Giao Trinh Kiem Nghiem PDF

Trng Trung Cp Bch khoa Si Gn Gio trnh KIM NGHIM
B Y T
KIM NGHIM THUC

(DNG CHO O TO DC S TRUNG CP)
1
Li gii thiu
Thc hin mt s iu ca Lut Gio dc, B Y t ban hnh

chng trnh khung o to trung cp ngnh Y t. B Y t t chc bin
son ti liu dy - hc cc mn c s v chuyn mn theo chng trnh
trn nhm tng bc xy dng b sch chun trong cng tc o to
trung cp y t.
Sch KIM NGHIM THUC c bin son da trn chng trnh

gio dc ngh nghip ca B Y t bin son trn c s chng trnh
khung c ph duyt. Sch c cc tc gi Nguyn Th Kiu Anh,
Trn Tch, V Th Thu Thu bin son theo phng chm: Kin thc c
bn, h thng; ni dung chnh xc, khoa hc; cp nht cc tin b khoa
hc, k thut hin i v thc tin Vit Nam. Sch c cu trc gm
22 bi bm st theo chng trnh gio dc vi nhng ni dung theo
hng dn chun quc gia. Ti liu l tin cc gio vin v hc
Sch KIM NGHIM THUC c Hi ng chuyn mn thm nh

sch v ti liu dy - hc trung cp v dy ngh ca B Y t thm nh
vo nm 2007. B Y t quyt nh ban hnh lm ti liu dy - hc chnh
sch phi c chnh l, b sung v cp nht.
B Y t xin chn thnh cm n cc tc gi v Hi ng chuyn mn

thm nh u t cng sc hon thnh cun sch; Cm n PGS. TS.
Trnh Vn Lu, TS. Phng Th Vinh c v phn bin, cun sch
sm hon thnh kp thi phc v cho cng tc o to nhn lc y t.
Ln u xut bn, chng ti mong nhn c kin ng gp ca

ng nghip, cc bn sinh vin v cc c gi ln xut bn sau c
hon thin hn.
V K A C V - B Y
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Bi 1
I CNG V CNG TC KIM TRA
CHT LNG THUC, M PHM
MC TIU
- Trnh by c s cn thit phi kim tra cht lng thuc.
- Bit c ni dung, h thng t chc kim tra cht lng thuc ca

Vit Nam.
1. CHT LNG V KIM TRA CHT LNG
1.1. Thuc v yu cu cht lng
1.1.1. Khi nim v thuc
rong "iu l thuc phng bnh, cha bnh" ban hnh ngy
24/1/1991 quy nh: Thuc l nhng sn phm c ngun gc t ng
vt, thc vt, khong vt, hay sinh hc c sn xut dng cho ngi
nhm:
- Phng bnh, cha bnh.
- Phc hi, iu chnh chc nng c th.
- Lm gim triu chng bnh.
- Chn on bnh.
- Phc hi hoc nng cao sc kho.
- Lm mt cm gic mt b phn hay ton thn.
- Lm nh hng qu trnh sinh sn.
- Lm thay i hnh dng c th.
huc lu hnh trn th trng a phn l cc tn dc v thuc y

hc dn tc (l cc thuc c sn xut theo phng php y hc c
truyn). rong c nhiu thuc di dng bit dc (bit dc l
nhng thuc mang tn ring, cn gi l tn thng mi ring ca mt c
s sn xut hay mt hng sn xut ln u t cho n v c php
a ra th trng ang c bo h quyn s hu cng nghip).
1.1.2. Cht lng thuc v yu cu cht lng
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Cht lng ca mt thuc l tng hp cc tnh cht c trng ca

thuc (v d; c cha ng cc thnh phn theo t l quy nh, c
tinh khit theo yu cu, ng gi c nhn quy nh,...) c th hin
mt mc ph hp vi nhng yu cu k thut nh trc tu theo
iu kin xc nh v kinh t, k thut, x hi,... nhm m bo cho
thuc t cc mc tiu sau:
- C hiu lc phng bnh v cha bnh.
- Khng c hoc t c tc dng c hi.
- n nh v cht lng trong thi hn xc nh.
- in dng v d bo qun.
huc l sn phm hng ho c bit, c quan h trc tip n sc

kho cng ng, n cht lng v hiu qu ca vic phng bnh, cha
bnh. V th thuc phi c bo m cht lng trong ton b qu
trnh sn xut (t nguyn liu cho n thnh phm), trong qu trnh bo
qun, lu thng phn phi n ngi s dng.
Mc tiu ca m bo cht lng trn ch c coi l t khi no

thuc p ng c cc yu cu c bn sau:
- huc c cha ng cc thnh phn theo t l quy nh ca cng

thc c ng k v c cp php (nh tnh, nh lng).
- huc c php sn xut v sn xut theo ng cc quy trnh

ng k v c php.
- C tinh khit t yu cu quy nh.
- huc c ng gi trong cc ng v bao gi vi nhn

thch hp v ng quy cch ng k.
- huc c bo qun, phn phi, qun l theo quy nh cht

lng ca thuc c duy tr trong sut tui th ng k hay thi hn
bo hnh.
t cc mc tiu trn, cn phi c nhiu yu t, trong 3 yu t

c bn phi c l:
a) Thc hnh sn xut thuc tt (GMP - Good Manufacture Practice)
hm sn xut ra c thuc theo d kin v t tiu chun k

thut t ra. Mun vy, phi tun th nhng quy nh cht ch v chi
tit v mi mt ca qu trnh sn xut, bao gm:
1) chc v nhn s.
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2) C s nh xng.
3) hit b.
4) V sinh.
5) guyn liu ban u.
6) hao tc sn xut.
7) Dn nhn v ng gi.
8) thng kim tra cht lng.
9) thanh tra.
10) s phn phi.
11) Cc khiu ni v bo co tai bin dng thuc.
b) Thc hnh kim nghim thuc tt (GLP - Good Laboratory

Practice)
Mc ch c bn ca LP l nhm xy dng c mt n v lm
cng tc kim nghim p ng y mi yu cu ca cng tc kim tra
cht lng thuc ra, m bo rng kt qu cc php phn tch thu
c l c tnh chn lc cao, chnh xc v ng n, c tnh php l.
ng thi gip cho vic tra cu v tm ra c nhanh chng ngun gc
cc sai st xy ra khi gp phi. Do vy, phi tun th nhng quy nh
cht ch v c chun ho cho mt c s kim nghim v cc mt:
1) chc v nhn s.
2) thng cht lng.
3) C s vt cht.
4) hit b phn tch v hiu chnh thit b phn tch.
5) huc th v cht i chiu.
6) iu chun cht lng v phng php phn tch.
7) Mu th.
8) h nghim v nh gi kt qu.
9) s ti liu.
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10) An ton trong phng th nghim.
c) Thc hnh bo qun thuc tt (GSP - Good Storage Practice)
hm gim st, kim tra cht ch thuc m bo cht lng n

ngi s dng. V vy, phi tun th nhng quy nh cht ch v nghim
ngt trong qu trnh bo qun, bao gm:
1) chc v nhn s.
2) h kho v trang thit b.
3) V sinh.
4) Cc quy trnh bo qun.
5) huc tr v.
6) i hng (vn chuyn bng cch gi hng).
7) s ti liu.
1.2. Kim tra cht lng thuc (Drug quality control)
1.2.1. Khi nim
Kim tra cht lng thuc l qu trnh o, xem xt, th nghim mt

hay nhiu c tnh ca thuc (thnh phm hoc nguyn liu) v so snh
kt qu vi yu cu t ra nhm xc nh s ph hp ca mi c
tnh .
khi nim trn ta thy kim tra cht lng thuc hay kim nghim
thuc l vic s dng cc phng php phn tch: l hc, ho hc, ho
l, sinh vt, vi sinh vt,... quy nh xc nhn mt thuc hay mt
nguyn liu lm thuc c t tiu chun quy nh hay khng. i mt
cch c th, kim tra cht lng thuc nhm tr li cc cu hi:
- y c phi l thuc cn kim tra khng?
- C m bo hot lc hay hm lng ng k khng?
- C t tinh khit theo yu cu khng?
- C b phn hu hay bin cht khng?
- bao gi, nhn c ng quy cch khng?
h vy, mc tiu c bn ca cng tc kim tra cht lng thuc l:
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- ngi s dng c dng thuc m bo cht lng, t hiu

qu s dng cao.
- Pht hin thuc khng t tiu chun, thuc gi, thuc km phm
cht,... x l v khng cho php lu hnh trn th trng.
rong ngnh Y t quy nh: t c cc thuc v nguyn liu lm

thuc u phi c kim nghim v xc nh cht lng, nu t tiu
chun quy nh mi c a vo s dng. Bi vy thuc phi c
kim tra cht lng mt cch nghim ngt, cht ch, bo m cho thuc
t cht lng trong mi hot ng sn xut, lu thng phn phi, xut
nhp khu, qun l v s dng thuc.
1.2.2. Khi nim v thuc t v khng t tiu chun, thuc gi

mo, thuc km phm cht
a) Thuc t tiu chun (thuc t cht lng)
L thuc p ng y cc yu cu k thut tiu chun ra

(hay thuc p ng y cc ch tiu cht lng trong tiu chun cht
lng ng k).
b) Thuc khng t tiu chun
L thuc khng p ng t nht mt ch tiu cht lng bt k trong

tiu chun ng k. huc khng t tiu chun l thuc km cht
lng.
c) Thuc gi
heo quy nh ca chc Y t th gii, thuc gi l ch phm

c sn xut khng ng vi nhn kha cnh nhn dng hay ngun
gc thuc, vi s c v mang tnh cht la o ca nh sn xut. Sn
xut sai thnh phn cng thc ng k, khng c hoc khng hm
lng hot cht, hoc c ng gi trong cc bao b gi mo. h vy,
c th ni thuc gi l nhng sn phm ca ngi sn xut mang
la o, gian ln. C th da vo mt s biu hin pht hin:
- huc khng c hoc c t dc cht.
- huc c cha dc cht khc vi tn dc cht ghi trn nhn.
- hn, bao gi ging hay gn ging vi nhn, bao gi ca mt thuc

khc,...
d) Thuc km phm cht
L thuc khng t tiu chun k thut m trc n t. Mc

khng t tiu chun c nhiu hnh thi khc nhau. t c cc nguyn
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nhn gy ra c th xc minh c bng cc phng php khoa hc, k

thut cho php. Cc nguyn nhn c th l:
- Do k thut sn xut, bo qun khng ng, nn thuc t bin cht.
- Do bao gi khng t tiu chun, nn a tp cht vo thuc.
- Do tui th (hn dng) ht.
- Do nguyn, ph liu khng t tiu chun.
- Do tc ng ca mi trng: nhit , nh sng, m,...
2. H THNG T CHC QUN L, KIM TRA CHT LNG THUC
h nc giao cho B Y t chu trch nhim qun l ton din cht

lng thuc. V vy, h thng t chc, qun l, kim tra cht lng thuc
ca ngnh Y t c chia lm 3 phn: thng qun l cht lng
thuc; thng kim tra cht lng thuc; thng thanh tra dc.
2.1. H thng qun l cht lng thuc
2.1.1. Cc qun l Dc Vit Nam
L c quan c B Y t u quyn thc hin cc nhim v trong lnh

vc qun l nh nc v cht lng thuc:
- Xy dng quy hoch, k hoch v qun l cht lng thuc v t

chc k hoch c ph duyt.
- Xy dng cc vn bn php quy v tiu chun v cht lng thuc

B ban hnh, hng dn kim tra vic thc hin cc vn bn trn.
- Qun l vic ng k tiu chun c s. Cung cp thng tin khoa

hc, k thut lin quan n m bo cht lng thuc.
- Ch o, gim st h thng kim tra cht lng thuc trn ton

quc.
- Kim tra v cp giy chng nhn c s sn xut t tiu chun

" hc hnh tt sn xut thuc" v phng kim nghim t tiu chun
" hc hnh tt kim nghim thuc".
- chc hng dn nghip v cho cn b qun l cht lng thuc

ca ngnh Y t, t chc o to v bi dng nghip v v tiu chun -
o lng - cht lng thuc.
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- Phi hp vi thanh tra B Y t thc hin chc nng kim tra, thanh
tra nh nc v cht lng thuc v x l vi phm php lut v cht
lng thuc theo thm quyn.
2.1.2. C quan qun l nh nc v cht lng thuc a phng
S Y t ch o qun l ton din v cht lng ca thuc a

phng (thng u quyn cho phng nghip v Dc) c nhim v:
- Ph bin, hng dn v t chc thc hin cc vn bn php lut

v qun l cht lng thuc ti a phng.
- hc hin chc nng kim tra, thanh tra nh nc v cht lng

thuc v x l vi phm v cht lng thuc trong phm vi a phng.
2.2. H thng kim tra cht lng thuc
2.2.1. C quan kim tra cht lng ca Nh nc v thuc
- rung ng l Vin Kim nghim trung ng ( i) v Vin

Kim nghim thnh ph Ch Minh.
ip B Y t qun l ch o cng tc kim tra cht lng thuc

trong ton quc v mt k thut. C nhim v:
+ ghin cu xy dng tiu chun Vit am v thuc.
+ Kim tra xc nh cht lng thuc lu hnh trn th trng.
+ hm tra k thut, gip B xt duyt cc tiu chun kim nghim

xt cp ng k sn xut v lu hnh thuc Vit am.
+ Pht hnh cc cht chun v cht i chiu dng trong kim

nghim.
+ Lm trng ti v cht lng khi c tranh chp khiu ni v cht

lng thuc.
+ ham gia o to cn b lm cng tc kim nghim.
+ vn v chnh sch cht lng thuc quc gia.
+ Xy dng tiu chun phng kim nghim thuc t tiu chun v

gip , kim tra cng nhn cc phng kim nghim thuc trong c
nc.
+ Kim tra vic kim nghim thuc theo tiu chun trong phm vi
ton quc.
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- tnh, thnh ph trc thuc rung ng l trung tm kim nghim

dc phm, m phm. l c quan trc thuc S Y t, c nhim v
nh Vin Kim nghim trung ng v Vin Kim nghim thnh ph
Ch Minh nhng gii hn trong phm vi tnh, thnh ph.
2.2.2. H thng t kim tra cht lng cc c s (phng kim

nghim, phng KCS)
Cng tc kim tra cht lng thuc c thc hin tt c cc c

s c lin quan ti thuc. u theo quy m ca c s sn xut (x
nghip, cng ty trung ng hoc a phng, cc c s nh,...), kinh
doanh (cng ty, ca hng,...), bnh vin (trung ng, a phng) m
lp phng kim nghim, phng KCS hay t kim nghim t kim tra
cht lng thuc.
Vi cc c s sn xut, bt buc phi c b phn t kim tra cht

lng. B phn ny phi c kh nng kim nghim xc nh cht lng
thuc c sn xut c s mnh theo tiu chun duyt. Phi kim
nghim, theo di c cht lng ca thuc trong sut qu trnh sn
xut t nguyn liu, bn thnh phm, thnh phm. Phi lp h s theo
di tng l sn phm. C s sn xut phi chu trch nhim v thuc do
c s sn xut ra.
Cc c s bo qun, phn phi thuc phi c b phn t kim

nghim (vi cc cng ty ln) hoc kim tra, kim sot qun l, nh
gi cht lng thuc, theo di cht lng trong qu trnh bo qun, cung
cp h s cht lng cho n v s dng thuc.
Cc bnh vin, tu theo quy m ln, nh cng phi c b phn kim

nghim cc thuc t pha ch, kim tra, kim sot cht lng thuc trc
khi phn phi n ngi s dng.
2.3. H thng thanh tra dc
Cng cc c quan qun l nh nc v cht lng thuc, thc hin

chc nng kim tra, thanh tra nh nc v cht lng thuc c t
chc t trung ng n a phng.
T LNG GI V BI TP
1. Mc tiu ca cng tc kim tra cht lng thuc. Cc yu cu c

bn t mc tiu trn.
2. i dung chnh ca cng tc kim tra cht lng thuc. iu kin

thuc c a vo lu thng, phn phi, s dng.
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3. h no l thuc t v khng t tiu chun? huc gi mo?

huc km phm cht?
4. rnh by h thng t chc kim tra cht lng thuc ca Vit

Nam.
Chn cu tr li ng cho cc cu hi 5 v 6 bng cch khoanh trn

ch ci u cu c chn:
5. heo phn cp:
a) thng qun l cht lng thuc Vit am gm:
A. Cc Qun l dc Vit am.
B. Vin Kim nghim trung ng.
C. rung tm kim nghim dc phm, m phm ca tnh.
D. Phng nghip v dc - S Y t.
b) thng kim tra cht lng thuc Vit am gm:
A. Phng hanh tra dc - S Y t.
B. Vin Kim nghim thnh ph Ch Minh.
C. rung tm kim nghim dc phm, m phm ca tnh.
D. Phng nghip v dc - S Y t.
6. Theo quy nh:
a) Mt thuc ghi trn nhn l vin nn paracetamol 500mg

nhng khi kim nghim th cha hot cht l aspirin, th ch
phm l:
A. huc t tiu chun.
B. huc khng t tiu chun.
C. huc gi.
D. huc km phm cht.
b) huc nh mt cloramphenicol 0,4% c 7 ch tiu yu cu v

cht lng, trong c ch tiu v th tch khng t, th
ch phm l:
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A. huc t tiu chun.
B. huc khng t tiu chun.
C. huc gi.
D. huc km phm cht.
Bi 2
CNG TC TIU CHUN HO V
KIM NGHIM THUC THEO TIU CHUN
MC TIU
- Trnh by c ni dung ca cng tc tiu chun ho.
- Trnh by c 3 ni dung chnh ca cng tc kim nghim thuc

theo tiu chun (ly mu, tin hnh kim nghim, nh gi kt qu v
vit phiu tr li).
1. CNG TC TIU CHUN HO
1.1. Khi nim
1.1.1. Mt s nh ngha
Tiu chun ho l mt lnh vc hot ng bao gm hai ni dung:

Xy dng cc tiu chun v p dng cc tiu chun trong thc t
nhm a cc hot ng ca x hi (c bit trong lnh vc sn xut v
kinh doanh) i vo n np t c hiu qu chung c li nht cho
mi ngi v cho x hi.
- iu chun l nhng quy nh thng nht v hp l c trnh by

di dng mt vn bn hoc mt th thc nht nh do mt c quan c
thm quyn ban hnh bt buc p dng cho nhng ni c lin quan.
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- i vi thuc, tiu chun l mt vn bn khoa hc k thut mang

tnh php ch trong quy nh: quy cch, ch tiu, yu cu k thut,
phng php th, ng gi, ghi nhn, bo qun v cc vn khc lin
quan n vic nh gi cht lng ca mt thuc (trong xy dng
tiu chun v yu cu k thut v phng php th l quan trng nht).
y l c s cc cc c quan kim nghim (hoc ngi kim
nghim) tin hnh thc nghim, nh gi kt qu, cng b kt qu (bng
phiu kim nghim) nh gi cht lng thuc l t hay khng t v
c c php lu hnh (hoc s dng) hay khng.
- V mt lch s, cng tc tiu chun ho gn lin vi lch s sn

xut ca loi ngi, ca cc phng thc sn xut ca tng ch x
hi khc nhau. hng hnh thc s khai ca tiu chun ho c t
thi c i, nhng pht trin c tnh t chc rng ri trn phm vi quc t
th ch c t u th k XX.
1.1.2. i tng ca cng tc tiu chun ho
Bao gm rt rng, hu nh trn tt c mi lnh vc, V d:
- Cc my mc, dng c, trang thit b cng ngh.
- guyn, nhin vt liu.
- ng, lm, hi sn, hng tiu dng.
- Cc nguyn tc, phng php, th tc, cc vn t chc, qun

l,...
- hut ng, k hiu, o lng,...
- Sn phm v bn sn phm.
rong ngnh Dc, mi hot ng sn xut, kinh doanh, s dng

thuc, mi vn c lin quan n cc i tng nu trn u phi tiu
chun ho.
1.1.3. Cc cp tiu chun v thuc
rc y, c 3 cp tiu chun l iu chun Vit am, iu chun

ngnh v Tiu chun c s.
in nay, ch p dng 2 cp tiu chun l iu chun Vit am v

iu chun c s.
- iu chun Vit am ( iu chun quc gia, Dc in Vit am)

