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Duoc Dien VN III PDF
Duoc Dien VN III PDF
1-ACID ACETYLSALICYLIC
Acidum acetylsalicylicum
Aspirin
C9H8O4
P.t.l: 180,2
P.t.l: 176,1
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
Khng c qu 2 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 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
Khng c qu 10 phn triu (Ph lc 7.4.7).
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
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
Khng c qu 10 phn triu (Ph lc 7.4.7).
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
C th chn mt trong hai nhm nh tnh sau:
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.
trong v mu sc ca dung dch
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
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
Khng c qu 0,1% (Ph lc 7.7, phng php 2).
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
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
C th chn mt trong hai nhm nh tnh sau:
Nhm I: B, C, E.
Nhm II: A, C, D, E, F.
C16H19 N3O4S
P.t.l: 349,40
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
C th chn mt trong hai nhm nh tnh sau:
Nhm I: A, D
Nhm II: B, C, D
A. Ph hng ngoi (Ph lc 3.2) ca ch phm phi ph hp vi ph hng
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
Khng khun.
8-AMPICILIN TRIHYDRAT
Ampicillinum trihydratum
P.t.l: 403,5
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
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
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
Khng c qu 30 phn triu (Ph lc 7.4.7).
Ly 1,0 g ch phm tin hnh theo phng php 3. Dng 3 ml dung dch
ch mu 10 phn triu chun b mu i chiu.
Tro sulfat
Khng c qu 0,2% (Ph lc 7.7, phng php 1).
Dng 1,0 g ch phm.
Mt khi lng do lm kh
Khng c qu 12% (Ph lc 5.16).
(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).
Arsen
Khng c qu 10 phn triu (Ph lc 7.4.2).
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
Caffeinum
P.t.l: 194,2
P.t.l: 212,2
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 acid.
15-CALCI GLUCONAT
Calcii gluconas
C12H22CaO14. H2O
P.t.l: 448,4
v cht ng phn i nh
C10H16O
P.t.l: 152,2
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
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%.
C18H26ClN3. 2H3PO4
P.t.l: 515,9
Cloroquin
phosphat
(RS)
-4-
(7-cloro-4-quinolylamino)
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).
trong v mu sc ca dung dch
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
Khng c qu 20 phn triu (Ph lc 7.4.7).
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.
Cch tin hnh: Chm ring bit ln bn mng 2 l mi dung dch trn.
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
Dung dch i chiu (2): Pha long 1 ml dung dch th vi ethanol (TT)
va 100 ml.
Cch tin hnh: Chm ring bit ln bn mng 10 l mi dung dch trn.
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
Khng c qu 0,1% (Ph lc 7.7, phng php 2).
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.
1 ml dung dch acid percloric 0,1 N tng ng vi 29,94 mg
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.
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
Tin hnh theo phng php sc k lp mng (Ph lc 4.4).
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.
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 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
Ho tan 0,350 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.
1 ml dung dch acid percloric 0,1 N tng ng vi 39,74 mg
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
Pha ng B
(% tt/tt)
Tin hnh
100
15
40
100
100
Bt u cn bng vi pha ng A
46 - 0 100
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
Nhm I: B, C.
Nhm II: A, C, D, E, F.
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.
B. Ph hng ngoi (Ph lc 3.2) ca ch phm phi ph hp vi ph hng
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.
C. Phng php sc k lp mng (Ph lc 4.4).
Bn mng: Silicagel GF254.
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).
Cch tin hnh: Chm ring bit ln bn mng 5 l mi dung dch trn.
Trin khai bn mng 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, 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
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).
Detector quang ph hp th t ngoi bc sng 254 nm.
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.
Detector ion ho ngn la.
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
Thuc c bng B. Trong l kn, trnh nh sng.
Ch phm
Dexamethason natri phosphat tim; Dexamethason natri phosphat nh mt.
25-DIETHYL PHTALAT
Diethylis phthalas
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
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
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
P.t.l: 46,07
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
Khng c qu 1 phn triu (Ph lc 7.4.7).
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
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
C6H12O6
P.t.l: 180,2
Glucosum monohydricum
Dextrose ngm mt phn t nc
C6H12O6. H2O
P.t.l: 189,2
CHOH
CH2OH
C3H8O3
P.t.l: 92,1
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
Khng c qu 35 phn triu.
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
Khng c qu 2% (Ph lc 6.6).
Dng 1,500 g ch phm.
Tro sulfat
Khng c qu 0,01% (Ph lc 7.7, phng php 2).
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
C6H7N3O
P.t.l: 137,14
Cch tin hnh: Chm ring bit ln bn mng 5 l mi dung dch trn.
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
Khng c qu 10 phn triu (Ph lc 7.4.7).
Ly 2,0 g ch phm th theo phng php 3. Dng 2 ml dung dch ch mu
10 phn triu 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
Khng c qu 0,1% (Ph lc 7.7, phng php 2).
