh tan trong nc v cloroform, hi tan
trong ethanol, tan trong nc nng v ethanol nng, trong cc dung dch hydroxyd
kim, amoniac v cc acid v c, rt kh tan trong ether.
nh tnh
Nhm I: A,C v D.
Nhm II: A v B.
A. im chy (Ph lc 5.19) ca ch phm sau khi lm kh 100 n 105
C, trong khong 270 n 274 C.
ngoi i chiu ca theophylin hoc ph hng ngoi ca theophylin chun (i vi
dng ngm nc phi sy kh 100 n 105 C trc khi th).
C. Ho tan khong 10 mg ch phm trong 10 ml nc, thm 0,5 ml dung
dch thu ngn (II) acetat 5% v yn, s xut hin ta tinh th trng.
D. Cho phn ng ca nhm xanthin (Ph lc 7.1).

(TT) bng cch un nng, ngui v pha long n 75 ml bng cng dung mi
trn.
php 2).
Gii hn acid
Thm 0,1 ml dung dch methyl (CT) vo 50 ml dung dch S, dung dch
c mu v phi chuyn sang vng khi thm khng qu 1,0 ml dung dch natri
hydroxyd 0,01 M.
Kim loi nng
Tp cht lin quan
Khng c qu 0,5%.
30: 30: 40).
Dung dch th: Ho tan 0,2 g ch phm trong hn hp dung mi gm 4 th
tch methanol (TT) v 6 th tch cloroform (TT) v pha long n 10 ml bng cng
hn hp dung mi.
hn hp dung mi trn.
Trin khai sc k n khi dung mi i c 15 cm. Sau ly bn mng ra,
kh ngoi khng kh v quan st di nh sng t ngoi bc sng 254 nm.
Trn sc k , ngoi vt chnh, bt k vt ph no ca dung dch th u khng
c m mu hn vt ca dung dch i chiu.
Mt khi lng do lm kh
Khng c qu 0,5% (i vi dng khan) v t 8,0 n 9,5% (i vi
dng ngm nc) (Ph lc 5.16).
(1,00 g; 105 C).
Tro sulfat
Dng 1,0 g ch phm.
nh lng
Ho tan khong 0,150 g theophylin (dng khan) hoc 0,160 g (dng ngm
nc) trong 100 ml nc. Thm 20 ml dung dch bc nitrat 0,1 N v lc. Thm 1
ml dung dch xanh bromthymol (CT). Chun bng dung dch natri hydroxyd
0,1 N.
1 ml dung dch natri hydroxyd 0,1 N tng ng vi 18,02 mg
C7H8N4O2.
Bo qun
trong l nt kn.
Ch phm
Thuc tim aminophylin. Vin nn theophylin.
Tc dng, cng dng
Gin kh - ph qun, gin c trn mch mu, li tiu. Tr hen suyn.

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Dc in Vit Nam III

Acid acetylsalicylic l acid 2-acetoxybenzoic, phi cha t 99,5 n l01,0%

un hn hp v cho khi sinh ra tip xc vi ming giy lc tm 0,05 ml

clorid 0,5%, 0,1 ml acid acetic (TT), 4 ml ethanol 96% (TT) v 15 ml nc vo 1

Ha tan 1,000 g ch phm trong 10 ml ethanol 96% (TT) trong bnh nn

Acid ascorbic l (R)-5-[(S)-1,2-dihydroxyethyl]-3,4-dihydroxy-5H-furan 2on, phi cha t 99,0 n 100,5% C6H8O6.

C th chn mt trong hai nhm nh tnh sau:

Acid benzoic l acid benzen carboxylic, phi cha t 99,0 n 100,5%

Ly 12 ml dung dch S v tin hnh th theo phng php 2. Dung dch i

Cho 1,0 g ch phm vo ng nghim, thm 10 ml acid sulfuric (TT), un

10C trong 1 gi. Lm ngui tht nhanh,

dung dch khng c c mu m hn mu ca hn hp gm 1 ml dung dch u

Acid salicylic l acid 2 - hydroxybenzencarboxylic, phi cha t 99,0 n

Ly 15 ml dung dch S v tin hnh th.