(TCVN).
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- iu chun c s ( C hoc CZ) do cc c s sn xut bin son,

c hiu lc trong phm vi quy nh ca cc cp qun l. C hai loi iu
chun c s: i vi nhng sn phm lu hnh ngoi th trng th tiu
chun phi c ng k vi vi c quan c thm quyn; vi cc sn
phm khng lu hnh trn th trng m ch dng trong n v (bnh
vin) th tiu chun do th trng n v xt duyt v ban hnh.
Vi cc thuc c trong chuyn lun ca Dc in Vit am th

tiu chun c s phi c mc cht lng khng c thp hn cc mc
quy nh trong tiu chun Dc in Vit am.
1.2. Cng tc xy dng tiu chun
iu chun Vit am v thuc c nh nc u quyn cho B Y t

t chc bin son, xt duyt v ban hnh sau khi ng k ti Cc iu
chun o lng cht lng h nc Vit am, cc tiu chun ny
c tp hp trong mt b sch gi l Dc in Vit am ( i ng
Dc in c B Y t giao trch nhim ny). ip vic cho i ng
Dc in Vit am l Vn phng i ng Dc in.
Mt s thuc cha c CV s s dng C do cc c s sn xut

bin son v c cp c thm quyn duyt.
1.2.1. Phng php xy dng tiu chun v yu cu k thut
Khi xy dng tiu chun v yu cu k thut cn ch ti vic kt

hp gia cc loi ch tiu phn nh ht c cht lng ca thuc
ph hp vi iu kin k thut, kinh t v thc t: cc ch tiu phn nh
v cng dng ca thuc (th hin tinh khit v hm lng). Ch tiu
phn nh v mc tin cy v an ton ( c, bn, hn dng,...).
iu chun v tm, sinh l (dng thuc qua cc ng vo c th). Ch
tiu v thm m (hnh thc ng gi, trnh by p, bo qun,...).
Da trn cc ni dung chnh ca yu cu k thut, cn c vo thc

t, iu kin k thut, la chn ra cc ch tiu thch hp, khng qu
nhiu hoc qu t nhng ni ln c trng cht lng thuc, ph hp
vi iu kin c th. Sau phi xy dng c mc cho cc ch tiu
trn. Mc ch tiu l gi tr c th hay l khong gi tr m thuc phi t
c.
1.2.2. Phng php xy dng tiu chun v phng php th
a) Cc loi quy trnh v phng php th
Mc ch chnh ca vic tiu chun ho mt phng php th l

chn cho c mt quy trnh th hay quy trnh phn tch sao cho khi p
dng s cho mt kt qu gn vi gi tr thc nht. rong kim nghim
thuc, cc loi quy trnh th thng c chia thnh 3 loi:
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- Cc php th nh tnh: l cc php th nhm chng minh rng

cht cn phn tch c mt trong mu em th.
- Cc php th v tinh khit: l cc php th nhm chng minh

rng mu em th t (hay khng t) v mc tinh khit.
- Cc php th nh lng: l nhng php th nhm xc nh hm

lng ca mu th (hoc thnh phn chnh ca mu) hay hm lng
ca cc hot cht c trong mu em th. Cc php th ny c tin
hnh bng cc phng php nh lng ho hc, ho l, vt l, sinh
hc,...
b) Cc yu cu cht lng i vi mt phng php th:
c th hin mt s im chnh sau:
- C tnh tin tin: th hin chnh xc ( ng, chm), tnh

c hiu.
+ ng: Phng php khi p dng s cho kt qu gn vi gi tr

thc nht
+ lp li: Cho bit s ph hp gia cc kt qu (hay chm)

ca cc php xc nh song song.
+ nh c hiu: Phng php cho php xc nh ng cht cn

phn tch v t chu nh hng bi s c mt ca cc cht khc trong
mu th.
+ C gii hn pht hin cao: c biu th bng tr s tuyt i, tc

lng ti thiu c th pht hin c (thng tnh bng g = 10-6g);
hoc tr s tng i, tc nng gii hn c th pht hin c
(thng tnh theo nng g/ ml).
- C tnh thc t: Phng php th a ra phi ph hp vi iu

kin thc t, c tnh kh thi cao (ph hp vi trang thit b, my, k thut,
ho cht, thuc th, trnh con ngi,...).
- C tnh kinh t: Phng php th a ra t tn km m vn p

ng cc yu cu nu trn.
- C tnh an ton cao: An ton lao ng v bo v sc khe (t dng

ho cht c hi, trnh c cc thao tc k thut phc tp, nguy
him,...).
1.3. Cng tc p dng tiu chun trong thc t
1.3.1. Mc ch ngha
15
p dng tiu chun l mt mt cng tc ca ton b cng tc tiu

chun ho. Qua p dng :
- Kim chng li cc kt qu nghin cu khi xy dng tiu chun

(mc ch tiu c ph hp khng? Phng php th ng hay sai?...).
- Xc nh hiu qu kinh t ca tiu chun (tiu chun c kch thch

cho sn xut, kch thch tiu th). rn c s tip tc sa i, hon
thin nng cao cht lng ca tiu chun.
gn chn vic a cc thuc khng t tiu chun ra lu hnh, s

dng. Pht hin thuc gi, thuc km cht lng, pht hin nguyn nhn
vi phm v tm cc bin php khc phc.
1.3.2. Cc hnh thc p dng tiu chun trong thc t
a) p dng tiu chun trong sn xut
gha l phi thc hin ng cc tiu chun (k thut, th tc,

nguyn tc v cc quy nh c lin quan) sn xut ra thuc t tiu
chun. V d: Phi kim tra x l nguyn, vt liu t tiu chun mi a
vo sn xut; trong qu trnh sn xut phi kim tra; tt c cc cng
on, 100% l sn xut ti c s; kim tra thu nhn sn phm,...
b) p dng tiu chun trong kim tra cht lng
gha l tin hnh thc nghim tt c cc ch tiu yu cu k thut

theo ng phng php th nu nh gi xem thuc c t tiu
chun hay khng t tiu chun.
c) Kim tra p dng tiu chun
Cng vic ny c tin hnh thng xuyn cc c s hoc h

thng kim tra nh nc: Vin Kim nghim trung ng, Vin Kim
nghim thnh ph Ch Minh, trung tm kim nghim, thanh tra
dc,... i dung kim tra bao gm:
- Kim tra c s vt cht ca cng tc kim nghim: i liu, trang

thit b, phng th nghim, ho cht, thuc th,...
- Kim tra nguyn liu, bn thnh phm, thnh phm v tt c cc

thuc ang lu hnh trn th trng.
1.3.3. Sa i, sot xt li tiu chun
c tin hnh khi thy tiu chun khng cn ph hp.
1.4. Gii thiu Dc in Vit Nam
16
1.4.1. Mt s nt chung v Dc in Vit Nam
a) Dc in Vit Nam l mt ti liu bao gm
- p hp cc tiu chun nh nc ( CV ) v thuc (ho dc v

cc ch phm, huyt thanh v vaccin, dc liu, ch phm ng dc).
Mi tiu chun cn c gi l mt chuyn lun.
- hng quy nh chung trong cng tc kim nghim, gii thiu cc

phng php kim nghim chung, cc ho cht, thuc th, thuc chun,
ch th,... dng phn tch v nh gi cht lng thuc.
- Mt s ph lc, cc bng tra cu,...
b) Dc in Vit Nam c gi tn theo ln xut bn (ging cc

nc khc), tun theo quy tc ln sau ph nh ln trc
- Dc in Vit am gm 638 chuyn lun tn dc v 284

chuyn lun ng dc, c xut bn vo cc nm 1972, 1977.
- Dc in Vit nam gm 357 chuyn lun tn dc, 64 chuyn

lun ng dc, v 32 chuyn lun v vaccin, c xut bn vo cc
nm 1983, 1990, 1991, 1994.
- Dc in Vit nam gm 342 chuyn lun ho dc, 276

chuyn lun v dc liu, 37 chuyn lun v ch phm ng dc, 47
chuyn lun ch phm sinh hc v 500 chuyn lun v ho cht thuc
th, c xut bn vo nm 2002.
1.4.2. Mt s quy nh chung khi s dng Dc in Vit Nam (hay

dng trong cng tc kim nghim thuc)
C nhiu quy nh, di y nu tm tt ni dung chnh ca 7 quy

nh:
1) Khi nim "cn chnh xc" ngha l cn trn cn phn tch c

nhy n 0,1mg (0,0001g). Khi nim "ly khong" c ngha l ly mt
lng vi chnh khng qu 10% so vi yu cu. Khi nim "n
khi lng khng i" ngha l x l ch phm n khi no chnh lch
gia 2 ln k tip nhau < 0,5mg.
2) ng phn trm khng c ch dn g, coi l cch biu din theo

% Kl/ . Cn cc trng hp khc s ghi c th.
3) Khi nim "alcol" khng c ch dn g, c ngha l alcol cha

khong 96% ( / ) ethanol (C2 6 ). Ethanol khng c ch dn g khc
ngha l ethanol tuyt i.
17
4) V nhit : Dng thang bch phn, k hiu oC. Khi khng ghi
c th, quy c:
hit chun 20oC
hit thng 20 - 30oC
c m 40 - 50oC
c nng 70 - 80oC
c cch thu 98 - 100oC
hit trong th "v mt khi lng do lm kh cho php hiu l:

100 C2oC.
o
hit ni bo qun:
t lnh < -10oC
Lnh 2 - 10oC
Mt 10 - 20oC
hit phng 20 - 35oC
hit phng c iu nhit 20 - 25oC
Nng 35 - 40oC
t nng > 40oC

o
ung C
o
thm C
o
trng C
5) V phng php: C th dng phng php hay phng tin

khc vi quy nh trong Dc in hoc C nhng vi iu kin cc kt
qu c chnh xc tng ng nhau. u cc kt qu khc nhau th
coi phng php hoc phng tin quy nh trong Dc in hay C l
chnh thc.
6) V hm lng: u trong chuyn lun khng ghi gii hn trn th

c ngha l khng c qu 101,0%.
7) Khi th tinh khit, nu pht hin thy tp cht l khng ghi

trong chuyn lun th vn phi ghi vo kt qu th.
18
2. KIM NGHIM THUC THEO TIU CHUN
h trn nu, kim nghim thuc l vic tin hnh phn tch mt
mu thuc i din cho l thuc bng cc phng php ho hc, l
hc, ho l, sinh hc,... c quy nh xem thuc t hay
khng t tiu chun, t quyt nh xem c c php lu hnh hoc
s dng hay khng. s nh gi ny chnh xc, i hi phi lm tt 3
vic sau: ly mu kim nghim, thc hnh phn tch, nh gi kt qu v
vit phiu tr li (phiu kim nghim, phiu phn tch).
2.1. Ly mu kim nghim
2.1.1. Quy nh v ly mu
Ly mu l mt tp hp cc thao tc nhm ly ra mt lng mu

thuc i din kim tra cht lng. Do vy, kt lun v mu thuc
mang tnh php l, cn phi tun th mt cch nghim ngt cc quy nh
v th tc ly mu nh sau:
a) i tng ly mu
- Vi h thng t kim tra: L cc nguyn liu dng lm thuc, bao b

ng gi, sn phm trung gian, sn phm cha ng gi, thnh phm.
- Vi h thng qun l nh nc: huc v cc nguyn liu lm

thuc ang trong qu trnh lu thng hoc tn tr trong kho.
b) Cc trng hp ly mu
- rng hp t kim tra cht lng: Phi ly mu kim tra ton b

cc l thuc ti cc c s sn xut, lu tr, phn phi. Vi cc c s
sn xut thuc, yu cu 100% s l phi c kim tra. Vic ly mu do
cn b chuyn mn ca phng kim tra cht lng sn phm (KCS) tin
hnh, c s chng kin ca cn b n v ly mu. h trng n v
cn c vo quy nh chung c th c nhng quy nh c th hn cho ph
hp vi tnh hnh ca c s.
- rng hp kim tra gim st cht lng hoc thanh tra: u tin
ly mu kim tra v gim st l cc thuc cha bnh, c gi tr kinh t
cao, c cht lng khng n nh v c bit l c nghi ng v hm
lng hoc hiu lc tc dng.
Ly mu kim tra gim st cht lng ca cc c s sn xut (ly

10% s l sn xut trong nm) hoc ly theo quy nh ca B Y t, S Y
t.
Ly mu thanh tra t xut trong nhng trng hp c thng tin

v cht lng thuc xu, thuc khng an ton, t hiu lc v c bit l
thuc gi hay thuc km phm cht.
19
Vic ly mu c thc hin bi cc thanh tra vin hoc cc cn b

c giy u nhim ca c quan kim tra, thanh tra v c s chng kin
ca cn b c s.
c) Cc iu kin cn lu khi ly mu
- i ly mu: i ni cha sn phm, mi trng xung quanh

khng c gy nhim bn hoc tc ng lm thay i tnh cht ca
mu v ngc li khng mu tc ng xu n mi trng.
- gi ly mu: Phi l ngi c chuyn mn nht nh v p ng

c yu cu ca qu trnh ly mu.
- Phi quan st kim tra s b l hng (phn loi nu cn), nhn xt

v phi ghi vo bin bn ly mu.
- Dng c ly mu: Sch, kh, p ng yu cu cn ly mu.
- ng mu: p ng yu cu ly mu (sch, khng lm hng

mu, kh, c nhn ghi chp y ,...).
- hao tc ly mu: phi thn trng, t m, quan st cn thn,...
- Phng thc ly mu: gi ly mu phi t tay ly mu, ghi

nhn, lm bin bn, ng gi, nim phong bo m v bo qun mu.
c bit lu phi ly ch k xc nhn ca n v c ly mu.
2.1.2. Tin hnh ly mu
a) S ly mu
Vic ly mu phi bo m cho c tnh khch quan, i din cho

c cht lng ca thuc cn ly kim tra. V vy, phi lu ly theo
hng dn sau (quy trnh c tm tt theo s hnh 1).
- l sn xut ly ra cc n v bao gi mt cch ngu nhin, c

mu ban u ly theo ng ch dn.
- rn u thuc ca cc mu ban u v gp thnh nhng mu

ring ca tng n v bao gi.
- rn u cc mu ring thnh cc mu chung.
- mu chung ly ra mt lng mu trung bnh th nghim.
- mu trung bnh th nghim ly ra thnh cc mu lu v mu th

kim nghim.
20
Hnh 1. S ly mu thuc
Sau khi ly mu xong, ngi ly mu t tay dn nhn nim phong,

bao gi (phi c ch k xc nhn ca ngi ly mu v c s c ly
mu) v bin bn ly mu (cng phi c ch k xc nhn).
b) Ly mu c th
Cn c vo l thuc phi ly mu, xem xt phn loi tin hnh ly

nh sau:
- Ly mu thuc c phn liu (l sn phm thuc dng thuc c phn

liu):
l sn phm ly ra cc n v bao gi mt cch ngu nhin bt

k: Cc gi c ly ra phi c lp vi d kin ca ngi ly mu
(khng nn la chn theo cm quan ly mu xu hay mu tt). L thuc
phi ng nht, hp l v s lng hay khi lng (V d khng qu
500.000 vin vi thuc vin, khng qu 50.000 ng vi dng ng,...). S
bao gi trong l ly ra to mu ban u tnh theo cng thc:
rong : n l s bao gi ly ra; : s n v bao gi cui cng trong

l (v d vi thuc tim: cc ng ng trong hp giy, cc hp giy ng
trong hm th n v bao gi cui cng l hm).
Ch :
21
+ Khi tnh theo cng thc trn, nu phn thp phn nh hn 0,5 b
qua, nu ln hn 0,5 th tng thm mt n v.
+ Khi > 100 lu nmax 30.
+ Khi < 100 c th dng bng:
Bng 1. Hng dn s lng n v trong ly mu
N n
1 - 10 1
11 - 40 2
41 - 80 3
81 - 100 4
- Ly mu sn phm l cht rn (ht, bt, vin):
+ rng hp mt bao gi:
* rc khi ly, xem xt sn phm c ng nht khng, nu khng

ng nht phi chn ring ra tng loi v ly theo cc loi .
* rng hp sn phm l ht, cc, tr trng hp phi xc nh c

ht, cn tt c phi c nghin nh thnh bt (khng c lm nh
hng ti tnh cht ca sn phm).
* Ly mu ban u 3 v tr khc nhau: trn, gia, di, sau trn

thnh mu chung.
* Dn u lng mu chung thnh lp phng hnh vung, dy khng

qu 2cm, chia mu thnh 2 ng cho, b 2 phn i din (hnh 2),
trn u 2 phn cn li v chia tip cho n khi lng mu cn li tng
ng vi 2 - 4 ln mu th cn ly. l mu trung bnh th nghim.
* Chia mu trung bnh th nghim thnh cc mu lu v mu kim

nghim.
Hnh 2. S ly mu ch phm l cht rn
22
* i vi thuc vin ch ng trong mt bao gi: cng ly mu ba v

tr khc nhau trong bao gi, chai, l, sau trn thnh mu chung, mu
trung bnh th nghim,... nh trn.
y mu ban u
theo cng thc: nu trn.
- Ly mu l sn phm lng:
+ rng hp mt bao gi: u sn phm l ng nht th ly mu

bt k v tr no cng c. u khng ng nht, trc khi ly mu phi
khuy u, sau mi ly mu.
+ rng hp nhiu bao gi: ly theo cng thc:
u l nhng chai l nh th c th ly ht th tch.
- Ly mu l cc sn phm thuc m, bt nho:
in hnh ly mu nh cc sn phm lng nhng ch khuy k,

trn u c hn hp ng nht, sau mi ly mu.
- ng gi v dn nhn:
Sau khi ly mu v cho vo ng, ngi ly mu ng gi, dn

nhn v nim phong mu, lm bin bn ly mu. Lu phi c ch k
xc nhn ca c s c ly mu nhn nim phong v bin bn ly
mu.
2.2. Tin hnh kim nghim
2.2.1. Nhn mu
B phn nhn mu ca c quan kim nghim phi kim tra xem mu

c p ng cc yu cu khng (cn nim phong khng, c thng
tin khng,...).
2.2.2. Kim nghim, x l kt qu
Cng vic ny do b phn k thut thc hin. hng thng gm

cc ni dung sau:
- Chun b ti liu: theo CV hoc C.
- Chun b dng c, ho cht, my,... p ng yu cu m tiu

chun quy nh. B tr th nghim mt cch hp l c mu lm v
khng lm nhim bn hoc bin cht mu cn th.
23
- in hnh cc th nghim phn tch theo tiu chun.
- Ngi lm kim nghim phi c cun s ghi chp y cc s

liu khi tin hnh th nghim, s ny gi l s tay kim nghim vin. S
tay kim nghim vin c coi l chng t gc ca cc s liu sau ny
cng b trn phiu tr li kt qu kim nghim (gi l phiu kim
nghim).
- X l cc s liu thc nghim quyt nh xem cc ch tiu th

theo tiu chun t hay khng t yu cu.
2.2.3. Vit phiu tr li kt qu
Kt qu kim nghim s c tr li bng phiu kim nghim hay

phiu phn tch.
(Cch trnh by Phiu kim nghim c trnh by chi tit mc 2.2

bi 3).
2.2.4. Lu mu kim nghim ti c quan kim nghim
Mu lu phi c nh s cng vi s ng k mu th cng loi,

nhng c nhn ring vi ch "mu lu" v bo qun trong iu kin theo
quy nh chung, mu ny c s dng n trong trng hp c tranh
chp v kt qu cng b ( Phiu kim nghim). hng thng, mu
lu ly t mt phn mu ly th, do vy s lng ly phi ging
nh mu ly th.
Cc mu lu phi c gi li theo ng thi gian quy nh. Cc

mu c hn dng phi lu tip 3 thng k t khi ht hn dng. Khi ht
thi gian lu, c quan lp bin bn x l theo quy ch.
S sch, phiu kim nghim phi lu gi t nht l 3 nm. Khi ht

hn lu, mun hu phi c gim c c quan duyt.
T LNG GI V BI TP
1. i dung chnh ca cng tc tiu chun ho.
2. rnh by phng php xy dng tiu chun v yu cu k thut.

V phng php th. Yu cu cht lng i vi mt phng php
th.
3. i dung chnh ca cng tc p dng tiu chun trong thc t.
4. rnh by mt s quy nh chung khi s dng Dc in Vit am

(dng trong cng tc kim nghim thuc).
24
5. Cch tin hnh ly mu kim nghim.
6. rnh by cc nhim v ch yu khi tin hnh kim nghim.
7. in cm t cn thiu vo ch trng trong cu di y:
a) Cc thuc c trong chuyn lun ca Dc in Vit am th

tiu chun c s phi c mc cht lng....................................
so vi tiu chun Dc in Vit am.
b) Cc yu cu chnh v cht lng i vi mt phng php

kim nghim gm: C tnh tin tin,......................................., c
tnh kinh t, c tnh an ton cao.
c) nh tin tin ca phng php kim nghim th hin

...................., tnh c hiu.
Chn cu tr li ng cho cc cu hi t 8 n 10 bng cch khoanh

trn ch ci u cu c chn:
8. heo quy nh:
a) S lng n v ly mu i vi l thuc c tng s 8 n v

ng gi l:
A. 1 B. 2 C. 3 D. 4
b) S lng n v ly mu i vi l thuc c tng s 850 n

v ng gi l:
A. 1 B. 2 C. 3 D. 4
c) S lng n v ly mu i vi l thuc c tng s 25 n

v ng gi l:
A. 1 B. 2 C. 3 D. 4
d) S lng n v ly mu i vi l thuc c tng s 103 n

v ng gi l:
A. 1 B. 2 C. 3 D. 4
9. Dc in Vit am quy nh v nhit :
a) hit thng l:
A. 20oC B. 20 - 30oC C. 70 -
80oC D. 40 - 50oC
25
b) c nng c nhit l:
A. 60oC B. 50 - 65oC C. 70 -
80oC D. 100oC
c) c cch thu c nhit l:
A. 98 - 100oC B. 65 - 75oC C.
80oC D. 105oC
10. Dc in Vit am quy nh:
a) ii hn hm lng, nu trong chuyn lun khng ghi gii hn

trn th c ngha l khng c qu:
A. 100,0% B. 100,5% C.
101,0% D. 102,0%
b) Dc in Vit am quy nh v sy hoc nung n khi

lng khng i, ngha l sy hoc nung ch phm n khi no
chnh lch gia 2 ln cn k tip nhau nh hn:
A. 0,5mg B. 0,4mg C. 0,3mg

D. 0,6mg
26
Bi 3
PHNG PHP X L S LIU, TNH TON
V TR LI KT QU KIM NGHIM
MC TIU
- Trnh by c ba loi sai s v cch hn ch cc sai s ny trong

kim nghim.
- Tnh c sai s ca kt qu thc nghim.
- Bit cch ghi chp, trnh by kt qu thc nghim v phiu kim

nghim.
- Trnh by c nm cch x l mu thng dng trong kim

nghim.
1. SAI S TRONG KIM NGHIM
1.1. Mt s khi nim
rong kim nghim thuc, ta thng phi tin hnh cc php th

nghim: o lng hay phn tch nh lng theo mt quy trnh c mt
s ln trn mu th v thu c cc kt qu tng ng x1, x2,... xn.
Gi tr trung bnh l ng tin cy hn c v

c ly lm kt qu ca php xc nh.
i tr trung bnh thng khc vi gi tr thc

xc nh, s sai khc ny chnh l sai s ca php xc nh.
Kt qu ca php xc nh c nh gi chnh xc ( ng
v chm).
+ ng phn nh s ph hp gia kt qu thc nghim thu c

(
+ chm ( lp li) phn nh s ph hp gia cc kt qu thu

c (x1, x2,... xn) trong cc th nghim cng iu kin quy nh ca
php xc nh (gi l cc php xc nh song song).
C th biu th sai s di dng sai s tuyt i v sai s tng i.
+ Sai s tuyt i:
27
+ Sai s tng i l t s gia sai s tuyt i v gi tr trung bnh
Khi tnh ton, nu thu c gi tr dng l sai s tha, gi tr m l

sai s thiu.
1.2. Cc loi sai s
1.2.1. Sai s th
L sai s khi kt qu thu c khc xa vi gi tr trung bnh ( ) hay
l do s cu th ca ngi lm, hay yu t khch quan do s thay i

t ngt no ca iu kin thc nghim.
loi sai s th cn lm nhiu ln v loi i nhng gi tr khng

hp l theo nhng quy tc nht nh.
1.2.2. Sai s h thng
- L sai s c th bit r nguyn nhn, n lm cho kt qu bin i

theo quy lut nht nh, nh hng n chnh xc ca kt qu.
- C th pht hin v loi tr sai s h thng bng cch hiu chnh li

thit b o, thay ho cht, thuc th t tiu chun quy nh, phn tch
mu chun, mu trng, c bit ch yu t k nng v tay ngh ca
ngi lm.
1.2.3. Sai s ngu nhin
quanh gi tr trung bnh, lm nh hng ti lp li ca kt qu, lm

gim chnh xc ca php xc nh.
sai s ny bng cch tng s th nghim v x l s liu bng phng

php thng k.
1.3. Tnh sai s ca kt qu thc nghim
1.3.1. i vi cc php th nghim thng thng
nghim vi cc quy trnh n nh, c chun ho, sai s tng