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
Dung dch S: Ho tan 10,0 g ch phm trong nc khng c carbon dioxyd
(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).
trong v mu sc ca dung dch
Dung dch S phi trong (Ph lc 5.12) v khng mu (Ph lc 5.17, phng
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.
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
Khng c qu 1 phn triu (Ph lc 7.4.8).
Dung dch th: Ho tan 4,0 g ch phm trong 100 ml nc, thm 10 ml
dung dch m acetat pH 6,0.
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
Dung dch S: Ho tan 10,0 g ch phm trong nc khng c carbon dioxyd
(TT) v pha long va 100 ml.
Dung dch S cho phn ng c trng ca ion kali v iodid (Ph lc 7.1).
trong v mu sc ca dung dch
Dung dch S phi trong (Ph lc 5.12) v khng mu (Ph lc 5.17, phng
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
P.t.l: 158,03
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).
Ly 10 ml dung dch S pha long thnh 15 ml bng nc v tin hnh th.
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
Trong chai l nt kn, trnh nh sng.
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
(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
Khng c qu 50 phn triu (Ph lc 7.4.7).
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).
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
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
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.
1 ml dung dch acid percloric 0,1 N tng ng vi 14,41 mg
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).
trong v mu sc ca dung dch
Dung dch S: Ho tan 10,0 g ch phm trong nc khng c carbon dioxyd
(TT) va 100 ml.
Dung dch S phi trong (Ph lc 5.12) v khng mu (Ph lc 5.17, phng
php 2).
Gii hn acid - kim
Bo qun
Trong l kn, trnh nh sng.
45-NATRI CALCI EDETAT
Natrii calcii edetas
C10H12CaN2Na2O8. xH2O
P.t.l: 374,3
St
Khng c qu 80 phn triu (Ph lc 7.4.11).
Ly 2,5 ml dung dch S, pha long vi nc va 10 ml v tin hnh th.
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).
Dng 0,100 g ch phm th.
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.
trong v mu sc ca dung dch
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
Khng c qu 20 phn triu (Ph lc 7.4.7).
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
phn triu chun b mu i chiu.
Mt khi lng do lm kh
Khng c qu 2,7% (Ph lc 5.16).
(1,000 g; 100 - 105oC; 2 gi).
Bo qun
Trong chai l nt kn, trnh nh sng.
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
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.
1 ml dung dch acid percloric 0,1 N tng ng vi 8,602 mg
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).
trong v mu sc ca dung dch
Dung dch S: Ho tan 20,0 g ch phm trong nc khng c carbon dioxyd
(TT) v pha long va 100,0 ml bng cng dung mi.
Dung dch S phi trong (Ph lc 5.12) v khng mu (Ph lc 5.17, phng
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
Khng c qu 50 phn triu.
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
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.
P.t.l: 84,0
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).
trong v mu sc ca dung dch
Dung dch S: Ho tan 5,0 g ch phm trong nc khng c carbon dioxyd
(TT), thm va 50,0 ml vi cng dung mi.
Dung dch S phi trong (Ph lc 5.12) v khng c c mu m hn mu
mu NV6 (Ph lc 5.17, phng php 2).
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
P.t.l: 322,2
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).
trong v mu sc ca dung dch
Dung dch S: Ho tan 2,2 g ch phm trong nc ri thm nc va 100
ml.
Dung dch S phi trong (Ph lc 5.12) v khng mu (Ph lc 5.17, phng
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
D tan trong nc, tan mt phn trong ethanol 96%, thc t khng tan trong
ether.
nh tnh
C th chn mt trong hai nhm nh tnh sau:
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.
C. Phng php sc k lp mng (Ph lc 4.4).
Bn mng: Silicagel GF254.
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.
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 18 cm. Quan st bn mng di nh
sng t ngoi bc sng 254 nm. Vt chnh trn sc k ca dung dch th
Cch tin hnh: Chm ring bit ln bn mng 20 l mi dung dch trn.
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
P.t.l: 248,2
Dung dch S phi trong (Ph lc 5.12) v khng mu (Ph lc 5.17, phng
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
Khng c qu 10 phn triu (Ph lc 7.4.7).
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
P.t.l: 121,95
C8H9NO2
P.t.l: 151,2
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
C th chn mt trong hai nhm nh tnh sau:
Nhm I: A v E.
Nhm II: B, C, D v E.
A. Ph hng ngoi (Ph lc 3.2) ca ch phm phi ph hp vi ph hng
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
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
C th chn mt trong hai nhm nh tnh sau:
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).
B. Ph hng ngoi (Ph lc 3.2) ca ch phm phi ph hp vi ph hng
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).
trong v mu sc ca dung dch
Dung dch S: Ho tan 0,5 g ch phm trong nc khng c carbon dioxyd
(TT) v pha long thnh 25 ml vi cng dung mi.
Dung dch S phi trong (Ph lc 5.12) v khng mu (Ph lc 5.17, phng
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%.
Tin hnh bng phng php sc k lp mng (Ph lc 4.4).