(C7H8 N4O2)2. C2H8 N2

Ho tan 1,0 g ch phm trong 10 ml nc , thm tng git 2 ml dung dch

Tp cht lin quan

Ethylendiamin: Ho tan 0,250 g ch phm trong 30 ml nc, thm 0,1 ml

Ampicilin l acid (6R) -6 -( - D - phenylglycylamino) penicilanic, phi

sau khi ho tan. C hai dung dch trn khng c c hn c mu S2 (Ph

Ct thu tinh (2 m 2 mm), c nhi bng kieselgur c silan ho v

C16H19 N3O4S. 3H2O

Ampicilin trihydrat l acid (6R) -6 -( - D - phenylglycylamino) penicilanic

vi git dung dch acid sulfuric 10% (TT), ta trng c to thnh. Ta ny

Thm mt hn hp gm 3 ml dung dch acid nitric 2 N (TT) v 7 ml nc

hp 5 pht v yn trong 15 pht. Cht th nghim khng c lng xung thp

A. Ho tan 10 mg ch phm trong 20 ml nc nng, lm lnh v thm 1 ml

Dung dch i chiu 1: Ho tan 0,1 mg jatrorrhizin chun trong 1 ml

o hp th (Ph lc 3.1) At v As ca dung dch th v dung dch chun

a: Khi lng ( mg) kali dicromat.

hydrocloric m c (TT) v 5 ml nc, lc. Thm vo dch lc 1 ml dung dch

Cn thu c trong php th "Mt khi lng do lm kh" khng c c

Khng c qu 1 phn triu (Ph lc 7.4.7).

Hm lng ethanol t 59,7 n 60,2% (tt/tt).

C8H10 N4O2 (khan)

C8H10 N4O2. H2O (monohydrat)

Cafein l 1, 3, 7 trimethyl - 3,7 dihydro - 1 H purin - 2, 6 dion, phi cha t

E. Ch phm p ng php th mt khi lng do lm kh.

Tp cht lin quan

vi 5 ml nc nng v sy 100 - 1050C trong 1 gi, khi lng cn cn li

Khng c qu 1,5% (Ph lc 7.4.14).

Calci gluconat l calci D-gluconat monohydrat, phi cha t 98,5 n

Ly 2,0 g ch phm tin hnh theo phng php 4. un nng dn dn v

Camphor l (1RS,4SR) - 1,7,7 - trimethylbicyclo - [2.2.1] heptan - 2 - on,

Camphor tng hp (loi racemic): T -1,5 n +1,5o; (loi t tuyn): T 39 n -44o.

C2H3Cl3O2 P.t.l: 165,4

Cloral hydrat l 2,2,2-tricloroethan-1,1-diol, phi cha t 98,5 n 101,0%

Ly 5 ml dung dch S, pha long vi nc ti 15 ml v tin hnh th.

Ly 50,0 ml ch phm cho vo cc thu tinh cn b sn. Bc hi cch

Lc 20,0 ml ch phm trong 5 pht vi 10,0 ml acid sulfuric m c (TT)

pentyldiethylamin diphosphat, phi cha t 98,5 n 101,0% C18H26ClN3.

Bt kt tinh trng hoc gn nh trng, khng mi, v ng, d bin mu khi

cng khng c m mu hn vt trn sc k thu c t dung dch i chiu

C18H21NO3. H2O P.t.l: 317,4

Codein l (5R, 6S) -4,5-epoxy-3-methoxy-N-methylmorphin-7-en-6-ol

Dung dch S: Ho tan 50 mg ch phm trong nc khng c carbon dioxyd

Tc dng v cng dng

C18H21NO3. H3PO4. 1/2H2O (Hemihydrat) P.t.l: 406,4

250 n 350 nm. Dung dch ch c duy nht mt cc i hp th 284 nm. hp

C22H29FO5 P.t.l: 392,5

Bn mng: Silicagel GF254.

E. Trn khong 5 mg ch phm vi 45 mg magnesi oxyd nng (TT) v

Detector quang ph hp th t ngoi bc sng 254 nm.