1% chng ta ch cn tin hnh thc hin ton b quy
trnh t 2 3 ln v ly kt qu l gi tr trung bnh ca 2 3 ln xc nh
.
28
chun, c th kt lun mu th em kim nghim t hay khng t tiu

chun.
1.3.2. i vi cc php th nghim mi nghin cu, p dng cho

cc i tng mu th mi (hay thm nh nh gi quy trnh th
nghim)
trnh th cng iu kin nhiu ln hn (t nht 5 6 ln) v s dng

phng php thng k nh gi kt qu th nghim.
- nh gi tr trung bnh:
- nh lch chun S (c trng cho lp li ca php xc nh,

cho bit mc st gn ca cc gi tr xc nh c xi so vi gi tr
trung bnh ):
rong thng k S2 gi l phng sai.
rong t l mt tr s ph thuc vo n (hay bc t do K = n - 1) v
Bng 2
K=n-1 1 2 3 4 5 6 7 8 9 10 20 Ln
t 12,7 4,3 3,2 2,8 2,6 2,5 2,4 2,3 2,3 2,2 2,1 2,0
0,95
t 63,7 9,9 5,8 4,6 4,0 3,7 3,5 3,4 3,3 3,2 2,8 2,6
0,99
29
hay .
h vy bin gii tin cy hay cn tin cy, hoc gii hn tin cy l gii
hn hai bn ca
* Sai s tng i l .
V d:
Kt qu nh lng cht XC (g/l) ca 5 th nghim cng iu kin

ca mt mu th l: 2,25; 2,19; 2,11; 2,38; 2,32.
- nh sai s tng i ca php nh lng?
Gii:
- nh gi tr trung bnh:
- nh lch chun:
- nh gii hn tin cy:
- Kt qu xc nh:
- Sai s ca php xc nh (Sai s tng i):
1.4. Phng php x l mu th
30
X l mu th l bc u tin, quan trng trong phn tch mu, n

thng l mt trong nhng nguyn nhn quyt nh dn n sai s ca
php th nghim. hn ch sai s, khi tin hnh kim nghim phi ht
sc lu giai on ny.
Mu th thng trng thi lng, rn, kh vi thnh phn rt a

dng: c th l cht v c, hu c, khong vt, thc vt,... do vy tu
thuc vo c im c th ca mu th v mc ch ca php xc nh
m ta la chn k thut x l mu cho thch hp. hng thng c mt
s cch sau y:
1.4.1. Ho tan mu
- Vi nhiu trng hp, chng ta c th dng nc ho tan

chuyn cht cn xc nh c trong mu th sang dung dch nc.
- i vi cht kh tan trong nc, c th ho tan bng dung dch

acid, dung dch kim, dung dch ca cht oxy ho kh thch hp, chuyn
ta kh tan thnh ta d ho tan.
1.4.2. Phn hu bng acid mnh
rong qu trnh phn hu mu th c th din ra cc phn ng oxy

ho, thu phn, ph hu cc lin kt ho hc,... Cc acid hay dng trong
x l mu l: acid hydrocloric c ( Cl), acid nitric c ( 3), acid
sulfuric c ( 2SO4), acid percloric (HClO4), hn hp Cl + 3, HNO3
+ HClO4, HNO3 + H2SO4, H2SO4+ H2O2,... C th thc hin qu trnh x
l mu nhit thng hoc nhit cao.
1.4.3. Phn hu mu bng k thut vi sng
y l phng php dng nhit da trn nng lng ca sng in

t c bc sng t 1 1000mm. Qu trnh tin hnh c th thc hin
trong bnh vi sng, bom vi sng, l vi sng.
1.4.4. Phn hu bng nhit
Phng php ny c dng ph bin phn hu cht hu c,

chuyn chng thnh cc cht bay hi. C th thc hin bng cch t
trn ngn la, t trong ng kn, t mu trong bnh kn c oxy hoc
nung trong l nung.
1.4.5. X l mu bng k thut tch pha
Cc cht cn xc nh trong mu th c th tch bng cch: kt ta,

chng ct, chit bng dung mi (lng lng, lng rn), cc k thut
sc k,...
31
Ch : rong qu trnh x l mu th cn lu bo ton c cht

cn xc nh (tch c hon ton, khng c mt mu) v khng
c a cht l vo lm nh hng ti kt qu th nghim.
2. TNH TON V TR LI KT QU KIM NGHIM
2.1. Tnh ton kt qu kim nghim
Kim nghim thuc thng tin hnh theo tiu chun c sn ( iu

chun Dc in Vit am (DV ) hoc C). Kim nghim vin cn
tun th nghim ngt cc yu cu ca php th, cc kt qu v s liu
thu c phi khch quan v chnh xc, c ghi chp li vo h s gi
l S tay kim nghim vin. S tay kim nghim vin c coi l chng
t gc ca cc s liu sau ny cng b trn phiu tr li kt qu kim
nghim (gi l Phiu kim nghim).
- X l cc s liu thc nghim v so snh vi tiu chun quyt

nh xem cc ch tiu th theo tiu chun t hay khng t yu cu.
2.2. Vit phiu tr li kt qu kim nghim
phiu phn tch.
Phiu kim nghim l vn bn php l ca cc t chc kim tra cht

lng thuc, xc nhn kt qu kim nghim theo ti liu k thut hp
php ca mt mu thuc.
Phiu phn tch l vn bn php l xc nhn kt qu phn tch ca

mt hay nhiu tiu ch trong tiu chun k thut ca mt mu thuc.
Do vy, sau khi hon thnh cc th nghim v x l s liu, nh gi

kt qu, kim nghim vin phi vit vo phiu tr li ni b (cha phi
phiu chnh thc), k tn chu trch nhim v a cho cn b ph trch
phng duyt li, trc khi a phng chc nng trnh lnh o duyt ln
cui, sau tr li chnh thc bng phiu ca c quan kim nghim (gi
l Phiu kim nghim hay Phiu phn tch). Cu ch vit trong phiu
kim nghim phi r rng, chnh xc, gn, y v thng nht.
- i dung chnh ca mt phiu kim nghim bao gm:
1) n c quan kim nghim.
2) S phiu kim nghim.
3) n mu kim nghim.
4) i sn xut.
32
5) S l, hn dng.
6) gi v ni gi mu.
7) Yu cu kim nghim (ghi r ni dung, s, ngy, thng, nm ca

cng vn hay giy t km theo).
8) gy thng, nm nhn mu.
9) S ng k kim nghim.
10) gi nhn mu.
11) iu chun th nghim.
12) nh trng mu khi nhn v m nim phong kim nghim.
13) Cc ch tiu kim nghim, cc gii hn cho php v kt qu.
14) Kt lun.
15) gy thng nm cp phiu kim nghim.
16) h trng n v kim nghim k v ng du.
2.3. V d
rung tm kim nghim Dc phm v m phm tnh V nhn mt

mu kim nghim l vin nn vitamin C 100mg ca Cng ty Dc phm
X. Sau khi tin hnh kim nghim theo tiu chun, kt qu c ghi
trong S tay kim nghim vin nh sau:
a) Tnh cht
Bng cm quan (mt quan st di nh sng thng v ngi) thy

ch phm l vin mu trng hay trng ng, gn nh khng mi.
Kt lun: t yu cu.
b) nh tnh
A. ghin mn 5 vin. Ly 0,15g bt vin, thm 10 ml nc. Lc, lc.
- hng giy qu vo dch lc: giy qu chuyn sang mu .
- h tng git dch lc vo 1 ml dung dch thuc th 2,6

diclorophenol indophenol: mt mu xanh.
33
- h tng git dch lc vo 1 ml dung dch bc nitrat 5% trong ng

nghim: ta en v lp bc trng bm y ng nghim.
B. Ly 5 ml dch lc vo ng nghim, thm ln lt 0,05 ml dung dch

natri nitroprusiat 1%, 2 ml dung dch natri hydroxyd 2M v nh tng git
dung dch acid hydrocloric 25%: mu vng chuyn thnh mu lam.
Kt lun: ng theo tiu chun.
c) ng u khi lng
Cn ring bit 20 vin:
164,0mg 149,6mg
156,2mg 160,1mg
158,0mg 147,8mg
156,9mg 162,3mg
154,5mg 160,3mg
159,4mg 149,2mg
157,2mg 152,6mg
151,9mg 155,3mg
160,8mg 158,3mg
153,9mg 156,1mg
Khi lng trung bnh:
Vin c khi lng cao nht l 164,0mg, chnh lch so vi gi tr

trung bnh:
Vin c khi lng thp nht l 147,8mg, chnh lch so vi gi tr

trung bnh:
Kt lun: t yu cu.
d) r
34
- Mi trng th: nc.
- hit : 37oC 0,5oC.
- Cho vo mi ng th mt vin nn, y a cht do. h 6 vin.
- Quan st bng mt: cc vin r ht thi im 5,45 pht.
Kt lun: t yu cu.
e) nh lng
- m20 vin TB = 0,15622g.
- Cn bt vin: mT (g).
- Ho tan mT bng hn hp (bao gm 100 ml nc v 10 ml dung

dch acid acetic 1M) trong bnh nh mc 100 ml.
- Lc.
- 50,0 ml dch lc +1 ml dung dch h tinh bt. nh lng ht V ( ml)

dung dch iod 0,1N c K = 1,0033.
m lng X (%) acid ascorbic trong ch phm so vi hm lng

ghi trn nhn c tnh theo cng thc sau:
Kt qu:
Ln 1 2 3
mT (g) 0,3165 0,3123 0,3140
V ( ml) 11,30 11,20 11,25
X (%) 98,56 99,00 98,90
m lng trung bnh:
Kt lun: t yu cu.
35
kt qu kim nghim v tnh ton, rung tm kim nghim vit

phiu v tr li kt qu cho Cng ty Dc phm X c trnh by nh
sau:
UB D V C X C A
kim nghim Dc phm v V AM
M phm
a ch c quan
PHIU KIM NGHIM

S: 05/K - 2006
Mu kim nghim: Vin nn vitamin C 100mg
Ni sn xut: Cng ty Dc phm X
S l, hn dng: L 010106 Hn dng: 01 2008
Ngi v ni gi mu: B T Cng ty Dc phm X
Yu cu kim nghim (ghi r ni dung, s, ngy, thng, nm ca cng

vn hay giy t km theo): Kim tra cht lng
Ngy, thng, nm nhn mu:15/01/2006 S ng k KN: 03 KN
Ngi nhn mu: rn h h
Tiu chun: Dc in Vit am
Tnh trng mu khi nhn v m nim phong kim nghim: huc

c ng trong l nha mu nu, nt kn, ngoi c dn nhn, in r
rng.
Yu cu Kt qu
1. Tnh cht: Vin nn mu trng hay trng ng, gn nh

t
khng mi.
ng
2. nh tnh: Phi cho php th nh tnh ca acid ascorbic
t
3. ng u khi lng: Khi lng trung bnh vin
7,5% t
4. r: Khng qu 15 pht
t
5. nh lng: m lng acid ascorbic (C6H8O6
(98,82%)
110,0% so vi lng ghi trn nhn.
36
Kt lun: Mu th t yu cu cht lng theo tiu chun Dc in

Vit am I.
gy... thng... nm...
h trng n v
(k v ng du)
T LNG GI V BI TP
1. rnh by cc loi sai s v cch khc phc.
2. rnh by cc bc nh gi sai s ca kt qu th nghim.
3. y nu 5 k thut x l mu.
4. Kt qu xc nh hm lng (g/l) cht X c trong mu th tin hnh

5 ln th nghim song song thu c nh sau:
Ln 1 Ln 2 Ln 3 Ln 4 Ln 5
0,0271 0,0282 0,0279 0,0271 0,0275
0,95.
5. in cm t cn thiu vo ch trng trong cu di y:
Phng php thng thng x l mu gm: o tan

mu,........................(A)............................, phn hu mu bng k
thut vi sng, phn hu bng nhit, x l mu bng k thut tch
pha. Phng php phn hu bng nhit dng phn
hu...............(B)............... Phng php ny c th thc hin bng
cch...........(C)............... trn ngn la hoc.......(D)................ trong
l nung.
6. rnh by ni dung chnh ca mt phiu kim nghim.
37
Bi 4
DUNG DCH CHUN, DUNG DCH ION MU,
THUC TH, CH TH MU
THNG DNG TRONG KIM NGHIM
MC TIU
- Trnh by c cch pha cc dung dch chun, dung dch ion mu,
thuc th, ch th mu thng dng trong kim nghim thuc.
- Tnh c h s hiu chnh ca dung dch chun khi pha bng

cc phng php khc nhau.
1. DUNG DCH CHUN
1.1. Cht i chiu
Cc dung dch chun c pha t ho cht tinh khit, t tiu chun

ca cht i chiu. Dc in Vit am cho php s dng cc cht i
chiu quc gia Vit am c thit lp, bo qun v phn phi ti Vin
Kim nghim theo s phn cng ca B Y t. hng cht i chiu quc
t, khu vc hay quc gia khc c s dng s do B Y t quy nh.
Cht i chiu l cht ng nht c xc nh l ng dng

trong cc php th c quy nh v ho hc, vt l v sinh hc.
rong cc php th , cc tnh cht ca cht i chiu c so snh
vi cc tnh cht ca cht cn th. Cht i chiu phi c tinh khit
ph hp vi mc ch s dng (nh tnh, nh lng).
1.2. Cch s dng cht i chiu
p ng mc ch s dng, cht i chiu phi c bo qun,

theo di v s dng ng. heo quy nh thng thng, cht i chiu
c ng trong bao b gc, kn, c nhn r rng, bo qun nhit
thp, trnh nh sng v m; nu cn iu kin bo qun c bit khc
th c hng dn ghi trn nhn.
rc khi m bao gi dng, cht i chiu cn c mt thi

gian t ti nhit phng th nghim.
Cc php th c tin hnh ng thi trn mu th v mu i

chiu c chun b trong cng iu kin ghi trong chuyn lun.
u trn nhn ca cht i chiu khng c ch dn phi lm kh v

trong php th ring ca chuyn lun khng ch nh phi lm kh th c
38
th s dng ngay cht i chiu m khng phi lm kh. rong trng

hp ny, cn hiu chnh li lng cn ca cht i chiu do khi lng
b gim khi lm kh hoc do hm lng nc. Mt khi lng do lm
kh hoc hm lng nc c xc nh theo hng dn chuyn
lun ca cht thuc tng ng. Khi cht i chiu c nc kt tinh, c
th c hng dn c bit trong mt php th ring.
1.3. Cc dung dch chun
rong kim nghim thuc bng phng php ho hc, cc dung dch
chun c pha t ho cht t tiu chun cht gc v dng xc
nh hm lng cc cht cn nh lng.
1.3.1. Quy nh chung
hng dung dch chun l nhng dung dch c nng c bit

chnh xc dng trong phn tch nh lng theo th tch.
ng ca cc dung dch chun thng c biu th bng:
ng ng lng gam : S ng lng gam cht tan trong

1000 ml dung dch.
ng phn t gam M: S phn t gam cht tan trong 1000 ml

dung dch.
u nng thc ca dung dch khng ng vi nng l thuyt

th cn tnh thm h s hiu chnh K. s ny l t s ca nng
thc Cthc v nng l thuyt Cl thuyt: . Khi nhn h s K

vi th tch ca mt dung dch chun ta c th tch ng ca dung
dch chun vi h s K = 1,000.
1.3.2. Phng php chung pha ch cc dung dch chun
C 4 phng php thng c dng pha ch v chun ho cc

dung dch chun trong kim nghim thuc:
a) Pha ch t cht gc
Cn chnh xc mt lng cht gc tng ng vi lng cht l

thuyt c tnh da vo nng v th tch dung dch chun cn
pha, ho tan trong dung mi va th tch (dung mi thng dng
l nc ct khng c carbon dioxyd). s hiu chnh K ca dung dch
ny c tnh bng lng cn thc t chia cho lng cht l thuyt.
39
V d: Pha 100,0 ml dung dch 2C2O4 0,1000 t cht gc

H2C2O4.2H2O c alt = 0,6303g. Khi tin hnh pha, lng cn
H2C2O4.2H2 thc t l 0,6290g. Vy:
b) Pha gn ng ri chun ho bng cht gc hoc mt dung dch

chun khc c h s K bit
- Dng cht gc: chun b dung dch chun t ho cht tinh khit t
tiu chun cht gc, sau khi c lm kh iu kin nht nh c
quy nh ring i vi tng cht. Cn chnh xc mt lng cht chun
gc, cho vo bnh nn, ho tan bng dung mi thch hp, chun bng
dung dch chun mi pha. nh h s hiu chnh theo cng thc:
rong :
a: lng cht gc cn, tnh bng g.
: chun l thuyt ca dung dch mi pha tnh theo cht gc, tnh
bng g/ ml.
V: th tch dung dch chun dng, tnh bng ml.
V d: Pha v xc nh nng dung dch chun a 2S2O3 0,1 t

Na2S2O3.5H2 (khng phi l cht gc).
V Na2S2O3.5H2 d mt nc kt tinh nn khng tho mn yu cu

cht gc, do pha dung dch chun a2S2O3 c nng xp x 0,1
bng cch: Cn trn cn k thut 24,82g a2S2O3.5H2O, ho tan vo
nc mi un si ngui, thm mt t a2CO3, thm nc cho
khong 1 lt trn u. vi ngy n nh, sau xc nh li nng .
ng dung dch a2S2O3 c xc nh bng cht gc K2Cr2O7

c T = 0,004904g/ ml nh sau: Cn chnh xc 0,1506g K2Cr2O7 ho tan
trong khong 50 ml nc ct trong mt bnh nn nt mi, thm 10 ml
dung dch K 20%, 5 ml dung dch Cl c. y nt v yn ch ti 10
pht. Thm 200 ml nc v chun bng dung dch a2S2O3 iu ch
trn n khi dung dch chuyn sang mu vng lc. hm 2 ml dung
dch h tinh bt v tip tc chun n khi dung dch chuyn t mu
xanh lam sang lc nht ht 30,5 ml dung dch a2S2O3.
s hiu chnh K ca dung dch a2S2O3 c tnh theo cng

thc:
40
- Dng mt lng chnh xc dung dch chun khc c h s K 0

bit:
rong trng hp ny, h s hiu chnh K c tnh theo cng thc:
rong :
C0 l nng ng lng l thuyt.
V0 l th tch (tnh bng ml) v K0 l h s hiu chnh ca dung dch

chun dng chun ho.
C: nng ng lng l thuyt ca dung dch chun cn pha.
V: th tch dung dch chun cn xc nh h s K, tnh bng ml.
V d: Pha v xc nh nng dung dch chun a 0,1 t

NaOH.
V a d ht m v d b carbonat ho nn khng tho mn yu

cu cht gc, do pha dung dch chun a c nng xp x 0,1
bng cch: o tan 4,50g a trong 5 ml nc. y kn bnh cha
bng nt cao su, yn 1 ngy ri gn ly dung dch trong pha trn v
pha long vi nc ct mi un si ngui n va 1 lt, trn u.
Sau xc nh li nng dung dch a bng dung dch Cl 0,1

c K = 0,9985 nh sau: Ly chnh xc 20,0 ml dung dch a
iu ch trn, thm 2 git dung dch da cam methyl v chun bng
dung dch Cl 0,1 n khi dung dch chuyn t mu vng sang hng
da cam ht 20,5 ml.
s hiu chnh K ca dung dch a c tnh theo cng thc:
c) Pha long nhng dung dch chun c nng cao
Dng dng c ong, o th tch chnh xc pha long cc dung

dch chun c nng cao thnh dung dch c nng thp hn
bng dung mi tng ng.
41
s hiu chnh ca dung dch pha c chnh l h s hiu chnh

ca dung dch dng pha long. hng dung dch chun c
nng nh hn 0,1 c chun b theo cch ny ngay trc khi
dng.
V d: chun b dung dch iod 0,01 , ngi ta ly chnh xc

10,00 ml dung dch iod 0,1 c K = 1,005 pha long trong va 100,0
ml bng nc ct. Dung dch iod mi pha c c nng l 0,01 vi
K = 1,005.
d) Dng ng chun
hng ng chun c cha mt lng cht gc va pha thnh

mt th tch nht nh dung dch chun . Dng dung mi pha ch theo
ng k thut ghi trn nhn ng, ta s c dung dch chun c nng
chnh xc theo quy nh.
V d: Pha dung dch Ag 3 0,1000 t ng chun Ag 3 0,1N c

ch dn pha va trong 1000 ml nc.
Chuyn ton b lng ho cht c trong ng chun vo bnh nh

mc 1000 ml, dng nc trng ra k ng ng cht chun. p trung
nc ra vo bnh nh mc trn. o tan v pha long trong nc ti
va 1000 ml.
2. DUNG DCH ION MU
Cc dung dch ion mu thng c chun b dng lm mu so

snh trong thc hin php th gii hn tp cht kim nghim nguyn
liu lm thuc. Cc dung dch ion mu c pha nng cao v c
pha long ti nng thch hp ngay trc khi dng.
2.1. Dung dch amoni mu 100 phn triu NH4
Cn chnh xc 0,297g amoni clorid sy kh 100 - 105oC n

khi lng khng i, ho tan vo nc trong mt bnh nh mc 1000
ml. hm nc va n vch.
2.2. Dung dch arsen mu 1000 phn triu As
Ho tan 0,330g arsen trioxyd trong 5 ml dung dch natri hydroxyd 2 M

v thm nc va 250 ml.
2.3. Dung dch calci mu 1000 phn triu Ca
Cn chnh xc 0,625g calci carbonat sy kh 100 - 105oC n

khi lng khng i, cho vo bnh nh mc 250 ml. Thm 3 ml dung
dch acid acetic 5 M. Lc cho tan. hm nc va n vch, lc u.
42
2.4. Dung dch clorid mu 500 phn triu Cl
Cn chnh xc 0,0824g natri clorid sy kh 100 - 105oC n

khi lng khng i, cho vo bnh nh mc 100 ml, ho tan vi nc
v thm nc va n vch, lc u.
2.5. Dung dch ch mu 1000 phn triu Pb
o tan 0,400g ch ( ) nitrat trong nc v thm nc va 250

ml, lc u.
2.6. Dung dch kali mu 2000 phn triu K
o tan 0,446g kali sulfat trong nc va 100 ml.
2.7. Dung dch magnesi mu 100 phn triu Mg
o tan 1,010g magnesi sulfat trong nc va 100 ml c dung

dch magnesi sulfat 1,010%.
Pha long 1 th tch dung dch magnesi sulfat 1,010% thnh 10 th

tch vi nc ngay trc khi s dng.
2.8. Dung dch nhm mu 200 phn triu Al
Ho tan 0,352g nhm kali sulfat (Phn chua) trong dung dch acid
sulfuric 0,1 M va 100 ml.
2.9. Dung dch nickel mu 1000 phn triu Ni
o tan 0,478g nickel ( ) sulfat trong nc va 100 ml.
2.10. Dung dch nitrat mu 1000 phn triu NO3
Ho tan 0,163g kali nitrat vi nc va 100 ml.
2.11. Dung dch nitrit mu 20 phn triu NO2
o tan 0,600g natri nitrit vi nc va 100 ml. Pha long 1 ml

dung dch ny thnh 200 ml vi nc.
2.12. Dung dch phosphat mu 500 phn triu PO4
Ho tan 0,0716g kali dihydrophosphat trong nc va thnh 100

ml.
2.13. Dung dch st mu 200 phn triu Fe
43
o tan 0,863g st amoni sulfat (phn st amoni) trong nc c

cha 25 ml dung dch acid sulfuric 1 M v thm nc va 500 ml.
2.14. Dung dch sulfat mu 1000 phn triu SO4
o tan 0,181g kali sulfat trong nc va 100 ml.
2.15. Dung dch sulfat mu 1000 phn triu SO4 trong ethanol
o tan 0,181g kali sulfat trong ethanol 30% va 100 ml.
3. HO CHT, THUC TH CH TH
lc 2.8 trnh by nhng ho

cht - thuc th v Ph lc 2.10 trnh by cc ch th dng trong kim
nghim thuc. i liu ny trnh by mt s thuc th v ch th hay dng
trong thc tp kim nghim thuc ca chng trnh.
3.1. Ho cht
3.1.1. Acid acetic bng
Acid acetic kt tinh c.
Cng thc ho hc: C 3C . Phn t lng 60,1.
Dng loi tinh khit phn tch.
Acid acetic bng l cht lng khng mu, mi hng cay. Khi lng
ring: Khong 1,05g/ ml. im ng c: Khong 16oC. m lng
CH3COOH: Khng c nh hn 98,0% (KL/KL).
* Acid acetic long (Dung dch acid acetic 12% - Dung dch acid
acetic 2 M): Pha long 11,43 ml acid acetic bng vi nc va 100
ml. m lng C 3C khong 11,5 12,5%.
* Acid acetic xM: Pha long 57x ( ml) (60x (g)) acid acetid bng vi
nc va 1000 ml.
3.1.2. Acid hydrocloric
Acid hydrocloric m c.
Cng thc ho hc: Cl. Phn t lng 36,46.
Acid hydrocloric m c l cht lng trong, khng mu, bc khi.

trng 20oC: Khong 1,18. m lng Cl: 35 38% (KL/KL), khong
44
11,5 M. Bo qun nhit khng qu 30 oC, trong bao b bng

polyethylen hoc vt liu khng phn ng vi acid hydrocloric.
* Dung dch acid hydrocloric 10%: Pha long 24 ml acid hydrocloric

m c vi nc va 100 ml.
* Dung dch acid hydrocloric long: Pha long 17 ml acid hydrocloric

* Dung dch acid hydrocloric xM (xN): Pha long 85x ( ml) acid
hydrocloric m c vi nc va 1000 ml.
3.1.3. Acid nitric
Acid nitric m c.
Cng thc ho hc: 3. Phn t lng 63,01.
HNO3 l cht lng bc khi, n mn, c nng mol khong 16 M.