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
C12H12N2O3
P.t.l: 232,2
Dung dch i chiu: Ho tan 0,1 g phenobarbital chun trong ethanol 96%
(TT) c 100 ml.
Cch tin hnh: Chm ring bit ln bn mng 10 l mi dung dch trn.
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).
trong v mu sc ca dung dch
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%.
Xc nh bng phng php sc k lp mng (Ph lc 4.4).
Bn mng: Silicagel GF254.
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.
Dung dch i chiu: Pha long 0,5 ml dung dch th thnh 100 ml bng
ethanol 96% (TT).
Cch tin hnh: Chm ring bit ln bn mng 20 l mi dung dch trn.
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
Khng c qu 0,1% (Ph lc 7.7, phng php 2).
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
C15H12N2O2
P.t.l: 252,3
Mt khi lng do lm kh
Khng c qu 0,5% (Ph lc 5.16).
(1,000 g; 105oC).
Tro sulfat
Khng c qu 0,1% (Ph lc 7.7, phng php 2).
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
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).
trong v mu sc ca dung dch
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).
Bn mng: Silicagel GF254.
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
Khng c qu 0,1% (Ph lc 7.7, phng php 1).
Dng 1,0 g ch phm.
nh lng
Tin hnh trong nh sng du.
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%
C4Hl0N2. C6H10O4
P.t.l: 232,3
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
C4H10N2.6H2O
P.t.l: 194,2
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).
trong v mu sc ca dung dch
Dung dch S: Ho tan 1,0 g ch phm trong nc khng c carbon dioxyd
(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
Khng c qu 20 phn triu (Ph lc 7.4.7).
Ly 12 ml dung dch S tin hnh th theo phng php 1. Dng dung dch
ch mu 1 phn triu chun b mu i chiu.
Tro sulfat
P.t.l: 202,1
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
C th chn mt trong hai nhm nh tnh sau:
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
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).
1 ml dung dch acid percloric 0,1 N tng ng vi 22,77 mg
C15H27N3O9P2.
Bo qun
Thuc c bng B. Bo qun trnh nh sng.
71-PROCAIN HYDROCLORID
Procaini hydrochloridum
Mt khi lng do lm kh
Khng c qu 0,5% (Ph lc 5.16).
(1,000 g; 100 - 1050C).
Tro sulfat
Khng c qu 0,1% (Ph lc 7.7, phng php 2).
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
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
C th chn mt trong hai nhm nh tnh sau:
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).
trong v mu sc ca dung dch
Mt khi lng do lm kh
Khng c qu 0,5% (Ph lc 5.16).
(1,000 g; 100 - 1050C).
Tro sulfat
Khng c qu 0,1% (Ph lc 7.7, phng php 2).
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
P.t.l: 548,6
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).
Bn mng: Silicagel G.
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
dung dch i chiu (2).
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
Khng c qu 0,1% (Ph lc 7.7, phng php 1).
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.
1 ml dung dch acid percloric 0,1 N tng ng vi 21,13 mg
C20H24N2O2. H2SO4.
Bo qun
Trong l kn, trnh nh sng.
74-QUININ HYDROCLORID
Quinini hydrochloridum
Vin nn
Tc dng v cng dng
Tr st rt
75-QUININ SULFAT
Quinini sulfas
P.t.l:783,0
Cch tin hnh: Chm ring bit ln bn mng 4 l mi dung dch trn.
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).
trong v mu sc ca dung dch
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.
Dung dch S phi trong (Ph lc 5.2) v khng c c mu m hn mu
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
T - 237 n - 245o, tnh theo ch phm lm kh (Ph lc 5.13).
Xc nh trn dung dch S.
Cc alcaloid cinchona khc
76- SORBITOL
Sorbitolum
C6H14O6
P.t.l: 182,2
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.
trong v mu sc ca dung dch
Dung dch S: Ho tan 5,0 g ch phm trong nc khng c carbon dioxyd
(TT) c 50,0 ml.
Dung dch S phi trong (Ph lc 5.12) v khng mu (Ph lc 5.17, phng
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
Khng c qu 0,5 phn triu (Ph lc 7.4.4).
Nickel
Khng c qu 1 phn triu (Ph lc 7.4.9).
Clorid
Khng c qu 50 phn triu (Ph lc 7.4.5).
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
Khng c qu 0,1% (Ph lc 7.7, phng php 2).
Dng 2,0 g ch phm.
Nc
Khng c qu 1,5% (Ph lc 6.6).
C10H20O2. H2O
P.t.l: 190,3
Nc
T 8,0% - 10,0% (Ph lc 6.6).
Dng 0,20 g ch phm.
Tro sulfat
Khng c qu 0,1% (Ph lc 7.7, phng php 1).
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.
Detector ion ho ngn la.
Nhit ct 1200C, nhit ca bung tim v ca detector 2600C.
Th tch tim: 1 l.
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
Khng c qu 25 phn triu.
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
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:
P.t.l.: 198,2
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 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
Khng c qu 0,1% (Ph lc 7.7, phng php 2).
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.