Khi lng ring: Khong 1,42g/ ml. m lng 3: Khong 70%
(KL/KL). Bo qun trnh nh sng.
* Dung dch acid nitric long: Pha long 14,09 ml (20g) acid nitric
* Dung dch acid nitric xM: Pha long 63x ( ml) acid nitric m c vi
nc va 1000 ml.
3.1.4. Natri hydroxyd
Cng thc ho hc: a . Phn t lng 40,00.
Dng loi tinh khit phn tch c cha hm lng kim ton phn
khng nh hn 97% tnh theo a v khng c c qu 2,0%
Na2CO3. atri hydroxyd c dng cc trng hay thi hnh tr, d ht m.
Bo qun trong ng kn.
* Dung dch natri hydroxyd xM (xN): Ho tan 40x (g) natri hydroxyd
trong nc v thm nc va 1000 ml.
* Dung dch natri hydroxyd long: Ho tan 8,5g natri hydroxyd trong
nc v thm nc va 100 ml.
3.2. Thuc th
3.2.1. Thuc th Nessler
45
Ho tan 10g kali iodid trong 10 ml nc v thm tng t mt, va cho

va khuy u, dung dch bo ho thu ngn diclorid cho ti khi xut
hin ta bn. hm 30g kali hydroxyd, sau khi tan ht li thm 1 ml
dung dch bo ho thu ngn diclorid. Pha long vi nc va 200
ml. yn v gn ly phn nc trong.
h nhy: Cho 3 git thuc th essler vo 10 ml dung dch

amoni mu 2 phn triu 4, mu vng cam phi xut hin ngay lp tc.
Bo qun trong l thu tinh mu da cam, c nt mi, trnh nh

sng.
3.2.2. Giy tm ch acetat
hng giy lc trng vo hn hp gm 10 th tch dung dch ch

acetat 9,5%* v 1 th tch dung dch acid acetic 2M, ro ri hong kh,
trnh nh sng. ni khng c acid hay kim. Ct thnh tng bng
di khong 5cm, rng 6mm.
Bo qun trong l thu tinh nt mi, trnh nh sng.
Dung dch ch acetat 9,5%*: o tan 9,5g ch acetat trong nc va

100 ml khng c carbon dioxyd.
3.2.3. Dung dch thic (II) clorid AsT
un nng 20g thic vi 85 ml dung dch acid hydrocloric c n khi

khng cn kh hydro bay ra. Pha long gp i dung dch ny bng acid
hydrocloric c. Bc hi dung dch trn n khi thu c th tch ban
u v lc qua giy mn.
3.2.4. Dung dch kali iodid 10% (Dung dch kali iodid long)
o tan 10g kali iodid trong nc mi un si ngui va 100

ml. Dung dch khng c c mu.
Bo qun trong l thu tinh mu, nt mi, trnh nh sng.
3.2.5. Dung dch bc nitrat 2%
o tan 2g bc nitrat trong nc v thm nc va 100 ml.
3.2.6. Dung dch thioacetamid
Ho tan 4g thioacetamid trong nc va 100 ml. Thm 1 ml hn

hp ca 15 ml dung dch natri hydroxyd 1 , 5 ml nc v 20 ml glycerin
85% vo 0,2 ml dung dch trn. un nng trong cch thu 20 giy, lm
lnh v dng ngay.
46
3.2.7. Dung dch bari clorid 25%
Ho tan 25g bari clorid trong nc v cho thm nc va 100 ml.
3.2.8. Thuc th Streng (magnesi uranyl acetat)
un nng cch thu 3,2g uranyl acetat, 10g magnesi acetat, 2 ml

acid acetic bng v khong 30 ml nc. Sau khi tan ht ngui. hm
50 ml ethanol v nc va 100 ml. yn 24 gi ri lc.
3.2.9. Dung dch natri sulfid 2%
o tan 2g natri sulfid trong nc, thm 2 3 git glycerin v pha

long vi nc va 100 ml.
Bo qun trong l nh, y, nt kn, ch mt, trnh nh

sng.
3.2.10. Dung dch st (III) clorid 5%
o tan 5g st ( ) clorid trong nc va 100 ml.
3.3. Mt s ch th mu
3.3.1. Da cam methyl
Bt kt tinh mu da cam, i khi c nh nu. Kh tan trong nc, d

tan trong nc nng, khng tan trong ethanol.
Vng chuyn mu: p 3,0 () n p 4,4 (vng).
Dung dch ch th da cam methyl: o tan 0,1g da cam methyl trong

80 ml nc v thm ethanol 96% va 100 ml.
3.3.2. en eriocrom T
Bt mu en hi nu c ng nh kim loi, t tan trong nc lnh. an

trong ethanol v methanol. rong mi trng kim (p 9,5 -10,0), dung
dch en eriocrom c mu xanh, cn phc cht ca ch th vi ion calci,
magnesi, km trong iu kin thch hp c mu tm . Khi chun
nhng cation trn bng rilon B vi ch th ny, mu chuyn t tm
sang xanh.
Ch th en eriocrom hay c chun b dng rn: trn u 1

phn en eriocrom vi 200 phn natri clorid c lm mn trc.
3.3.3. methyl
47
inh th ng nh hay bt kt tinh mu nu. n nh khng tan

trong nc, kh tan trong ethanol, tan trong cc dung dch kim v
carbonat kim.
Vng chuyn mu: p 4,4 () n p 6,0 (vng).
Dung dch ch th methyl: o tan 50mg methyl trong mt hn

hp ca 1,86 ml dung dch natri hydroxyd 0,1 v 50 ml ethanol 96%.
Sau khi tan ht, thm nc va 100 ml.
3.3.4. phenol
Bt mu . Kh tan trong nc, ethanol v aceton, d tan trong

kim v carbonat kim.
Vng chuyn mu: p 6,8 (vng) n p 8,4 ().
Dung dch ch th phenol: o tan 0,1g phenol vi 2,82 ml dung

dch natri hydroxyd 0,1 v 20 ml ethanol 96%. Sau khi tan ht, thm
nc va 100 ml.
3.3.5. Kali cromat
inh th mu vng, d tan trong nc, khng tan trong ethanol.

rong mi trng trung tnh, tc dng vi bc nitrat cho ta .
Dung dch ch th kali cromat: o tan 5g kali cromat trong nc v

thm nc va 100 ml.
Khi dng, c 100 ml dung dch lc cui chun , cho 1 - 2 ml dung

dch ch th.
3.3.6. Phenolphtalein
Bt kt tinh trng hay vng nht, khng tan trong nc, tan trong
ethanol. Vng chuyn mu: p 8,2 (khng mu) n p 10,0 ().
Dung dch ch th phenolphtalein: o tan 0,1g phenolphtalein trong

80 ml ethanol 96% v thm nc va 100 ml.
3.3.7. Tinh bt
Bt rt mn, khng mi, khng v.
Ch th h tinh bt: ghin 1g h tinh bt trong ci vi 5 ml nc cho

ti khi thnh mt hn hp ng nht ri va va khuy vo 100 ml
nc si. un si tip 2 - 3 pht cho ti khi thu c mt cht lng ch
hi c.
48
Dung dch ch pha dng trong 2 - 3 ngy. Mun dng c lu

hn phi thm 10mg thu ngn ( ) iodid.
T LNG GI V BI TP
1. Cht i chiu c dng lm g v trong cc php th no?
2. rnh by cch pha dung dch chun t cht gc. Cho v d.
3. rnh by cch pha dung dch chun gn ng ri chun ho

bng cht gc. Cho v d.
4. rnh by cch pha dung dch chun bng cch pha long
nhng dung dch chun c nng cao. Cch pha ny
thng dng trong trng hp no? Cho v d.
5. rnh by cch pha dung dch ion mu:
a) Amoni mu 100 phn triu H4.
b) Arsen mu 1000 phn triu As.
c) Clorid mu 500 phn triu Cl.
d) Ch mu 1000 phn triu Pb.
e) St mu 200 phn triu Fe.
f) Sulfat mu 1000 phn triu S 4.
6. rnh by cch chun b cc ch th:
a) Da cam methyl. b) en eriocrom .
c) phenol. d) Kali cromat.
e) Phenolphtalein. f) tinh bt.
7. nh h s hiu chnh K ca dung dch a2S2O3 0,1 khi chun

bng cht chun gc K2Cr2O7 c T = 0,004904g/ ml c tin
hnh nh sau: Cn chnh xc 0,1518g K2Cr2O7 ho tan trong
khong 50 ml nc ct trong mt bnh nn nt mi, thm 10 ml
dung dch K 20%, 5 ml dung dch Cl c. y nt v yn
ch ti 10 pht. hm 200 ml nc v chun bng dung dch
Na2S2O3 0,1 vi ch th l dung dch h tinh bt ht 29,15 ml
dung dch a2S2O3.
8. nh h s hiu chnh K ca dung dch iod 0,1 khi chun

bng dung dch a2S2O3 0,1 c K = 1,0082. Bit rng chun
49
10,00 ml dung dch iod trn vi ch th h tinh bt ht 10,76 ml

dung dch a2S2O3.
9. rnh by cch pha dung dch acid hydrocloric 10%.
10. rnh by cch pha v xc nh nng ca dung dch natri

hydroxyd 0,1N.
11. rnh by cch pha dung dch acid acetic long.
12. rnh by cch pha dung dch acid nitric 2M.
13. in t hoc cm t cn thiu vo ch trng trong cu sau:
a) Ch th da cam methyl trong dung dch c p < 3 c

mu.......A..... v trong dung dch c p > 4,4 c mu.....B........
b) Ch th methyl trong dung dch c p < 4,4 c mu.....A.......

v trong dung dch c p > 6,0 c mu.......B.......
c) Ch th phenol trong dung dch c p < 6,8 c mu.......A.....

v trong dung dch c p > 8,4 c mu.....B........
d) Ch th phenolphtalein trong dung dch c p < 8,2 c

mu.......A..... v trong dung dch c p > 10 c mu........B.....
Chn cu tr li ng cho cc cu hi t 14 v 15 bng cch khoanh

14. Vng chuyn mu ca ch th:
a) Da cam methyl trong khong p t:
A. 3,0 - 4,4 B. 3,5 4,5 C. 2,8 3,5 D.

5,0 6,1
b) methyl trong khong p t:
A. 3,0 - 4,4 B. 4,4 6,0 C. 4,8 5,5 D.

5,6 6,3
c) Phenolphtalein trong khong p t:
A. 4,0 - 5,4 B. 3,5 4,5 C. 6,5 7,8 D.

8,2 10,0
15. pha dung dch:
a) Acid acetic 1M ngi ta:
50
A. Pha long 5,7 ml dung dch acid acetid bng vi nc va

100 ml.
B. Pha long 6,0 ml dung dch acid acetid bng vi nc va

100 ml.
C. Pha long 12,5 ml dung dch acid acetid bng vi nc

va 200 ml.
D. Pha long 6,2 ml dung dch acid acetid bng vi nc va

100 ml.
b) pha dung dch acid hydrocloric 10% ngi ta:
A. Pha long 28 ml acid hydrocloric m c vi nc va

100 ml.
B. Pha long 20 ml acid hydrocloric m c vi nc va

100 ml.
C. Pha long 60 ml acid hydrocloric m c vi nc va

200 ml.
D. Pha long 24 ml acid hydrocloric m c vi nc va

100 ml.
16. Trnh by cch pha dung dch thuc th essler, dung dch thic
( ) clorid As , dung dch kali iodid 10%, dung dch thioacetamid,
thuc th Streng v dung dch natri sulfid 2%.
51
Bi 5
MT S PHNG PHP PHN TCH
HO L DNG TRONG KIM NGHIM
MC TIU
- Trnh by c khi nim chung v phng php tch v sc k,

ng dng sc k lp mng trong kim nghim.
- Trnh by c nguyn tc ca phng php o th, ng dng o

pH v chun o th.
- Trnh by c nguyn l c bn ca phng php o quang ph

hp th UV-VIS v ng dng nh tnh, nh lng.
1. CC PHNG PHP TCH
1.1. Khi nim
Cc phng php tch (cc phng php phn chia) l nhm cc

phng php vt l, ho hc, ho l nhm a mt hn hp phc tp
gm nhiu cht thnh cc hn hp n gin hn v t tch ring ra
tng cht (hoc nhm cht).
Hn hp cn tch c th l ng nht (mt pha), v d c nhiu

cht cng c trong mt dung dch (pha lng). n hp cn tch c th l
khng ng nht (t nht c hai pha khng trn ln vi nhau: nu hn
hp gm hai pha lng gi l nh dch, nu hn hp gm pha lng v rn
gi l hn dch).
u theo hn hp cn tch l ng nht hay khng ng nht m la

chn cc phng php tch thch hp.
1.2. Cc phng php tch thng dng
1.2.1. Phng php lc
php n gin, nhng hiu qu.
- K thut lc: C th lc p sut thng hoc lc p sut gim

(lc chn khng). Vt liu thng dng l giy, bng thu tinh, phu lc
thu tinh xp,...
1.2.2. Phng php ly tm
52
L phng php dng lc ly tm lm lng kt ta xung. c

lng ph thuc vo lc ly tm.
1.2.3. Phng php chia ct pha
- C th thc hin bng cch: chn lc c hc (da vo hnh dng,

kch thc, mu sc,... tch cc cht), lng i (dng dng cht lng
chy qua li i cc ht nh), loi bt dung mi bng cch c c hay bay
hi,...
1.2.4. Phng php chit
tch ly mt cht (hay mt nhm cht) t mt hn hp nghin cu trong

dung mi A. C s ca phng php l da trn s phn b ca cht
tan gia 2 pha A v B khng ho ln vo nhau. i lng c trng l
h s phn b Kp.
rong : CB: l nng cht tan trong dung mi B; CA: l nng

cht tan trong dung mi A.
th Kp l hng s.
lng - lng hoc chit lng - rn.
a) Chit lng - lng
C 3 cch:
- Chit n: Chit mt ln, trong phng th nghim chit bng bnh

gn, lc tay hoc my. iu sut chit thp.
- Chit lp (chit nhiu ln): Sau ln chit 1, trong dung dch cn cht
tan, thm dung mi mi chit tip. u cng mt lng dung mi ta chit
nhiu ln tt hn chit t ln.
Chit nhiu ln tn thi gian, thng chn ti u 3 ln.
rong phng th nghim c th chit gin on hoc lin tc. rong

cch chit lin tc, dch chit c un si lin tc dung mi bay hi,
ta thu hi cho chy lin tc vo bnh ng dung dch cn chit (nh vy
53
tit kim c dung mi nhng c nhc im do lin tc un si d

lm phn hu cht cn tch).
- Chit ngc dng: Cho dung mi v dung dch cn chit i ngc

chiu nhau, hai pha tip xc cht ch, pha trn v di chuyn ngc
chiu nhau. y l mt qu trnh lin tc.
rong kim nghim chit lng - lng c ng dng rt nhiu v

thng dng mt pha l nc v mt pha l dung mi hu c.
b) Chit lng - rn
hng c 2 cch:
- Dng pha rn (nh Al2O3, nhm silicat, than,...) chit ly cc

cht t mt pha lng, ch yu nh s hp ph.
- Dng pha lng (dung mi hoc cc h dung mi) chit ly cc

cht t mu phn tch l cht rn (nh bt, dc liu, cn kh ca mu
th,...). V d chit hot cht t bt dc liu bng dng c chit
Soxhlet.
2. PHNG PHP SC K
2.1. Khi nim v phng php sc k
m 1903, nh thc hc ngi ga M.S. svet khi cho dch chit

clorophyl t l cy qua ct CaC 3, sau cho ether du ho chy qua
thy cc sc t ca clorophyl c tch ring thnh nhng lp mu khc
nhau trn ct (khng mu, vng, lc vng, lc lam, vng, xm). Ct vi
h thng cc lp mu tch, ng t tn l sc (hay sc k ) v
k thut tch ny ng gi l phng php sc k.
gy nay c th ni sc k l phng php tch cc cht da vo

s phn b khc nhau ca chng 2 pha khng ho ln vo nhau v
lun tip xc vi nhau, mt pha ng yn gi l pha tnh (Stationnary
phase: SP) v mt pha di chuyn gi l pha ng (Mobile phase: MP).
rong qu trnh pha ng chuyn ng dc theo h sc k ht lp pha
tnh ny n lp pha tnh khc s lp i lp li qu trnh hp ph v phn
hp ph. qu l cc cht b hp ph nhiu (c i lc ln) vi pha tnh
s di chuyn chm hn cc cht b hp ph t (c i lc yu) v chng c
th tch ra khi nhau.
2.2. Phn loi cc phng php sc k
ng c th l lng hoc kh, pha

tnh c th l lng hoc rn. Da vo trng thi tp hp ca pha ng
ngi ta chia sc k thnh 2 nhm ln: sc k kh v sc k lng. Da
vo c ch trao i ca cc cht gia pha ng v pha tnh, hoc cch
54
b tr pha tnh ngi ta li chia cc phng php sc k thnh nhm nh

hn. Cc dng sc k c bn c minh ho bng 3.
Bng 3. Cc dng sc k c bn
Cch b tr C ch tch
Dng sc kh Pha ng Pha tnh
pha tnh ca cc cht
Kh - p ph Kh n Ct p ph
Kh - lng Kh Lng Ct Phn b
Lng - n Lng n Ct p ph
Lng - Lng Lng Lng Ct Phn b
Lng - ha trao Lng n Ct rao i ion

i
Lp mng Lng n Lp mng p ph
iy Lng n iy sc k Phn b
y (sc k el) Lng Lng Ct Theo kch thc
phn t
- Qu trnh sc k thng gm 3 giai on chnh: a mu th ln

pha tnh, cho pha ng chy qua pha tnh, pht hin cc cht v x l
kt qu.
2.3. Mt s phng php sc k
2.3.1. Sc k lp mng
a) Khi nim
c k lng - rn, trong pha tnh rn (l

cht hp ph c chn ph hp theo yu cu phn tch) c tri
thnh lp mng ng u trn bn knh, nha hay kim loi. Sau a
hn hp cht cn tch ln pha tnh bng cch chm dung dch mu
nghin cu ln bn mng (cch ra bn mng 2 - 3cm). Pha ng l mt
h dung mi n hoc a thnh phn c trn vi nhau theo mt t l
nht nh (cho dung mi pha ng chy bng cch t bn mng vo h
dung mi ny theo hng phn c vt chm di). Di tc dng ca
lc mao qun, dung mi s chuyn ng qua lp hp ph, cc cu t s
di chuyn theo hng pha ng nhng vi vn tc khc nhau a n
vic tch cc cu t ra khi nhau, ta thu c mt sc k trn lp
mng.
55
g nh tnh, th
tinh khit, cng c th nh lng. u im c bn l thit b n
gin, thi gian phn tch nhanh, kh chn lc.
b) i lng c trng
h s lu gi f (Retard factor)
khng lp li do ph thuc
f
nhiu yu t kh kim sot nh: cht lng v hot tnh ca cht hp
ph, m ca cht hp ph, cht lng ca dung mi,... Do ngi
ta thng dng h s lu gi tng i td.
rong c l khong cch t im xut pht n tm ca vt sc k

cht c chn lm chun i chiu c sc k trong cng iu kin
v trn cng bn mng vi mu th.
S ( nh gi kh
nng tch cc cht):
rong :
dA, dB: l khong cch t im xut pht n tm ca vt sc k ca cht

A v cht B trn sc (A v B l 2 cht trong cng hn hp, d B> dA).
DA, DB l ng knh ca vt sc k ca cht A v B trn sc .
Yu cu: S > 1, gi tr ti u S = 1,5.
c) Thit b, ho cht chnh
polyamid, sephadex,... Cht hp ph c th c tri di dng nho c

cht kt dnh thnh bn mng dnh chc, hoc dng bt mn khng c
cht kt dnh thnh bn mng khng dnh chc. in nay, trong thc t
c bn mng trng sn nh Silicagel , Silicagel F254, Silicagel HF254.
56
t ca
cht nghin cu. Dung mi c th l n hoc hn hp. Cc dung mi
phi t tinh khit cao.
ph hp v c np y kn.
micropipet hay ng mao qun thng, ng mao qun nh mc chnh

xc.
quang t ngoi, my o mt vt.
d) Cc bc tin hnh
ph hp vi yu cu phn tch, iu ch va ca cht hp ph, tri bn

mng, lm kh t nhin, hot ho bn mng 105 oC 110oC.
kh trong bnh bng cch lt giy lc xung quanh thnh trong ca bnh,
pha dung mi (lng dung mi s dng sao cho sau khi thm u vo
giy lc, cn li 1 lp dy 5 10mm y bnh). y np bnh v yn
1 gi.
mu khng qu nh v khng qu ln (thng thng 0,1 -

tch 0,001 - 0,005 ml). im chm xut pht phi cch mp di bn
mng 1,5 - 2,5cm v cch b mt dung mi 0,8 - 1,0cm. Vt chm phi
nh gn (ng knh 2 6mm), cc vt chm cch nhau 15mm, vt
chm cch b bn ca bn mng t nht 1cm.
k (cc vt chm phi trn b mt ca lp dung mi). y kn bnh v

yn nhit c nh. hng khi ng i ca dung mi c 10 -
12cm th kt thc giai on trin khai sc k.
Lm bay hi dung mi cn ng li trn bn mng. Pht hin vt sc k

bng phng php ho hc hoc ho l (hin mu bng phun thuc th
hoc dng n UV 254nm v 366nm). Quan st mu vt, o v tnh f
(hoc td, RS).
kt qu trn rt ra kt lun v nh tnh, th tinh khit theo yu

cu ca php phn tch. nh lng c th da trn din tch, m
mu ca cc vt hoc x l bng cc bin php ho hc thch hp ly
cht nghin cu ra khi bn mng.
57
V d: ch hn hp Morphin, papaverin (hoc codein) bng sc k

lp mng.
+ Bnh chy sc k.
+ ng ong, ci chy s, tha s.
+ ng mao qun.
+ Bnh ng iod lm hin mu.
+ Dung dch chun morphin 0,5%.
+ Dung dch chun papaverin 0,5%.
+ Dung dch hn hp morphin v papaverin (dung dch bi tp).
+ Cloroform, aceton, methanol, amoniac c, iod tinh th, silicagen,

thch cao.
+ Lm lp mng dnh chc: cn 2,5g silicagen v 0,3g thch cao, cho

vo ci s nghin mn (cho thch cao trc, sau thm dn silicagen).
Sau , cho dn dn 7 ml nc ct trn u, trnh c bt kh (tt c qu
trnh cho nc v trn phi lm nhanh trong vng 1 - 2 pht). t 2
phin knh nh ln mt phin knh to hn ( bi t nc cho dnh cht
vo ). ay tri cm knh to, dng mt que nh qun bng tm hn hp
bt nho qut nh ln xung quanh mp cc phin knh nh, sau dng
tha hn hp bt nho ln, nghing knh cho lp bt dn u. yn
cc phin knh tri bt nho trong khng kh hoc trn mt bp nng
chng 15 pht ri cho vo t sy (sy 105 oC trong 1 gi).
+ Pha dung mi: Pha hn hp dung mi: cloroform-

,5: 1. Sau cho vo bnh
sc k ( lt mt khoanh giy lc xung quanh dung mi chng bo
ho v lt y bng mt ming giy lc trn), y np, yn mt lt.
+ Chy sc k: Ly phin knh t sy ra, ngui, gt bt hai

bn mp, chm dung dch chun morphin, papaverin, dung dch hn hp
ln phin knh (ch khng lm thng lp bt v chm git nh nhiu
ln). Dng phin knh chm dung dch vo bnh chy sc k, cho
dung mi chy mt on khong 12 15cm ly phin knh ra, sy n
ht mi amoniac.
58
+ Pht hin: t bn mng vo bnh c cha sn mt t tinh th iod

khong 5 pht. Ly ra, cc vt alcaloid s c mu vng nu. o, tnh,
xc nh f v cho bit trong hn hp c morphin v papaverin khng.
+ Yu cu sc thu c r, o v tnh c f, nh tnh ng.
2.3.2. Sc k trao i ion
- rn. y pha tnh l

mt cht c kh nng trao i ion (cation v anion). Qu trnh sc k xy
ra da vo phn ng trao i ion gia cc thnh phn trong pha ng v
cht trao i ion np sn trong ct sc k. Cht trao i ion thng dng
l cc cht tng hp c gi l nha trao i ion hay ionid (ionid c kh
nng trao i cation gi l cationid, ionid c kh nng trao i anion gi
l anionid).
hng trnh trao i gia ion ionid v ion trong pha ng c th

biu th nh sau:
+ Vi cationid:
+ Vi anionid:
h vy sau qu trnh sc k, chng ta c th ti sinh nha tr v

trng thi ban u (bng cch cho cationid tip xc vi dung dch acid c
nng thch hp, anionid tip xc vi dung dch base c nng thch
hp).
phng th nghim, ct trao i ion thng l ct thu tinh hnh tr, y c

lp kho thot dung dch, di y thng lt bng thu tinh ngn
khng cho cc ht nha lt vo lm tc kho. rong ct tu theo php
phn tch m nhi cationit hoc anionit. Sau , cho dung dch cn phn
tch chy qua (pha ng) phn ng trao i gia ion trong ionid v ion
cn xc nh s xy ra.
n c ng dng tch cc ion, nh lng cc

cht, lm sch cc ion trong nc,...
thch hp, nhng thng ch chn loi nha c dung lng trao i
ln, bn vng ho hc, c trng nc xc nh, c kch thc ng
nht,... Khi tin hnh sc k khng bao gi c nha kh hoc c
bt kh.
59
V d: nh lng a2SO4 bng phng php sc k trao i ion
- Nguyn tc:
Da trn phn ng trao i thun nghch gia cc ion trong dung

dch cht nghin cu vi cc ion trong mt cht gi l ionid. Qu trnh
trao i tun theo nh lut tc dng khi lng.
i vi a2SO4, khi cho dung dch chy qua ct trao i ion (cha
cationid dng +) trong ct s xy ra phn ng:
2RH + Na2SO4 = 2RNa + H2SO4
Dung dch chy t ct ra l 2SO4, em nh lng dung dch 2SO4

ny bng dung dch a bit nng , suy ra c hm lng
Na2SO4 c trong mu phn tch.
- Dng c, ho cht:
+ Ct trao i ion (dng Buret).
+ ng nghim nh.
+ Cationid (loi trao i acid mnh).
+ Dung dch Cl 0,1 .
+ Ch th da cam methyl.
+ Dung dch chun a 0,1 .
- Cch tin hnh:
+ Chun b ct trao i ion: Ly khong 10 - 15g cationid (loi acid

mnh) ngm trong Cl 0,1 trong 2 ngy ( cationid dng ). Sau
cho vo ct trao i ion (dng buret c lt di mt t bng thu
tinh). Ch khng bt kh ln vo, phi lun lun cho dung dch ngp
trn cationid t nht 0,5cm trong qu trnh chy sc k cng nh khng
chy. Cho chy thm t t 20 ml Cl 0,1 na cationid hon ton
dng acid . a ct bng nc ct cho n khi nc chy ra khng
cn acid t do (th bng ch th da cam methyl).
+ Cho chy sc k: Cn chnh xc (hoc ly th tch chnh xc) mu

cn phn tch (sao cho lng a 2SO4 cha trong mu khong 0,1g) cho
vo cc, pha long hoc ho tan vi khong 20 ml nc, khuy cho tan,
cho chy qua ct trao i ion vi tc 5 - 10 git trong 1 pht. a cc
bng nc ct v cho chy qua ct tip. a ct tip bng nc ct n
khi nc chy ra khng c acid (th vi ch th da cam methyl). ng tt
c dung dch trao i v nc ra vo bnh nn to.
60
+ Chun : hm vi git ch th da cam methyl vo bnh nn ri

em chun bng dung dch a (c nng chnh xc khong
0,1 ) n khi mu chuyn t sang vng. hi th tch dung dch
NaOH. Tnh% Na2SO4 trong mu. Bit a2SO4 c M = 142.
+ i phc li ionid: Sau khi lm xong, cho dung dch Cl 0,1 chy
qua ionid v ngm cationid.
3. PHNG PHP QUANG PH HP TH T NGOI - KH KIN
L phng php phn tch xc nh cc cht da trn c s s hp

th cc bc x in t vng t ngoi (UV) v kh kin (V S) ca cc
phn t cht nghin cu.
3.1. nh sng v mu sc
(kh kin), hng ngoi ( ),... c c im va mang tnh cht sng v

va mang tnh cht ht.
-von (k hiu l
eV) hoc kC/mol (1eV = 23 kCal/mol).
- n s nh sng l s dao ng hon chnh m sng thc hin

c trong 1 giy.
C l vn tc ca nh sng (trong chn khng C = 3.1010cm/s).
Hnh 3. S mt dao ng sng hon chnh
10-9 m).
phn tch min sng quang hc (hay c ng dng) gm 3 vng:
Vng t ngoi: 185 400nm
61
Vng kh kin: 400 760nm
Vng hng ngoi: 700
tia c bc sng gn nhau:
: 760 630nm.
Cam: 630 600nm.
Vng: 600 570nm.
Lc: 570 500nm.
Lam: 500 450nm.
Chm: 450 430nm.
Tm: 430 400nm.
h vy, nh sng t nhin l nh sng a sc. rong thc t, nh

sng t nhin l nh sng trng (khng mu) v cc tia sng ph nhau
tng i mt (ngha l mi bc sng u c mt bc sng ph ho
ho thnh nh sng trng) gi l cc cp mu ph nhau (hay b sung
nhau).
V d: Cp mu ph nhau:
xanh lc.
Da cam lc xanh.
Vng xanh (lam).
Lc vng tm.
Lc - ta.
hp th c chn lc ngha l c tia b hp th nhiu, c tia b hp th t,

do phn nh sng phn x p vo mt ngi quan st l tia ph vi
tia b hp th v cho ta cm thy mu ca tia . V d nu vt hp
th tia sng mu vng ta thy vt c mu xanh lam. V vy ta ni mu
ca vt v mu m vt hp th l hai mu ph nhau.
hm tia sng n sc l chm tia sng c bc sng bng nhau

(c mt bc sng duy nht).
62
3.2. nh lut c bn v s hp th nh sng (nh lut Lambert-

Beer)
3.2.1. nh lut
Chiu mt chm tia sng n sc c cng l o qua mt dung

dch c chiu dy l (cm), nng C. Sau khi b hp th, cng chm
tia cn li l .
Hnh 4. S nh sng truyn qua dung dch
ng):
vi K l h s hp th.
c gi l h s
= D khi C = 1mol/l v l = 1cm) c trng cho bn
cht ca cht nghin cu trong dung dch ch ph thuc vo bc sng
nh sng n sc.
+ u C tnh theo % (KL/ ) ta c: D = E1%1cm.C.l v E1%1cm l h s

hp th ring (h s tt ring).
truyn qua thp, mt quang cao v ngc li.
3.2.2. iu kin p dng nh lut
- nh sng phi n sc.
63
- Cc yu t ho hc khc: p , cc cht l,... khng c nh hng
3.3. Quang ph hp th v ng dng
3.3.1. Quang ph hp th UV-VIS
ng biu din s ph thuc ca mt quang D (hoc h s
hp th nh sng cc bc sng khc nhau ca cht nghin cu. rn

quang ph hp th tu tng cht n c th c mt hoc nhiu cc i
max
Hnh 5. Ph hp th UV VIS ca vitamin B12
3.3.2. ng dng
-
V S l nhng thng tin v cu trc ca cht phn tch do c th dng
nh tnh nhn bit cc cht. V d dung dch vitamin B 2 (Riboflavin) c 4
cc i hp th l 223nm, 267nm, 373nm v 444nm.
tinh khit hoc s phn hu ca cht phn tch. V d vi B2 ta lun c:
64
nh lut Lambert - Beer nh lng cc cht.
V d: nh tnh, nh lng vitamin B12 bng phng php quang

ph hp th UV-VIS.
- Nguyn tc:
Da trn vic o ph hp th t ngoi v kh kin ca cht . Ph

hp th l th biu din gia mt quang ( hp th) ca dung dch
cht nghin cu vo bc sng ca tia sng n sc. hit lp ph hp
th bng cch o mt quang ca mt dung dch c nng xc nh
vi cc bc x c di sng gim hoc tng dn, sau v th biu
din s ph thuc ca D -
nghin cu. rn ph hp th s nhn thy cc cc i hp th (ng vi
bc sng, s hp th l cc i) v cc cc tiu nu c. Cc cht
khc nhau thng c ph hp th khc nhau. Do vy thng dng ph
hp th nh tnh cc cht hoc th tinh khit cc cht cn c vo
dng ph, cc cc i v cc cc tiu hp th, t l cng hp th
ca cc cc i hoc ca cc cc tiu hp th.
Vi vitamin B12 dung dch 0,0025% trong nc c 3 cc i hp th:

361 1nm v 550 2nm, 278nm 1nm; t s hp th 361nm vi
hp th 278nm l 1,70 n 1,90; t s hp th 361nm vi
hp th 550nm l 3,15 n 3,45.
- Dng c, ho cht:
+ My quang ph UV-VIS.
+ Bnh nh mc dung tch 10, 25, 50, 100 ml.
+ Cc pipet chnh xc.
+ Cc c m.
+ Dung dch tim B12 ml.
- Tin hnh:
Pha long dung dch tim vitamin B12 c nng khong 0,0025%
ml). Qut ph hp th ca dung dch cc bc sng t 200nm
n 650nm, dng cuvet thch anh c b dy 1cm, mu trng l nc
ct.
+ m cc cc i hp th. i chiu vi l thuyt kt lun.
65
+ C th lm song song mt php o vi dung dch vitamin B12

chun (0,0025%) ta c ph chun. Khi hai ph phi c cng hnh
dng v cc cc i cc bc sng trng nhau.
3.3.3. Mt s iu kin khi p dng
max
trn quang ph l tt nht v khi l cc i hp th D max, php o nhy
mc sai s o nh hn so vi cc bc sng khc.
- 0,80; tt nht D = 0,43.
t - Beer.
ngi, cho phn ng ph,... (V d, ampicilin hp th rt yu vng UV,

nhng nu cho phn ng thu phn sau tc dng vi Cu2+ s c
sn phm hp th mnh 320nm).
in nay vi k thut mi hin i hn, vng o ti u ca mt

quang c m rng hn v thng ghi trong catalog ca my ca tng
nh sn xut.
3.4. Cc b phn c bn ca my o quang ph UV-VIS
Cc my c nhiu loi v cu to khc nhau, song u c mt s

chung:
Hnh 6. S cu to ca my quang ph UV-VIS
3.4.1. Ngun sng

760nm, nu dng n halogen (c cha hi 2, Br2 bn trong) c th ko
di thang sng pht x ti 1000nm.
2 hay n D2 (deuterium).
3.4.2. B n sc ho
him v ch yu l to ra tia n sc.
- u my dng knh lc mu, knh tt nht cng ch c th t c

mc n sc 10nm.
66
- u my dng lng knh hoc cch t c kh nng to ra nh sng

gn nh n sc ( 1nm).
3.4.3. Mu o
ng dung dch o bng cuvet. C nhiu loi cuvet chiu dy khc

nhau. u o vng UV phi dng cuvet thch anh, nu o vng V S
c th dng cuvet thch anh, thu tinh, nha. Khi dng cuvet lu khng
c cm tay hoc lm try xc vo phn trong sut ca cuvet.
3.4.4. Detect
L tn gi chung ca mt loi thit b tip nhn thng tin di dng

mt tn hiu no (nh quang, nhit,...) ri chuyn ho thnh mt tn
hiu tng ng gip ngi s dng nhn ra.
rong my o quang ph UV-V S, detect ch yu l t bo quang

in chuyn cng nh sng thnh dng quang in. bo
quang in c nhiu loi, c th l t bo chn khng, bn dn hoc ng
nhn quang.
bo quang in c hin tng mt mi, nhy gim khi phi

lm vic lin tc nn lu khng c chiu nh sng lin tc vo t
bo quang in.
3.4.5. B khuch i
him v chnh l khuch i tn hiu cho mnh ln trc khi a

vo b phn ghi o. C th dng khuch i mt chiu hoc khuch i
xoay chiu.
3.4.6. B phn ghi o
u theo cc hng sn xut, c th l my c, my ghi, my hin

s, km my tnh,... nh k thut in t pht trin, b phn ny ngy
cng c hon thin.
3.5. Cc cch xc nh nng dung dch trong phng php o

quang ph hp th UV-VIS
3.5.1. Phng php trc tip
kt qu nng CX.
67
, E1%1cm c th c trong bng tra cu (hoc t xc nh

t cht chun gc).
(c kim tra k v thang bc sng v v hp th).
V d: nh lng vitamin B12 trong dung dch thuc tim bng

phng php quang ph hp th UV-VIS.
Chun b dung dch th t mu ch phm nh v d phn nh tnh

vitamin B12 trn v o mt quang ca dung dch ny bc sng
361nm.
m lng vitamin B12 (mg/ ml) c tnh theo cng thc:
rong :
D: i tr mt quang o c ca dung dch th vitamin B12 207:

hp th ring (E1%1cm) ca vitamin B12 bc sng 361nm.
n: s pha long ca dung dch cn xc nh.
3.5.2. Phng php ng chun
c nng bit trc C1, C2, C3, C4,

C5 em o mt quang tng ng
D1, D2, D3, D4, D5. V th D - C.
cn xc nh CX c DX.
X da vo ng chun
xc nh CX.
Yu cu:
+ ng chun phi thng. Hnh 7. th biu din mi

quan h
+ CX phi nm trong khong C1 ca mt quang vo nng
68
C5 (tc khi o DX phi nm trong

khong D D5).
V d: nh lng Fe3+ bng phng php o quang.
- Nguyn tc:
Da vo phn ng to phc mu gia Fe3+ v CNS

trng acid:
Fe3+ + 3CNS = Fe(CNS)3
Phc ny c kh nng hp th nh sng vng kh kin, do c

th dng phng php o hp th vng kh kin nh lng
Fe3+.
- Dng c v ho cht:
+ My quang ph UV-V S (c th dng mt my o quang km b

knh lc mu).
+ Pipet chnh xc.
+ Bnh nh mc 25 ml.
+ Cc thu tinh.
+ ng so mu.
+ Dung dch FeCl3 0,01M (hoc Fe( 3)3 0,01M).
+ Dung dch KC S 0,1M.
+ Dung dch Cl 10%.
+ Dung dch Fe3+ cn nh lng: dung dch X (bnh 7) tin hnh

theo phng php nhn mt, so snh; dung dch Y (bnh 8) tin hnh
theo phng php ng chun.
- Tin hnh:
+ Chun b dy dung dch theo bng sau:
Bng 4. B tr dung dch chun b nh lng Fe3+
69
+ Phng php so mu bng mt:
Ly 6 ng so mu (ng ging nhau), nh s t 1 n 6. dung

dch t cc bnh 2, 3, 4, 5, 6 vo cc ng t 1 n 5 tng ng. ng 6
dung dch cn xc nh bnh th 7 vo. So snh cng mu ca
ng s 6 xem gn bng (hoc bng) mu ng no (hay gia hai ng
no). tnh c nng ca dung dch Fe3+.
+ Phng php so snh mt quang:
* Chn bc sng (hoc chn knh lc mu):
Da trn nguyn tc cc cp tia sng ph nhau, cho nn vi dung

dch o c mu (ng vi bc sng 630 760nm) s o mt
quang D mu vng lc cam (ng vi bc sng 450 570nm).
chn c bc sng (hoc knh lc mu) thch hp, ta lm nh sau:
dch ny trong khong t 450 670nm v xc nh cc i hp th

max). o hp th ca cc dung dch nh lng bc sng ny.
em o mt quang ca hai dung dch ny (mu trng l dung dch

bnh 1) cc bc sng t 450nm 570nm bng cc knh lc. ng vi
mi knh lc, vi hai dung dch ta c hai gi tr mt quang tng
ng D1 v D2 2 D1 cc im o . Knh lc no cho
max th chnh l knh lc mu thch hp dng cho nh lng.
* o mt quang ca dung dch t bnh 2 n bnh 6 bc sng

hoc knh lc xc nh c trn vi mu trng l dung dch bnh
1.
* Lp ng chun biu din mi quan h gia mt quang D 1, D2,

D3, D4, D5 ca 5 bnh 2, 3, 4, 5, 6 trn. V th s ph thuc ca D v
nng Fe3+.
* o mt quang Dy ca dung dch Y (bnh s 8), da vo ng

chun v suy ra nng Cy ca Fe3+ trong dung dch Y.
70
3.5.3. Phng php so snh
0:
D0 .C0.l
Cx cn xc nh (cng iu kin
o nh vi dung dch chun):
Dx .Cx.l
tnh c
+ Dung dch phi tun theo nh lut Lambert Beer.
+ C0 v Cx khc nhau khng nhiu (thng 10%).
V d: nh lng novocain bng phng php chit o quang
- Nguyn tc:
ovocain l mt baz tng hp, c kh nng to cp ion mu vi

mt s cht acid (v d mu azoin nh da cam methyl, tropeolin OO,...).
rong mi trng dung dch m acetat (c p = 4 - 5) novocain di
dng cation (B+) v acid mu nh da cam methyl di dng anion (A-)
to thnh cp ion B+A- c mu chit c vo cloroform:
B+: dng cation ca ancaloid, base tng hp.
B+A
nh lng, ly lp cloroform em o mt quang bc sng

420nm.
- Dng c, ho cht:
+ Buret.
+ Pipet chnh xc cc loi.
71
+ Bnh gn 50 ml.
+ Bnh nh mc 25 ml.
+ Cc thu tinh.
+ Phu lc, giy lc.
+ ng nghim to.
+ Dung dch novocain chun 1mg/ ml (0,1%).
+ Dung dch tim novocain nh lng (khi dng phi tnh pha
long c nng gn chun).
+ Dung dch m acetat (p = 4,20).
+ Dung dch da cam methyl 0,1%.
+ Cloroform.
- Tin hnh:
Cho vo 5 bnh gn cc cht theo bng sau:
Bng 5. B tr dung dch chit nh lng novocain
Chit cc bnh vi C Cl3 bng cch lc nh 5 pht (lm 3 ln, mi

ln 6 ml CHCl3). p dch chit C Cl3 (3 ln) ca tng bnh gn vo
tng bnh nh mc 25 ml tng ng, thm C Cl3 vo tng bnh cho
n vnh, lc u. Lc qua giy lc kh vo cc ng nghim to tng
ng (sch v kh).
o mt quang D ca cc dch lc (trong ng nghim) bc

sng 420nm vi mu trng l dch chit ca bnh S0.
72
nh kt qu theo phng php so snh:
rong :
Cx: nng dung dch novocain cn nh lng (mg/ ml).
Cch: nng dung dch novocain chun (mg/ ml).
: mt quang trung bnh ca bnh X1 v X2.
: mt quang trung bnh ca bnh S 1 v S2.
Ch : Khi o mt quang ca dch chit khng c s dng

cuvet nha.
3.5.4. Phng php thm
x cn xc nh c Dx
.Cx.l
t vo dung dch cn xc nh v o
mt quang Dx + t .(Cx + Ct).l.
tnh c
dch tun theo nh lut Lambert - Beer v Ct 10%Cx). Phng php

ny c u im loi tr c mt s yu t nh hng c cng trong
dung dch (hoc trong mu phn tch) m ta cha bit.
V d: nh lng Berberin trong vin nn Berberin theo phng

php thm.
- Nguyn tc:
Dung dch Berberin trong nc c cc i hp th nh sng bc

sng 263nm v 345nm, v th c th p dng phng php o quang
nh lng berberin. hng v trong vin nn, thnh phn phc tp,
ngoi berberin cn c t dc, do c th dng phng php thm
khc phc c mt s yu t nh hng.
73
- Dng c, ho cht:
+ Cn phn tch.
+ Ci, chy s.
+ Bnh nh mc.
+ Cc thu tinh.
+ iy lc bng xanh.
+ Phu lc.
+ Pipet chnh xc.
+ Berberin hydroclorid dng lm chun.
+ Mu vin nn berberin.
- Tin hnh:
+ Pha dung dch berberin 0,1% (dng lm chun): Cn chnh xc trn

cn phn tch mt lng cn thit pha (qua tnh ton), ho tan bng
nc nng.
+ Cn chnh xc 20 vin nn berberin cn nh lng. nh khi

lng trung bnh ca mt vin. ghin trong ci s thnh bt mn.
+ Cn chnh xc m gam mt lng bt vin (tng ng vi khong

0,05g berberin) cho vo cc c m loi 100 ml, tm t bt bng 10 ml
nc ct. hm 60 ml nc nng, khuy k. lng ngui 15 pht, gn
chuyn dung dch vo bnh nh mc 100,0 ml. Phn cn li thm tip
nc nng, khuy k, sau tp trung ht vo bnh nh mc 100,0 ml
trn, thm nc n vch, lc k. Lc qua giy lc kh, b 20 ml nc
lc u. Ly chnh xc 1,00 ml dch lc cho vo bnh nh mc 100,0 ml
khc, thm nc n vch. Lc k. em o mt quang bc sng
345nm vi dung dch so snh l nc ct c D x.
+ Song song tin hnh mt th nghim nh trn nhng sau khi cn

chnh xc m gam bt vin, cho thm mt lng chnh xc dung dch
chun berberin 0,1% (10,00 ml dung dch berberin chun 0,1% tng
ng 0,01g berberin) vo trc khi ho tan, cc giai on sau tin hnh
tng t. Kt qu o mt quang c D'x.
74
Dx, D'x v lng berberin chun bit thm vo, tnh hm lng
berberin trong mt vin.
4. PHNG PHP O TH
4.1. Khi nim
cc ion ca cht nghin cu da vo s o in th ca dung dch cha

cc ion .
ca phng php o th l o sut in ng ca mt

pin to bi mt in cc c th thay i ph thuc vo nng ion ca
cht nghin cu trong dung dch (gi l in cc ch th) v mt in cc
c th khng thay i (gi l in cc so snh).
C hai in cc c nhng vo dung dch phn tch. Khi ta c:
Ex = Ess - Ect
rong :
Ex l in th ca dung dch th.
Ess l th in cc so snh.
Ect l th in cc ch th.
Hnh 8. S mch o th
bt c ion no nu tm c in cc ch th tng ng cho ion .

thut thc hin ta c 2 cch:
75
+ o th trc tip ca dung dch cha ion cht cn xc nh bng

cch nhng in cc ch th cho ion v in cc so snh vo dung
dch phn tch, t theo phng trnh ernst tnh ra kt qu (hoc o
theo cch so snh: o th ca dung dch bit nng v o th ca
dung dch cn xc nh, t tnh ra nng ca ion cht cn xc nh).
rong phn tch, phng php ny thng c p dng o p
(nng ca ion +).
+ o th ca dung dch trong qu trnh chun , t xc nh

c im tng ng tnh ra nng ca cht cn phn tch.
rong phn tch gi l phng php chun o th.
heo cc nh ho hc quy c:
+ Catod ( xy ra qu trnh kh, tc l xy ra s nhn e) v cc

thng tin lin quan vit bn tri.
+ Anod ( xy ra qu trnh oxy ho, tc l xy ra s cho e) v cc

thng tin lin quan vit bn phi.
+ anh gii gia cc pha ghi bng vch thng |.
+ u mch c cu mui th c ghi bng 2 vch thng song song

||.
4.2. Mt s in cc thng dng trong phng php o th
4.2.1. Cc in cc ch th
L cc in cc c in th ph thuc vo nng ca ion cht

nghin cu. V d:
+
dng o p ):
L mt bnh cu nh bng thu tinh c thnh mng, trong bnh cha

dung dch m c p xc nh (hoc dung dch Cl). Bn trong bnh c
cm si dy Ag c ph lp AgCl bn ngoi. on b c t trong
mt ng bo v, hnh 9.
76
Hnh 9. S in cc thu tinh
Mch o:
+
Ag|AgCl|dung dch m|mng thu tinh|dung dch cn o | |)
Khi nhng in cc vo dung dch cn o +, cc ion H+ dung dch

o s trao i vi ion H+ trn b mt mng thu tinh, xut hin th in
cc.
(Eott gi l in th khng i xng, chnh l hiu s in th gia 2

pha ca mng thu tinh, n l hng s ph thuc nhit v bn cht
ca mi in cc c th).
+ Dy Ag nhng vo dung dch Ag 3: l cc ch th cho ion Ag+
Ag - e = Ag+ Ag = EoAg + 0,059lg[Ag+]
+ Dy Ag nhng vo dung dch X : l cc ch th cho X .
Ag+ + X AgX = [Ag+] [X ]
4.2.2. Cc in cc so snh
L cc in cc c th khng i trong sut qu trnh o. V d:
77
dung dch KCl c nng c nh (Ag/AgCl/KCl/mng xp/dung dch o)
2Cl2
(calomel), KCl c nng c nh.
(Dy dn tr | g| g2Cl2|KCl| mng xp | dung dch o)
4.2.3. Cc in cc t hp
cho gn v thun tin cho ngi s dng, hin nay cc hng sn

xut cc in cc t hp l mt in cc kp gm mt in cc ch th
v mt in cc so snh:
Calomel.
h Ag/AgCl.
- Calomel.
Cc in cc ny thng c cu to ng trc, in cc so snh bao

quanh in cc ch th.
4.3. S dng my o th o pH v chun o th
4.3.1. o pH
so snh l
calomel.
0,05 p (hoc 0,003V).
+ h s b xem dung dch cn o c p khong bao nhiu.
78
+ iu chun my bng t nht hai dung dch m (thng dng

dung dch m c p 4,00 v p 7,00 i vi o dung dch th vng
acid; v dung dch m c p 9,00 v p 7,00 i vi o dung dch th
vng kim).
+ o p ca dung dch cn th.
Lu tt c cc php o u cn phi tin hnh trong cng mt iu

kin nhit khong 20oC 25oC.
V d: o p ca dung dch bi tp.
- Nguyn tc:
S dng my o th vi in cc ch th l thu tinh v in cc so

snh l calomel (hay Ag/AgCl) hoc in cc t hp.
hng nm iu chnh chnh ca my o th (p metre):
Hnh 10. S my o pH Jenway (Anh)

1: m chn chc nng: off, mV, p ; 2: iu chnh nhit ;
3: iu chnh dc (slope); 4: iu chnh th bt i xng (Buffer hoc
AP);
5: Mn hnh hin s; 6: in cc t hp; 7: Dung dch cn o.
- Dng c, ho cht:
+ My o p .
+ in cc thu tinh, calomel (hoc in cc t hp).
+ Cc dung dch.
+ Dung dch m chun p = 7,00; p = 4,00, p = 9,00.
+ Ch th mu vn nng.
79
- Tin hnh:
+ iu chnh nm 1 my ch o p , iu chnh nm 2 n
nhit ph hp.
+ Dng giy ch th th dung dch cn o xem p khong no. i

s dung dch bi tp c p khong 5.
+ Chun my: chn hai dung dch m chun p = 7,00; p = 4,00.

a in cc bng nc ct, thm kh in cc bng khn mm. Cho
in cc ngp vo dung dch m 7,00. iu chnh nm 4 v ng gi tr
7,00. a in cc bng nc ct, thm kh in cc bng khn mm.
Cho in cc ngp vo dung dch m 4,00. iu chnh nm 3 v ng
gi tr 4,00.
+ hay dung dch m bng dung dch cn o, mn hnh s ch tr s

p ca dung dch.
Ch : Mi khi thay dung dch o, phi dng bnh phun nc ct ra

sch cc, lau kh bng giy sch mn v mm.
4.3.2. Chun o th
cc ch th thch hp v mt in cc so snh. in hnh chun v

ghi s bin i ca in th theo th tch dung dch chun cho vo.
Dng phng php th, thit lp quan h gia in th E v th

tch dung dch chun thm vo.
im tng ng (Vt) l ng vi im un ca ng biu din.

Vt tnh ra kt qu.
ch quan, c th chun vi
nhng dung dch c, c mu. C kh nng t ng ho.
80
Hnh 11. B tr th nghim nh lng bng phng php chun

o th
V d: Chun 3PO4 bng dung dch a theo phng php o

th.
Cp in cc hay dng l: hu tinh + calomel (hay Ag/AgCl) hoc

in cc t hp thu tinh - calomel, hu tinh Ag/AgCl.
Phng trnh ca phn ng nh lng l:
H3PO4 + NaOH = NaH2PO4 + H2O (1)
NaH2PO4 + NaOH = Na2HPO4 + H2O (2)
NaH2PO4 + NaOH = Na3PO4 + H2O (3)
h vy trong qu trnh nh lng, p ca dung dch lin tc thay

i v ti cc im tng ng (1), (2) c s thay i t ngt ca p
(im tng ng (3) khng r). u ta ghi chp quan h gia th tch
dung dch (V ml) chun a cho vo dung dch cn nh lng 3PO4
vi in th E ca dung dch (hoc p ) sau mi ln cho a , ri v
th ta s c ng cong chun . th hoc bng theo di ta
xc nh c th tch dung dch chun a im tng ng.
tnh c nng ca dung dch 3PO4.
- Dng c, ho cht:
+ My o th.
+ My khuy t.
+ Que khuy.
81
+ Buret.
+ Cc ng dung dch.
+ in cc: thu tinh + calomel (hay cc tng hp).
+ Dung dch NaOH 0,1N.
+ Dung dch cn nh lng 3PO4
- Tin hnh:
+ Ly chnh xc 10,00 ml H3PO4 cn nh lng cho vo cc 250 ml

t trn my khuy t. hm que khuy lp in cc v ni vi my (ch
in cc cch y cc khong 2cm trnh que khuy chy lm v
in cc). hm nc ct cho ngp in cc. dung dch a 0,1
ln trn buret.
+ Bt my o ch o th E (mV) hoc o p . hi gi tr th E
ban u.
+ Bt my khuy t, nh a 0,1 t buret xung, sau mi ln

thm 1 ml NaOH 0,1N ml) tt my khuy, ghi th E. heo di
cho n khi thy c hai bc nhy th, ghi nh th tch a 0,1
tng ng vi ln cn 2 im ny (im tng ng).
+ Lp li ng tc chun trn, nhng ln cn 2 im tng

ng thm d qua chun
ml), li tt my khuy v ghi gi tr th ca dung dch. Kt qu ghi vo
bng nh sau:
VNaOH ( ml) E (mV)
V ng cong chun E = f(VNaOH). ng cong c dng:
82
im un ca ng cong ng vi im kt thc (im tng

ng) c xc nh bng phng php hnh hc.
th tch Vt tnh nng CM ca 3PO4.
T LNG GI V BI TP
1. y nu cc phng php tch cc cht bng phng php chit.
2. rnh by nguyn tc, i lng c trng, cch tin hnh ca sc

k lp mng.
3. u nguyn tc, cch tin hnh ca sc k trao i ion.
4. in t hoc cm t cn thiu vo ch trng trong cu sau:
a) Phng php lc l phng php dng tch........................

khi pha rn.
b) Phng php ly tm l phng php dng.................... lm

lng kt ta xung.
c) Phng php chit l phng php dng............................

tch ly mt cht (hay mt nhm cht) t mt hn hp nghin
cu trong dung dch.
5. rnh by nh lut c bn v s hp th nh sng: nh lut

Lambert-Beer.
6. rnh by khi nim v ng dng ca quang ph hp th UV-VIS.
7. Cc b phn chnh ca my o quang ph UV-VIS.
8. y nu cc k thut xc nh nng dung dch trong phng

php o quang.
83
9. rnh by khi nim in cc ch th. y nu mt s in cc ch

th thng dng.
10. rnh by khi nim in cc so snh. y nu mt s in cc

so snh thng dng.
11. y trnh by cch o p bng my o th.
12. u nguyn tc ca chun o th v cch xc nh im

tng ng.
13. nh th oxy ho kh ca h gm cc Ag nhng trong dung dch

AgNO3 0,1mol/l; 0,001mol/l. Bit Eo = 0,80V.
14. Tnh th oxy ho kh ca h gm cc Ag ph lp AgCl nhng

trong dung dch KCl c nng 1mol/l. Bit E o = 0,80V v TAgCl =
1,6.10-10.
15. Pha long 100 ln dung dch cloramphenicol ri em o mt

quang bc sng 279nm vi b dy cuvet l 1cm c 0,820.
nh nng % ca dung dch cloramphenicol em nh lng.
Bit E1%1cm ca cloramphenicol bc sng 279nm l 297.
16. Ly chnh xc 10,00 ml dung dch tim vitamin B12 pha cho
thnh 100,0 ml. o mt quang ca dung dch thu c
bc sng 361nm, b dy cuvet l 0,5cm c 0,470. nh s
ml ca dung dch vitamin B12 em nh lng. Bit E1%1cm ca
vitamin B12 bc sng 361nm l 207.
Chn cu tr li ng cho cc cu hi t 17 n 19 bng cch

khoanh trn ch ci u cu c chn:
17. Theo quy c:
a) Vng t ngoi nm trong khong:
A. 185 400nm B. 220 350nm
C. 200 400nm D. Ln hn 200nm
b) Vng kh kin nm trong khong:
A. 350 600nm B. 400 760nm
C. 300 800nm D. Ln hn 400nm
18. rong vng quang ph kh kin:
a) ia mu ng vi mt chm tia c bc sng:
84
A. 570 500nm B. 760 630nm
C. 500 450nm D. 450 430nm
b) ia mu tm ng vi mt chm tia c bc sng:
A. 600 570nm B. 760 630nm
C. 430 400nm D. 450 430nm
c) ia mu chm ng vi mt chm tia c bc sng:
A. 600 570nm B. 760 630nm
C. 430 400nm D. 450 430nm
19. rong vng quang ph kh kin:
a) Mu ph vi mu:
A. Xanh lc B. Da cam C. Lc
xanh D. Vng
b) Mu lc vng ph vi mu:
A. B. Da cam C.
Tm D. Vng
c) Mu vng ph vi mu:
A. B. Xanh lam C.
Tm D. ta
Bi 6
XC NH GII HN TP CHT
TRONG THUC V TRONG DC LIU
MC TIU
- Trnh by c phng php xc nh gii hn tp cht trong thuc.
- Trnh by c cch xc nh gii hn tp cht, t l vn nt trong

dc liu.
85
1. TH GII HN CC TP CHT TRONG THUC
1.1. Mc ch
Xc nh gii hn tp cht trong thuc thc cht l th tinh khit

ca thuc nhm xc nh phm cht ca thuc. u thuc cng tinh
khit th hiu qu tc dng cng cao, n nh.
Cc tp cht trong thuc mc d rt nh nhng n c th:
- y tc hi cho sc kho (v d tp cht bari tan, arsen, ch,...).
- y hin tng tng k ho hc, nh hng n phm cht hay

bn vng ca thuc.
- Mt s tp cht c th khng c tc dng c hi nhng li l nhng

cht xc tc y nhanh qu trnh phn hu thuc (V d: cc vt kim loi,
m,...).
- Mt s tp cht khng gy hi, khng gy tng k ho hc, khng

lm phn hu thuc, khng gy phn ng ho hc,... nhng n biu th
cho mc sch (hay mc tinh ch cha ) ca thuc.
- Khi bit mc tinh khit ca thuc (c bit trong trng hp

khng t yu cu) cho php xem xt cc ngun gc gy ra cc tp cht
ny v tm bin php khc phc. Cc nguyn nhn c th l:
- guyn liu, ph liu hoc bn thnh phm dng sn xut thuc

cha tinh khit.
- Quy trnh sn xut quy nh khng c thc hin nghim

chnh.
- nh hng ca cc dng c s dng.
- Phng php sn xut cha tt.
- rong qu trnh bo qun, cc phn ng ph do nhiu yu t nh:

mi trng, vn v sinh, cht bo qun,... lm pht sinh cc tp cht.
- Do dng gian ln ca ngi sn xut,...
Bi vy, CV (Dc in) v C thng quy nh cho php mi

thuc ch c c nhng lng rt nh cc tp cht nht nh bo
m cho thuc c sch nht nh, tc l thuc c cht lng, t
hiu qu tc dng cao nht.
1.2. Phng php xc nh gii hn tp cht trong thuc
86
1.2.1. Phng php xc nh
p cht trong thuc c th l cht v c, cht hu c, cht phn

hu hoc tp cht lin quan.
Xc nh gii hn tp cht trong thuc tc l xc nh xem cc tp

cht c vt qu gii hn cho php hay khng, cc phn ng th tp
cht c tnh cht bn nh lng v c thc hin bng phng php
so snh.
Cc tp cht cht hu c, cht phn hu hoc tp cht lin quan

thng c xc nh bng phng php sc k. p cht v c c
xc nh bng phn ng ho hc. rong ni dung ca bi ny, chng ti
ch trnh by cch xc nh tp cht v c trong thuc. Qu trnh xc nh
c tin hnh nh sau:
Bnh 1: Ly mt th tch dung dch thuc em th.
Bnh 2: Ly mt th tch dung dch mu. (Dung dch mu l dung dch

c cha tp cht cn th vi lng cho php).
thuc th. So snh kt qu phn ng hai bnh (thng l so mu hoc

so c) t xc nh c gii hn tp cht cn th c trong mu
thuc em th.
+ c v nhng ho cht, thuc th s dng khng c c tp

cht ang cn th.
+ Khi pha dung dch mu phi s dng cn phn tch v dng c

ong o th tch chnh xc.
+ ai bnh phn ng so snh phi ging nhau: bng thu tinh

khng mu, c ng knh bng nhau, dy nh nhau,...
+ Khi so snh, quan st c th nhn t trn xung, quan st mu

th nhn ngang trn nn trng.
+ Phi cho cc thuc th vo hai bnh phn ng ging nhau v: thi

gian, s lng v th tch cui.
- Khi phn tch, nu pht hin c mt tp cht l th phi ghi li v

bo co.
1.2.2. Pha cc dung dch mu
87
pha dung dch mu ca mt tp no , ch cn cn lng chnh

xc cht tinh khit ca tp (cht gc) pha vo mt th tch xc nh
theo tnh ton ta s c mu tp chun c nng xc nh thng
biu th theo mg/ ml; % hoc phn triu (nh trnh by mc 2, bi
4).
V d: Pha dung dch mu Cl- nh sau:
nc v thm nc cho 1 lt (dng bnh nh mc). c dung dch

c cha:
ml dung dch A pha long bng nc cho 100,0 ml. Dung dch ny c
cha (tng ng 0,005mgCl-/ ml hay dung dch

0,0005% hoc 5 phn triu).
1.2.3. Pha dung dch th
pha, gi thit mu em kim tra c cha mt lng tp cht cho

php ti a, t tnh h s pha long thch hp, sau tin hnh pha
theo tnh ton ny.
V d: Pha dung dch th tp Cl trong paracetamol (theo tiu

chun Cl khng c qu 0,01%):
V dung dch mu Cl- khi em th l dung dch c cha 0,0005% (hay
5 phn triu). Do h s pha long dung dch th s l

c cch pha nh sau: Cn 1,000g paracetamol ho tan trong nc cho
20,00 ml lc. Ly 10,00 ml dch lc em th v so snh vi 10,00 ml
dung dch mu chun Cl - 0,0005%.
rong Dc in hoc C c ghi r cch pha dung dch th l

da trn c s cch tnh ny, ngi lm kim nghim lm theo ch dn
khng cn phi tnh ton.
1.3. Mt s thuc th trong cc phn ng ho hc xc nh gii

hn tp cht
Mt s thuc th xc nh gii hn tp cht thu c sn phm

phn ng v hin tng quan st pht hin c trnh by trong
bng 6.
Bng 6. Kt qu xc nh gii hn ca mt s tp cht
88
Ion cn th (tp Hin tng

Thuc th Sn phm
cht) quan st
Cl- AgNO3 a trng
SO42- BaCl2 BaSO4 a trng
Mu vng (nu
NH4+ Nessler nhiu c mu
nu )
Ca2+ (NH4)2C2O4 CaC2O4 a trng
iy tm gCl2
Arsen Zn + HCl AsH3 chuyn t vng
sang nu
- Na2S (H2S)
Kim loi nng en hoc nu
- Thioacetamid
Acid mercapto-
Feri mercaptoacetat Mu hng
acetic
St
Acid nu hay
Ferisulfisalicylat
sunfosalicylic vng
8- Mu vng rm
Nhm hydroxyquinolin (tan trong
CHCl3)
(oxiquinolat nhm)
8-
Mu vng (tan
Magnesi hydroxyquinolin Oxiquinolat Mg
trong CHCl3)
Phosphat Sulphomolybdic (NH4)3H4[P(Mo2O7)6] Mu vng

Km K4[Fe(CN)6] K2Zn3[Fe(CN)6]2 a trng
1.4. Mt s v d p dng
1.4.1. Th gii hn tp cht amoni
C 2 phng php th gii hn tp cht amoni, chng ti ch trnh

by phng php A l phng php hay c s dng trong php th
ny.
in hnh ng thi phn ng hai bnh nh sau:
89
ml dung dch ion amoni ( 4+) mu c

nng 1phn triu, thm nc thnh 15 ml, thm tip 0,3 ml thuc th
Nessler, lc u ri yn 5 pht.
tiu chun (chuyn lun) vi nc (kim ho nu cn bng dung dch

a 2M), thm nc thnh 15 ml, thm tip 0,3 ml thuc th essler,
lc u ri yn 5 pht.
So snh mu ca 2 bnh: Mu ca bnh 2 khng c m hn mu

ca bnh 1.
1.4.2. Th gii hn tp cht arsen
C 2 phng php th gii hn tp cht arsen, chng ti ch trnh

by phng php A l phng php hay c s dng trong php th
ny.
th:
m mt bnh nn nt mi c 100 ml xuyn

qua nt c ng thu tinh ng knh trong 5mm
(phn di ca ng c ko b li c ng
knh trong l 1mm), di 200mm.
Cch u ng 15mm, c mt l trn thnh ng

(vi ng knh 2 - 3mm), khi gn ng vo nt th
l ny phi cch mt di ca nt t nht 3mm.
u trn ca ng c mt a trn phng vung gc
vi trc ng.
Mt ng thu tinh th hai di 30mm (cng

ng knh v cng c a trn phng tng t).
khong 60mg bng tm ch acetat ( ), t mt

ming giy tm thu ngn ( ) bromid ( ) hnh trn
hay vung c kch thc ph kn l trn gia 2 ng Hnh 12. Dng c
thu tinh, gi cht 2 ng thu tinh vi nhau bng 2 th Arsen
dy l xo.
chuyn lun, ho tan hoc pha long vi nc thnh 25 ml, thm 15 ml

acid hydroclorid (TT), 0,1 ml dung dch thic ( ) clorid As ( ), 5 ml
dung dch kali iodid 20% ( ). yn 15 pht, thm 5g km ht khng
c As ( ). y ngay bnh nn bng nt lp sn giy th trn.
gm bnh nn trong nc nhit sao cho kh gii phng ra u n.
90
Song song tin hnh mt mu so snh trong cng iu kin (dng 1

ml dung dch arsen mu 1 phn triu, thm nc thnh 25 ml thay cho
ch phm cn th).
Sau t nht 2 gi, ly cc ming giy tm thu ngn ( ) bromid ra so

snh cc vt mu. Vt mu ca ming giy trn bnh cha ch phm cn
th nht hn mu ming giy trn bnh cha dung dch arsen mu.
Ch : Dung dch thic ( ) clorid As l dung dch thic ( ) clorid

dng cho php th Arsen.
1.4.3. Th gii hn tp cht clorid
ml dung dch ch phm cn th ( pha theo ch dn),

thm 1 ml dung dch acid nitric 2M v 1 ml dung dch bc nitrat 2% ( ).
ml dung dch clorid mu 5 phn triu v 5 ml nc.

Thm 1 ml dung dch acid nitric 2M v 1 ml dung dch bc nitrat 2% ( ).
yn 5 pht, trnh nh sng. So c ca 2 bnh: c bnh 1

phi khng bng c bnh 2.
1.4.4. Th gii hn tp cht kim loi nng
C 5 phng php th gii hn tp cht kim loi nng, chng ti ch

trnh by phng php 1 l phng php hay c s dng trong php
th ny.
in hnh ng thi phn ng hai bnh nh sau:
ml dung dch ch phm cn th (c pha ch

theo ch dn ca chuyn lun), thm 2 ml dung dch m acetat p = 3,5,
lc u, thm 1 - 2 ml dung dch thioacetamid ( ), lc ngay ri yn 2
pht.
ml dung dch ion ch mu 1 phn triu (hoc 2 phn

triu tu theo ch dn), thm 2 ml dung dch ch phm cn th, thm 2 ml
dung dch m acetat p = 3,5; lc u, thm 1 - 2 ml dung dch
thioacetamid ( ), lc ngay ri yn 2 pht.
So snh mu ca 2 bnh: Mu ca bnh 1 khng c m hn mu

ca bnh 2.
1.4.5. Th gii hn tp cht st
ml dung dch ch phm cn th (c pha theo ch

dn ca chuyn lun), thm 2 ml dung dch acid citric 20% ( ), thm 0,1
ml acid mecaptoacetic ( ), lc u, kim ho bng dung dch amoniac
10M ( ), thm nc thnh 20 ml.
91
ml dung dch st mu 1 phn triu, sau thm 2

ml dung dch acid citric 20% ( ), thm 0,1 ml acid mecaptoacetic (TT),
lc u, kim ho bng dung dch amoniac 10M ( ), thm nc thnh
20 ml.
Sau 5 pht, so snh mu hng ca 2 bnh: Mu ca bnh 1 khng

c m hn mu ca bnh 2.
1.4.6. Th gii hn tp cht sulfat
ml dung dch bari clorid 25% ( ), thm 1,5 ml dung dch

sulfat mu 10 phn triu, lc u, yn 1 pht. hm tip 15 ml dung
dch ch phm cn th ( pha theo ch dn), thm 0,5 ml acid acetic 5M
(TT).
ml dung dch bari clorid 25%, thm 1,5 ml dung dch

sulfat mu 10 phn triu, lc yn 1 pht. hm tip 15 ml dung dch
sulfat mu 10 phn triu, thm 0,5 ml acid acetic 5M (TT).
yn 5 pht. So c ca 2 bnh: c bnh 1 phi khng bng

c bnh 2.
1.4.7. Th gii hn tp cht phosphat
ml dung dch ch phm cn th ( pha theo ch

dn), thm 4 ml thuc th sulphomolybdic. Lc, thm 0,1 ml dung dch
phosphat mu 5 phn triu.
ml dung dch phosphat mu 5 phn triu, thm 98 ml

nc ct. hm 4 ml thuc th sulphomolybdic. Lc, thm 0,1 ml dung
dch phosphat mu 5 phn triu.
Sau 10 pht, ly mi bnh 10 ml dung dch, em so snh mu vng:

Mu ca bnh 1 khng c m hn mu ca bnh 2.
2. XC NH TP CHT LN TRONG DC LIU
p cht ln trong dc liu bao gm tt c cc cht ngoi quy nh

ca dc liu : t, , rm r, cy c khc, cc b phn khc ca
2.1. Cch xc nh
trn t giy, quan st bng mt thng hoc knh lp (khi cn c th

dng ry phn tch tp v dc liu) v tch ring tp ra khi dc
92
rong :
2.2. Ch
trn cha phn bit c, khi c th phi lm cc phn ng ho hc,

dng knh hin vi, dng cc phng php vt l, ho l khc,... pht
hin ra tp cht v vy khi tnh phi tnh c cc tp cht loi ny.
+ Vi dc liu dng ht v qu rt nh khong 10g.
+ t v qu nh va khong 20g.
+ Dc liu thi thnh lt khong 50g.
3. CCH XC NH T L VN NT CA DC LIU
Cn a gam (thng t 100 200 g) dc liu c loi b tp

cht, ry qua ry c s theo quy nh ca chuyn lun. Cn ton b phn
lt qua ry (gi s c m gam). tnh t l % vn nt ca dc
liu:
Ch : i vi cc dc liu dng lt mng, khi ry ch lc nh,

trnh lm nt vn thm dc liu. Phn bt vn v bi khng phn bit
c bng mt, thng c tnh vo phn tp cht.
4. XC NH TRO TON PHN CA DC LIU
Cn chnh xc khong 1 3 g mu, nung nhit khng qu

450oC (dng chn s hoc chn Pt) n khi lng khng i. Xc nh
cn tro v tnh% tro ton phn theo dc liu lm kh trong khng kh
(chn nung c xc nh khi lng trc).
Ch : Cn tro thu c phi trng hoc gn nh trng. u cn tro

cn en chng t carbon cha chy ht, khi phi thm mt t nc
nng, khuy u, lc qua giy lc khng tro (gi ly c nc lc v c
cn trn giy lc). rc tin cho giy lc c cn vo chn nung v em
nung n khi cn thu c gn nh trng. Sau cho tip phn nc lc
93
vo chn, lm bc hi n kh, nung tip 450oC n khi lng khng

i. Cn khi lng v tnh % tro ton phn.
5. XC NH TRO SULFAT
Cn chnh xc khong 1 g mu cho vo chn nung (chn s hoc Pt)

bit khi lng, lm m mu vi acid sulfuric ( ), t cn thn, ri li
lm m vi acid sulfuric v nung kh 800 oC n khi lng khng i.
Cn. tnh % cn tro.
Ch : u cn tro th kim loi nng th nhit khi nung ch

500oC - 600oC.
6. XC NH TRO TAN TRONG NC
un si tro ton phn ( phn 4) vi 25 ml nc trong 5 pht. Lc

qua phu xp hoc dng giy lc khng tro, ra bng nc nng. em
nung cn 15 pht ( nhit khng qu 450 oC). Xc nh khi lng
cn khng tan trong nc. Khi :
Khi lng tro tan trong nc = Khi lng tro ton phn - Khi
lng cn khng tan trong nc. nh % tro tan trong nc so vi dc
liu lm kh trong khng kh.
T LNG GI V BI TP
1. Cho bit mc ch ca vic xc nh gii hn tp cht trong thuc.
2. rnh by phng php xc nh gii hn tp cht trong thuc.
3. rnh by cch xc nh mt s tp cht thng dng:
- Arsen. - St.
- Amoni. - Sulfat.
- Phosphat. - Kim loi nng.
4. Cch xc nh tp cht ln trong dc liu?
5. Cch xc nh t l vn nt ca dc liu?
6. rnh by cch xc nh tro ton phn v tro tan trong nc ca

dc liu.
7. Cch xc nh khi lng ca chn nung trc khi dng xc

nh cn tro ca mu th.
94
Bi 7
PHNG PHP CHUNG
XC NH MT S CH S VT L
MC TIU
- Trnh by c phng php xc nh: khi lng ring, t trng, ch

s khc x, gc quay cc v gc quay cc ring, nhit nng chy.
- Bit cch th r v ho tan ca vin nn, vin nang.
1. KHI LNG RING V T TRNG
1.1. nh ngha
Khi lng ring l khi lng ca mt n v th tch cht xc

nh nhit t:
rong : m: l khi lng (gam) ca cht xc nh nhit t.
V: l th tch ( ml) ca cht xc nh nhit t.
rong ngnh Dc thng xc nh Dt 20oC (vit D20).
T trng (t trng tng i) ca mt cht l t s gia khi lng

ca mt th tch cho trc ca cht v khi lng ca cng mt th
tch nc ct cng iu kin nhit (ngnh Dc xc nh 20 oC).
rong : m, mo l khi lng (gam) ca cht xc nh v ca nc

ct 20oC.
m suy ra t biu thc tnh:
(Do20 l khi lng cn (gam) trong khng kh ca 1 ml nc

o
20 C).
1.2. Phng php xc nh t trng d20 ca mt cht lng
95
1.2.1. Phng php dng picnomet
- Cn chnh xc picnomet rng, kh, sch: m1.
- Cn chnh xc picnomet y cht th 200C: m2.
- cht th, ra sch, lm kh.
- Cn chnh xc picnomet y nc 20 0C: m3.
- Tnh:
1.2.2. Phng php dng cn thu tnh Mohr - Westphal
Mc phao vo n cn, t
phao chm trong nc ct 200C v chnh thng bng bng cc con m
t cc v tr thch hp.
V d:
hm kh, li t phao chm trong cht lng cn xc

nh (ging nh iu kin khi lm vi nc ct) 20 0C v cng chnh
thng bng bng cc con m t cc v tr thch hp ta s c gi tr
M1.
1.2.3. Phng php dng t trng k
+ Lau sch t trng k bng ethanol hoc ether. Dng a thu tinh
trn u cht lng cn xc nh.
+ t nh nhng t trng k vo cht lng (khng c chm vo

thnh hoc y bnh ng). iu chnh nhit v 20 oC.
+ c kt qu khi t trng k n nh.
96
+ trng k Baume: Vic chia vch c tnh theo Baume ( 0Be).

S chuyn i gia 0Be v t trng tnh theo cng thc sau:
* Vi cht nng hn nc:
* Vi cht nh hn nc:
+ u k (alcoholmeter): hng thng cho bit cn tc l hm

lng % ( / ) ca cn em xc nh.
1.3. Phng php xc nh t trng d20 ca m, sp, nha, nha

thm
+ Cn chnh xc picnomet kh, rng, sch 200C: c M1.
+ Cn picnomet y nc 200C: c M4.
+ nc, lm kh picnomet, cho vo picnomet mu th un

chy (dng ng ht hoc phu cung nh) khong 1/3 n 1/2 th tch
ca picnomet, lm ngui n 200C.
+ Cn picnomet c cht xc nh 200C: c M2.
+ hm nc ct n y, cn 200C: c M3.
+ nh kt qu:
Ch : Khi ly kt qu xc nh:
cnomet cho kt qu vi 4 s l.
- 3 s l.
2. XC NH CH S KHC X
2.1. Khi nim
97
Ch s khc x
cht so vi khng kh l t s gia sin
ca gc ti (i) v sin ca gc khc x
( ) ca chm tia sng chiu t khng
kh vo cht .
rong trng hp hai mi trng

c ch s khc x l n1 v n2 ta s c:
n1. sin i = n2.sinR.
trng cho cht lng, cht rn v cht

kh tinh khit, do vy dng gi tr ch
s khc x nh tnh, xc nh
tinh khit ca cht.
2.2. Ch s khc x - khc x k (Refratometer)
sng t mi trng km chit quang vo mi trng chit quang, khi

tng gc ti (i), gc khc x ( ) cng tng theo:
Khi gc ti i tng dn n 90o, gc khc

x tng ti gi tr gii hn 1. Do vy sin i
= sin900 = 1 v , trong n l ch
s khc x cn xc nh ca mi trng
(cht xc nh), l ch s khc x ca bn
thu tinh trn ta p cht lng cn o.
x 20oC 0,5o
589,3nm (ng vi vch D
x k c trang b h thng b chnh v

c hiu chun li cho kt qu c
, bit tnh c n = . sin 1), nhng trn my thng ghi lun gi tr
98
l thuyt 0,0001, cn phi thng xuyn

hiu chun li my vi cc cht chun ca nh sn xut my cung cp,
hoc xc nh ch s khc x ca nc ct 25 oC l 1,3325 v 20oC
l 1,3330, ng thi phi thng xuyn kim tra nhit v sch ca
kho
thang o nng ca ng Sacharose nn thng gi l
ng vi nc ct n = 1,333 th C1%ng = 0%
n = 1,381 th C1%ng = 30%
n = 1,530 th C1%ng = 95%
3. XC NH GC QUAY CC V GC QUAY CC RING
3.1. Khi nim
nh sng t nhin l cc dao ng sng xy ra theo mi hng

trong mt phng vung gc vi phng truyn sng.
nh sng phn cc l nh sng trong cc dao ng sng xy ra

theo mt hng nht nh trong mt phng vung gc vi phng
truyn sng. Mt phng cha dao ng sng c gi l mt phng
phn cc.
phng hay s khc x qua cc mi trng (khi chiu nh sng t nhin

ti b mt ca mi trng vi gc ti m tia ti v tia phn x to thnh
gc 900 th lc tia phn x tr thnh phn cc, mt phng ti l mt
phng phn cc).
hoc dung dch), cht ny c kh nng lm quay mt phng ca nh

sng phn cc i mt gc no gi l . Cht lm quay
mt phng phn cc theo cng chiu kim ng h gi l cht hu tuyn
(k hiu +), cht lm quay mt phng phn cc ngc chiu kim ng
h c gi l cht t tuyn (k hiu -).
0
C khi cho chm tia
sng n s
ca n natri) qua lp cht lng hay dung dch ca cht xc nh c b
dy l 1dm.
99
20
- D ca mt cht rn l gc quay cc o
c khi cho chm tia sng D truyn qua lp dung dch c nng 1%
(KL/ ) v c b dy 1dm 200C.
3.2. My o gc quay cc (Phn cc k)
to
1
chm sng chiu vo bn phn cc P to ra nh sng phn cc qua
lng knh thch anh Q i vo cht quang hot ng o C lm quay mt
phng phn cc, chiu ti bn phn tch A (A phi quay i mt gc ng
bng gc ngc vi gc m cht quang hot C lm quay i nh b
phn lm quay th trng quan st li ging nh ban u khi cha
t cht quang hot vo). c m A phi quay chnh l gc quay cc
ca cht quang hot.
Hnh 13. S my o gc quay cc
C 2 loi phn cc k l phn cc k nhn bng mt thng v phn

cc k in t. gun sng thng dng l n hi natri hay hi thu
ngn.
+ Chn bc sng thch hp theo yu cu (thng dng tia D).
+ Chn nhit thch hp (thng 19,5 oC - 20o5C).
+ Xc nh im ca phn cc k: vi ng o rng (khi xc nh

vi cht lng), vi ng o cha y dung mi (khi xc nh vi cht rn).
+ nh gc quay cc ring:
100
rong :
l: chiu di ng o (dm).
d: t trng ca cht lng.
C: nng phn trm ca cht th rn trong dung dch.
Cn c vo gc quay cc o c, c th tnh nng phn trm

ca cht th trong dung dch:
rong : d20 l t trng ca dung dch 200C.
4. XC NH NHIT NNG CHY, KHONG NNG CHY
4.1. Khi nim
Nhit nng chy (gi tt l im chy) ca mt cht l nhit

hiu chnh, ti ht cht rn cui cng ca cht th nghim chuyn
thnh trng thi lng, bt u bin mu, ho than hoc si bt.
Khong nng chy (gi tt l khong chy) ca mt cht l khong

nhit hiu chnh, k t khi cht rn bt u nng chy v xut hin
nhng git cht lng u tin, n khi cht rn chuyn hon ton sang
trng thi lng.
kt thc nng chy khng xc nh r rng, ta c th ch xc nh

nhit kt thc, hoc nhit bt u nng chy nu nhit cng
nm trong gii hn quy nh trong chuyn lun ring ca ch phm.
4.2. Phng php xc nh
Dc in Vit am trnh by 3 phng php xc nh nhit

nng chy v khong nng chy p dng cho cc i tng khc nhau.
rong chng trnh ny ch trnh by phng php hay p dng nht
4.2.1. Dng c
hp, thng dng l du parafin hoc du silicon, lng cht lng

nhn chm c nhit k v mu th sao cho bu thu ngn cch y
bnh 2cm.
101
trong cht lng.
0,5oC.
- 8cm, ng knh trong 1,0

0,1mm, thnh ng dy khong 0,10 0,15mm.
4.2.2. Cch xc nh
cht ht m thch hp, hoc sy kh 2 gi 100 105oC.
qun xung mt phng cng c mt lp ch phm cao 4 6mm. i

ng mao qun trong bnh ht m trc khi tin hnh o.
ng cht lng n khi nhit thp hn im

chy d kin ca cht th khong 10 oC, iu chnh ngun nhit sao cho
nhit cht lng tng 1oC/pht, hoc cho nhit cht lng tng
3oC/pht khi cc cht th khng bn vi nhit.
im chy d kin khong 5oC, ly nhit

k ra, nhanh chng buc ng mao qun c ch phm vo nhit k, sao
cho lp ch phm ngang vi phn gia bu thu ngn ca nhit k. t
li nhit k vo bnh cht lng.
xung, so snh vi
mt im no trn thnh ng, c xc nh l im bt u nng
chy v nhit m ti cht th tr thnh cht lng hon ton, c
xc nh l im cui ca s chy hay im chy. in hnh xc nh t
nht 3 ln. Cc kt qu o c phi chnh lch khng qu 1 oC. Ly kt
qu trung bnh ca cc ln xc nh. u kt qu o c chnh lch
qu 1oC, lm thm 2 ln na. Ly kt qu trung bnh ca 5 ln xc nh.
nhit k chun v s khc bit nu c gia nhit ca on ct thu

ngn ngoi cht lng trong iu kin th nghim v ca on ct thu
ngn ngoi cht lng trong iu kin hiu chun. hit ca on ct
thu ngn ngoi cht lng c xc nh bng cch t bu thu ngn
ca nhit k ph im gia ca phn ct thu ngn l ra ngoi cht
lng ca nhit k chnh.
nh nhit hiu chnh theo cng thc sau:
Thiu chnh = T + 0,00016N (TS - t)
102
rong :
: hit c trn nhit k chnh.
TS: hit trung bnh ca on ct thu ngn ngoi cht lng ca

nhit k chnh trong iu kin chun ho.
t: hit ca on ct thu ngn ngoi cht lng ca nhit k

ph ti im chy.
: S khong chia (oC) ca on ct thu ngn ca nhit k chnh

ngoi cht lng.
5. PHP TH R CA VIN NN V VIN NANG
5.1. Khi nim
r ca vin nn, vin nang l kh nng tan r ca chng trong

mi trng th theo quy nh (thng l nc) o bng thit b th r
c quy nh (My th r Erweka hay mt thit b tng ng)
trong thi gian nht nh c quy nh tng chuyn lun.
5.2. Thit b
hit b th r (hnh 14) bao gm:
di 75,0 - 80,0mm, ng knh trong 21,5mm v chiu dy thnh ng

khong 2mm.
Mt a hnh tr y trn mi ng, c ng knh 20,55 - 20,85mm

v chiu dy 9,35 - 9,65mm, c lm bng cht do trong sut. a c
5 l hng, ng knh mi l l 2mm, 1 l gia cn 4 l cn li t
cch u nhau trn mt vng trn c bn knh 6mm t tm a.
Cc ng c gi v tr thng ng trong 6 l trng ca 2 tm

nha cng trong sut c ng knh 90mm v chiu dy 6mm. Cc l
cch u nhau v cch u tm. Mt di ca tm nha pha di c
gn 1 tm li an bng cc si thp khng g c ng knh 0,635mm
v kch thc mt l l 2mm.
103
Hnh 14. Thit b th r vin nn, vin

nang
1. gun cung cp nhit 5. ng

hnh tr
2. B iu nhit 6. i
3. Cc ng mi trng th 7. B
phn iu khin
4. a y
ai tm nha c c nh v cch u nhau 77,5mm bng cc

thanh kim loi c cht thng ng pha ngoi v mt thanh kim loi
c gn cht vo tm tm nha pha trn, sao cho gi ng th c
th lp rp vi b phn c vn hnh thit b chuyn ng ln xung
mt khong t 50 - 60mm vi tn sut 28 - 32 ln/pht.
Gi ng th c nhng chm trong mt bnh thch hp,

thng l cc thu tinh c dung tch 1000 ml cha cht lng c
quy nh. h tch cht lng phi sao cho khi gi ng th v tr
cao nht th li kim loi phi di b mt cht lng t nht 15mm v
104
khi gi ng th v tr thp nht th li kim loi cch y cc thu tinh t

nht 25mm v ming cc ng thu tinh phi trn b mt cht lng.
Mt thit b ph hp duy tr nhit ca cht lng l 370C

0,50C.
5.3. Cch th
5.3.1. Chun b
- Cho mt th tch thch hp mi trng th (thng l nc) vo

cc.
- Vn hnh my iu nhit nhit ca mi trng th t 370C

0,50C.
- Cho vo mi ng th mt vin nn hoc mt vin nang ri y a

cht do vo tng ng.
5.3.2. Vn hnh thit b
hng gi ng ng th thit b vo trong cc ng cht lng v vn

hnh thit b theo thi gian quy nh.
5.3.3. nh gi kt qu
- Sau thi gian quy nh hoc khi thy cc vin r ht, ly gi

ng th ra khi cc cht lng.
- Mu th c coi l t yu cu v r khi khng cn cn, tr

nhng mnh v nang hoc v bao khng tan ca vin nn, cn li trn
mt li ca thit b th hoc dnh vo b mt di ca a y. u
cn cn th n ch l mt khi mm, khng c c nhn kh rn s thy
c.
Kt qu:
+ u c 6 vin u r ht: Mu th t yu cu v r.
+ u cn di hai vin cha r ht: h li trn 12 vin na.
Ch phm t yu cu v r khi 16 trong s 18 vin th t r

theo quy nh.
i vi vin nn khng bao thng thng thi gian r yu cu khng

qu 15 pht.
105
i vi vin nang thng thng thi gian r yu cu khng qu 30

pht.
5.3.4. Th r ca vin nn v vin nang bao tan rut
- in hnh theo cc bc nh trn. ing mi trng v thi gian

nh sau:
+ iai on 1: Mi trng th l acid hydrocloric 0,1M; trong 120

pht. t c cc vin th phi cn nguyn vn, khng th hin s gii
phng hot cht.
rong giai on ny, thng khng y a nha ln trn vin khi

th.
+ iai on 2: Mi trng th l dung dch m phosphat p = 6,8;

trong 60 pht.
u c vin dnh a th th li vi 6 vin khc khng dng a.
- nh gi kt qu: h i vi vin nn v vin nang thng.
Cch pha dung dch m phosphat pH 6,8: rn dung dch acid

hydrocloric 0,1 v dung dch natri phosphat 0,2 theo t l 3: 1. iu
chnh p n 6,8 0,05 bng dung dch acid hydrocloric 2 , hoc dung
dch natri hydroxyd 2 .
5.4. V d
5.4.1. nh gi r ca vin nang Cloxacilin 250mg
- Mi trng th: nc.
- hit : 370C 0,50C.
- Cho vo mi ng th mt vin nang Cloxacilin ri y a cht do

vo tng ng. h trn 6 vin.
- hi gian ti a: 30 pht.
- Quan st bng mt nu thy cc vin th r ht th ghi thi gian.
- Mu th c coi l t yu cu v r khi khng cn cn tr

nhng mnh v nang. u cn cn th n ch l mt khi mm, khng
c c nhn kh rn s thy c.
- Kt qu:
+ u c 6 vin u r ht: Mu th t yu cu v r.
106
+ u cn di hai vin cha r ht: h li trn 12 vin na. Ch

phm t yu cu v r khi 16 trong s 18 vin th t r theo quy
nh.
5.4.2. nh gi r ca vin bao tan trong rut Diclofenac 50mg
- rong 120 pht u trong mi trng acid hydrocloric 0,1M: Cho

vo mi ng th mt vin bao tan trong rut Diclofenac, khng y a
cht do. Sau thi gian quy nh, b dung dch acid hydrocloric 0,1M v
thay bng dung dch m phosphat p = 6,8.
- rong ti a 60 pht tip theo trong dung dch m phosphat p =

6,8: c y a cht do vo tng ng.
- hit : 370C 0,50C.
- h trn 6 vin.
- Mu th c coi l t yu cu v r khi khng cn cn, tr

nhng mnh v bao khng tan ca ch phm cn li trn mt li ca
thit b th hoc dnh vo b mt di ca a y. u cn cn th n
ch l mt khi mm, khng c c nhn kh rn s thy c.
- Kt qu:
+ Sau 120 pht trong mi trng acid hydrocloric 0,1M: t c cc

vin th phi cn nguyn vn, khng th hin s gii phng hot cht.
+ Sau ti a 60 pht trong mi trng m phosphat: Quan st bng

mt nu thy cc vin th r ht th ghi thi gian. t c cc vin th
phi r ht.
+ u cn di 2 vin khng t yu cu: h li trn 12 vin na.

Ch phm t yu cu v r khi 16 trong s 18 vin th t r
theo quy nh.
6. PHP TH HO TAN CA VIN NN V VIN NANG
6.1. Khi nim
ho tan ca mt ch phm l t l hot cht c gii phng ra

khi dng thuc theo thi gian vi cc iu kin quy nh trong tng
chuyn lun.
Vi mi ch phm c cc quy nh c th v thit b th, mi trng

ho tan, thi gian th nghim v phn trm hot cht c gii phng
(Ch s Q).
6.2. Thit b
107
u thit b c th c mt bnh hoc 6 - 8 bnh th.
6.2.1. Thit b kiu gi quay
hit b bao gm: (hnh 15).
Hnh 15. Thit b o ho tan ca vin nn, vin nang

(kch thc tnh bng mm)
Mt bnh hnh tr C bng thu tinh borosilicat hoc bng cht liu
trong sut thch hp, c y hnh bn cu v c dung tch 1000 ml (hnh
15A). Ming bnh c vin rng, c y bng np c mt s l nh,
trong c mt l tm ca np.
Mt ng c vi b phn iu tc c kh nng duy tr tc quay

ca gi trong phm vi 4% tc t. ng c ny gn vi mt b phn
khuy bao gm trc quay A v gi hnh ng tr B (hnh 15B). r kim loi
phi quay c mt cch nh nhng, khng b lc l nhiu trong khi
quay. B phn gi gm c 2 phn:
+ Phn np trn c mt l thot nh c gn vi trc. p ny

c lp 3 ci nhp n hi, hoc bng cch thch hp c th gi
chc chn phn di ca gi ng trc vi trc ca bnh trong khi quay
v c th tho phn di ra d dng khi cn cho ch phm th vo gi.
+ Phn di tho lp c l mt gi hnh ng tr c lm bng

vi ry kim loi, mp khu c hn lin, ng knh si dy l
0,254mm, c cnh hnh vung ca l ry l 0,381mm; gi hnh ng tr
ny c vnh kim loi bao quanh y trn v y di. i c th c
m mt lp vng kim loi
108
trng acid. Khong cch t gi n y trong ca bnh lun c gi

trong khong 23 - 27mm trong qu trnh th.
0
C
0
0,5 C.
6.2.2. Thit b kiu cnh khuy
hit b ny ging nh thit b gi quay m t trn, ch khc l gi

c thay bng cnh khuy D (hnh 15C v 15D). Cnh khuy c lp
t sao cho i qua tm ca trc v cnh di ca n ngang bng vi
mt y ca trc. rc cnh khuy c lp t v tr sao cho khng
lch qu 2mm so vi trc ca bnh v cnh y ca cnh khuy cch
mt y trong ca bnh t 23 - 27mm. hit b c vn hnh sao cho
cnh khuy quay trn mt cch nh nhng v khng c rung ng r
6.3. Cch th
6.3.1. Chun b mi trng ho tan
Mi trng ho tan c ch dn trong tng chuyn lun ring. u

l dung dch m th p phi iu chnh sai khc khng qu 0,05 n
Cho mt th tch quy nh mi trng ho tan ui kh vo bnh

(th tch quy nh 1%). Lm m mi trng ho tan n nhit 37
0,5o
6.3.2. Cho vin vo thit b th
u khng c ch dn g khc th th ng thi trn 6 vin, cho mi
- Khi dng thit b gi quay: cho vin nn hay vin nang vo trong gi
- Khi dng thit b kiu cnh khuy: cho vin nn hay vin nang chm
xung y bnh trc khi cho cnh khuy quay; c th dng mt dy
xon bng kim loi hay thu tinh gi cho vin thuc nm ngang di
y bnh. Cn loi tr bt khng kh khi b mt vin.
6.3.3. Vn hnh thit b
Vn hnh thit b ngay tc quay c ch dn trong chuyn lun

ring.
6.3.4. Ly mu lc mu
109
u theo ch dn chuyn lun m ly mu ra th pht th 45

hoc sau nhng khong thi gian quy nh, hoc ly mu ra lin tc; cho
php chnh lch so vi thi gian quy nh l 2%. V tr ht mu
khong gia b mt mi trng ho tan v mt trn ca gi quay hay
cnh trn ca cnh khuy, im ny phi cch thnh bnh t nht 10mm.
r trng hp phn tch mu lin tc, o mu t ng khi mu ly
ra sau khi phn tch li tr v bnh ho tan, cng nh trong trng hp
ly mu phn tch mt ln; cn cc trng hp khc phi thm mt th
tch mi trng ho tan bng th tch mu th ly nhit 37
0,5oC, hoc c th dng php tnh hiu chnh. Lc mi trng ho tan
qua giy lc c ng knh l lc thch hp.
6.3.5. Xc nh lng hot cht
Xc nh lng hot cht cha trong dch lc bng phng php

c ch dn trong chuyn lun ring.
6.3.6. nh gi kt qu
- Phn trm dc cht gii phng so vi hm lng ghi trn nhn
- u v vin nang nh hng ti kt qu phn tch, ly t nht 6

vin nang, loi b ton b thuc trong nang, ho tan v nang rng trong
mt th tch mi trng ho tan c ch dn trong chuyn lun ri tnh
hiu chnh. s hiu chnh khng c ln hn 25% hm lng ghi
Bng 7. Gii hn v phn trm dc cht gii phng i vi vin

nn, vin nang
(Theo USP 24)
S Yu cu kt qu
Ln vin (Phn trm hot cht ho Kt lun - Gii php
th tan)
1 6 - t: Mu th t yu cu
v ho tan. Dng th
nghim.
- Khng t. Lm ln 2.
2 6 rung bnh ca 12 vin - t: Mu th t yu cu

v ho tan. Dng th
no < Q - 15% nghim.
- Khng t. Lm ln 3.
3 12 rung bnh ca 24 vin - t: Mu th t yu cu
110
v ho tan.
vin < Q - 15% v khng
c vin no < Q - 25% - Khng t: Mu th khng
t yu cu v ho tan.
6.4. Th tc ho tan ca vin nn v vin nang bao tan rut
- in hnh cc bc nh trn. ing mi trng v thi gian nh
+ iai on 1: dng 1000 ml dung dch acid hydrocloric 0,1 M lm

cht lng. h trong 2 gi.
+ iai on 2: 1000 ml dung dch m phosphat p 6,8. h trong
+ rong mi trng m p 6,
Bng 8. Gii hn v phn trm dc cht gii phng i vi vin

bao, vin nang tan trong rut
(mi trng th l Cl 0,1M) ( heo USP 24)
S Yu cu kt qu
Ln vin (Phn trm hot cht Kt lun - Gii php
th ho tan)
1 6 Khng c vin no vt - t: Mu th t yu cu. Dng

10% so vi hm lng th nghim.
ghi trn nhn.
- Khng t. Lm ln 2.
2 6 rung bnh ca 12 vin - t: Mu th t yu cu. Dng

phi nh hn 10% so vi th nghim.
hm lng ghi trn
nhn. - Khng t. Lm ln 3.
3 12 rung bnh ca 24 vin - t: Mu th t yu cu.

phi nh hn 10% so vi
hm lng ghi trn - Khng t: Mu th khng t
nhn. yu cu v ho tan.
6.5. V d
111
6.5.1. nh gi ho tan ca vin nang Cephalexin (DVN III)
b: i quay.
ml nc.
dch lc bng nc c dung dch cephalexin c nng khong

ml.
o hp th ca dung dch thu c bc sng 262nm vi mu

trng l nc.
Song song lm mt mu chun cephalexin c cng nng .
Yu cu: Khng c t hn 80% lng cephalexin (C 16H17N3O4S)

ghi trn nhn c ho tan trong 45 pht.
6.5.2. nh gi ho tan ca vin bao Ibuprofen (DVN III)
ml dung dch m phosphat p 7,2 (Phi

hp 250 ml dung dch K 2PO4 0,2 M vi 175 ml dung dch a 0,2 M,
thm nc va 1000 ml).
60 pht.
Ly mu v x l mu: Lc dung dch sau khi ho tan. Pha long

dch lc vi dung dch m phosphat p 7,2 c dung dch
ibuprofen c nng thch hp.
o hp th ca dung dch thu c bc sng 221nm trong

cuvet thch anh c chiu dy 1cm vi mu trng l dung dch m
phosphat pH 7,2.
nh hm lng ibuprofen theo A (1%, 1cm) l 449 bc sng

221nm.
Yu cu: Khng c t hn 85% lng ibuprofen (C 13H18O2) ghi

trn nhn c ho tan trong 60 pht.
T LNG GI V BI TP
112
1. Hy nu cc phng php xc nh t trng d20 ca cht lng.
2. rnh by khi nim v ch s khc x.
3. rnh by s tng qut v nguyn tc hot ng ca my o

gc quay cc.
4. rnh by cch tin hnh v tnh kt qu o nng sut quay cc

ca cht lng v cht rn.
5. rnh by khi nim, cch xc nh nhit nng chy, khong

nng chy ca cht rn.
6. Phn bit khi nim r v ho tan ca vin nn, vin nang.
7. rnh by cch tin hnh v nh gi kt qu th r ca vin

nang Cloxacilin 500mg?
8. rnh by cch tin hnh v nh gi kt qu th r ca vin

nang bao tan trong rut omeprazol 20mg?
9. gi ta xc nh t trng 200C ca xir ho bng picnomet, kt

qu thu c nh sau:
- Khi lng ca picnomet 10,0625g.
- Khi lng ca picnomet cha y xir: 21,4280g.
- Khi lng ca picnomet cha y nc: 20,0831g.
y tnh t trng ca ch phm.
10. nh gc quay cc ring ca mt tinh du, bit rng gc quay

cc l +1,23 o trong ng o c chiu di 1dm v tinh du c t
trng l 0,8437.
11. nh gc quay cc ring ca cloramphenicol, bit rng gc quay

cc ca dung dch 6,032% c chun b t ch phm l +2,64
o trong ng o c chiu di 2,2dm.
Chn cu tr li ng cho cc cu hi t 12 v 13 bng cch khoanh

12. heo quy nh:
a) h r phi th trn s vin l:
A. 4 B. 5 C. 6 D. 7
113
b) Yu cu v r i vi vin nn khng bao l khng qu:
A. 14 pht B. 15 pht
C. 16 pht D. 17 pht
c) Yu cu v r i vi vin nang thng l khng qu:
A. 20 pht B. 30 pht
C. 35 pht D. 25 pht
13. heo quy nh:
a) Khi th ho tan ca vin nn, vin nang, mi trng ho

tan l dung dch m th p phi iu chnh sai khc khng
qu:
A. 0,02 n v B. 0,10 n v
C. 0,05 n v D. 0,07 n v
b) Khi th ho tan ca vin nn, vin nang, thi gian ly mu

cho php chnh lch so vi thi gian quy nh l:
A. 1% B. 3%
C. 4% D. 2%
14. Vit cm t cn thiu vo ch trng trong cu sau:
a) ho tan ca vin nn, vin nang l t l hot cht c

................... ra khi dng thuc theo thi gian vi cc iu
kin quy nh trong tng chuyn lun.
b) r ca vin nn, vin nang l kh

nng.................................... ca chng trong mi trng th
theo quy nh.
114
Bi 8
KIM NGHIM THUC BT, THUC CM
MC TIU
- Trnh by c cc yu cu k thut v phng php th nh

gi cht lng thuc bt, thuc cm.
- Gii thch v nh gi c kt qu kim nghim i vi mt mu

kim nghim thnh phm c th ca cc dng bo ch trn.
- Trnh by c v d v kim nghim cc dng bo ch thuc bt.
1. KIM NGHIM THUC BT
1.1. Khi nim
huc bt l dng thuc rn, kh ti, ung, tim hoc dng ngoi,
c bo ch t mt hay nhiu loi bt thuc c kch thc xc nh,
bng cch trn u thnh hn hp ng nht.
1.2. Yu cu k thut v phng php th
1.2.1. Cm quan
theo tng loi ch phm ca cc nh sn xut.
- Cch th: ri mt lng bt va thnh mt lp mng trn mt

t giy trng mn. Quan st mu sc bng mt thng, di nh sng t
nhin.
- nh gi: Ch phm t yu cu nu t nh m t.
1.2.2. m
ch dn khc.
+ u theo tng ch phm m c yu cu s dng phng php xc

nh m khc nhau nh: Sy trong t sy p sut thng, sy p
sut gim, lm kh trong bnh ht m vi nhng cht ht nc mnh
nh acid sulfuric m c,...
115
+ xc nh m ca ch phm thuc bt, ngi ta dng hp

lng thu tinh hoc chn cn c np mi lm b ng mu th. B c
lm kh trong 30 pht theo phng php v iu kin quy nh ca
chuyn lun, ngui trong bnh ht m, sau cn xc nh khi
lng. Cn ngay vo b mt khi lng chnh xc mu th theo quy nh
trong chuyn lun. Mu th c dn thnh lp mng c dy khng
qu 5mm. u mu th c kch thc ln th nghin nhanh trc khi
cn. in hnh lm kh trong iu kin quy nh vi cng dng c
lm kh b. Sau khong thi gian quy nh, ly chn cn ra, ngui ti
nhit phng trong bnh ht m, ri cn ngay.
1.2.3. mn
theo tng ch phm.
Php th ny thng c dng cho tt c cc thuc bt kp, cc

thuc bt dng p, thuc bt dng pha ch thuc dng cho mt,
tai.
Cc c bt c quy nh da vo cc s ca ry.
Cch th: Chn c ry thch hp theo quy nh ca tiu chun.

Cn mt lng thuc bt, em ry qua ry c c quy nh.
+ i vi bt th hoc na th: ly 25g -100g bt. Cho vo ry thch

hp, lc ry theo chiu ngang quay trn t nht 20 pht v ry ti khi
xong. Cn chnh xc s lng cn li trn ry v s thu c trong
hp hng.
+ i vi bt na mn, mn hay rt mn: ly khng qu 25g bt, cho

vo ry thch hp, lc ry theo chiu ngang quay trn t nht 30 pht ri
ry ti khi xong. Cn chnh xc s lng cn li trn ry v s thu
c trong hp hng.
+ i vi cht c du hay bt c xu hng bt mt ry th trong qu

trnh ry thnh thong chi cn thn mt ry, tch ri nhng ng t li
khi ry.
+ Khi quy nh dng mt ry xc nh c bt th khng c c

di 97% khi lng thuc bt qua c c ry .
+ Khi quy nh dng 2 ry xc nh c bt th ry c s ry cao

hn ln trn ry c s ry thp hn v tin hnh ry; khng c c
di 95% khi lng thuc bt qua ry c s ry cao hn v khng
c qu 40% khi lng thuc bt qua ry c s ry thp hn.
116
Quy nh s dng c ry xc nh mn ca thuc bt c

trnh by bng 9.
Bng 9. Quy nh c ry xc nh mn ca thuc bt
C bt Dng 1 ry Dng 2 ry
- Bt th 1400 1400/355
- Bt na th 710 710/250
- Bt na mn 355 355/180
- Bt mn 180 180/125
- Bt rt mn 125 125/90
V d:
kim tra mn ca bt st trng A c yu cu l bt mn, dng 2

ry s 180 v 125. gi ta lm nh sau: ry s 180 ln trn ry s
125, cho 10,0027g ch phm ln ry s 180 v tin hnh ry. Lng bt
qua ry s 180 l 9,6703g; ton b bt qua ry s 180 c ry qua ry
s 125 v lng bt qua ry s 125 l 3,5935 g.
Lng ch phm (%) qua ry s cao hn l:
Lng ch phm (%) qua ry s thp hn l:
a thy, lng ch phm qua ry c c ry cao hn l 96,68% >

95% v lng ch phm qua ry c c ry nh hn l 35,93% < 40%,
do ch phm t yu cu v mn.
1.2.4. ng u khi lng
phi th ng u khi lng. ing thuc bt pha tim hoc

truyn tnh mch, nu khi lng nh hn hoc bng 40 mg th khng
phi th ng u khi lng nhng phi t yu cu ng u
hm lng.
117
c ly bt k. Khi lng thuc phi nm trong gii hn cho php

theo bng 10.
t c cc n v phi t quy nh trong bng.
u c mt n v c khi lng lch ra ngoi quy nh ny th th

li vi 5 n v khc, nu ln th li c qu mt n v khng t th l
thuc khng t yu cu.
Bng 10. Gii hn cho php chnh lch khi lng i vi thuc
bt
Khi lng ghi trn nhn Chnh lch cho php

(%)
Di hoc bng 0,50g 10
Trn 0,50 - 1,50g 7
Trn 1,50 - 6,00g 5
Trn 6,00g 3
i vi cc ch phm ng gi trong hp, l th sau khi cn c v

phi b ht thuc ra, dng bng lau sch thuc, cn v ri tnh theo
lng thuc trong tng hp hoc l.
chnh lch c tnh theo t l phn trm so vi khi lng trung

bnh bt thuc trong mt n v ng gi.
1.2.5. ng u hm lng
r khi c ch dn khc, php th ny p dng cho cc thuc bt

ung, tim c trnh by trong cc n v ng gi mt liu c cha
mt hoc nhiu hot cht, trong c cc hot cht c hm lng di
2mg hoc di 2% (KL/KL) so vi khi lng thuc mt liu.
Php th ng u hm lng c tin hnh sau php th nh

lng v hm lng hot cht trong gii hn quy nh.
Cch th: ly 10 n v ng gi nh nht bt k, xc nh hm

lng hot cht tng gi theo phng php nh lng ch dn trong
chuyn lun.
+ Ch phm em kim tra t yu cu php th nu khng qu mt

n v c gi tr hm lng nm ngoi gii hn 85 - 115% ca hm
118
lng trung bnh v khng c n v no nm ngoi gii hn 75 - 125%

ca hm lng trung bnh.
+ Ch phm khng t yu cu php th nu qu 3 n v c gi tr

hm lng nm ngoi gii hn 85 - 115% ca hm lng trung bnh,
hoc 1 n v tr ln nm ngoi gii hn 75 - 125% ca hm lng.
+ u hai hoc ba n v c gi tr hm lng nm ngoi gii hn 85

- 115% nhng trong gii hn 75 - 125% ca hm lng trung bnh th
th li trn 20 n v khc, ly ngu nhin. Ch phm t yu cu, nu
khng qu 3 n v trong tng s 30 n v em th c gi tr hm lng
nm ngoi gii hn 85 - 115% ca hm lng trung bnh v khng c
n v no c gi tr hm lng nm ngoi gii hn 75 - 125% ca hm
lng trung bnh.
1.2.6. nh tnh
in hnh nh tnh theo cc phng php c quy nh trong tiu

chun, thuc bt phi cho cc phn ng ca cc hot cht c trong ch
phm.
1.2.7. nh lng
Ly thuc ca 5 n v ng gi nh nht bt k, trn u. in hnh

nh lng theo cc phng php c quy nh trong tiu chun, hm
lng ca tng hot cht trong ch phm phi nm trong gii hn cho
php theo bng 11.
Bng 11. Gii hn cho php v hm lng hot cht i vi thuc

bt, thuc cm
Lng ghi trn nhn Chnh lch cho php (%)
i 100mg 15
rn 100mg ti 1g 10
rn 1g n 5g 5
Trn 5g 1
1.2.8. Gii hn nhim khun
nhim khun".
nh gi theo " h gii hn nhim

khun" mc 2, bi 13.
119
1.3. Cc loi thuc bt
1.3.1. Thuc bt ung
ca thuc bt.
huc bt si bt phi t thm yu cu v tan.
ng thuc bt tng ng vi mt liu vo

mt cc thu tinh c cha 200 ml nc nhit 15 - 20oC, xut hin
nhiu bt kh bay ra. Khi ht bt kh bay ra, thuc phi tan hon ton.
h nh vy vi 6 liu n. Mu th t yu cu nu mi liu th u
tan trong vng 5 pht, tr khi c ch dn ring.
1.3.2. Thuc bt dng ngoi
huc bt dng ngoi phi p ng cc yu cu cht lng chung

ca thuc bt. goi ra, phi t cc yu cu ring sau:
- v khun: huc bt p, dng cho vt thng rng hoc

trn da b tn thng nng, thuc bt dng cho mt phi v khun.

mc 3, bi 13.
1.3.3. Thuc bt pha tim
thuc bt v yu cu i vi thuc tim, thuc tim truyn dng bt nh:

v khun, cht gy st,...
2. KIM NGHIM THUC CM
2.1. Khi nim
huc cm l ch phm c dng ht nh xp hay si ngn xp,

thng dng ung, nhai, hay pha vo nc hay mt cht lng thch
hp hoc pha thnh dung dch, hn dch hay xir.
2.2.1. Cm quan
dng v mu sc, khng c hin tng ht m, b mm v bin mu.
120
- Cch th: ri mt lng bt va thnh mt lp mng trn mt

t giy trng mn. Quan st mu sc bng mt thng, di nh sng t
nhin.
nh gi: Ch phm t yu cu nu t nh m t.
2.2.2. m
g c cha hm lng nc qu 5,0%, tr

ch dn khc.
+ a s cc thuc cm: s dng phng php lm kh (Dc in

Vit am Ph lc 5.16).
+ i vi thuc cm cha tinh du: th bng phng php ct vi

dung mi (Dc in Vit am II - Ph lc 9.6).
2.2.3. Kch thc ht - t l vn nt
u khng c ch dn ring trong chuyn lun, cn thuc ca 5 n

v ng gi nh nht bt k. y qua ry s 2000 v ry s 250. on b
cm phi qua ry s 2000. l vn nt qua ry s 250 khng qu 8%
2.2.4. ng u khi lng
k. Khi lng thuc phi nm trong gii hn 5% so vi khi lng ghi

trn nhn.
i quy nh ny th th
2.2.5. ng u hm lng
ng gi mt liu, c cha mt hoc nhiu hot cht, trong c cc

hot cht c hm lng di 2mg hoc di 2% (KL/KL) so vi khi
nh trong php th nh lng. u theo yu cu c th ca ch phm

dng n liu m quy nh th ng u hm lng trong chuyn
121
lng hot cht tng gi theo phng php nh lng ch dn trong
2.2.6. Xc nh tnh ho tan
hm 20 phn nc nng vo 1 phn thuc cm, khuy trong 5

pht. i vi loi thuc cm tan, phi hon ton tan ht. i vi dng
thuc cm dng treo phi l lng u trong nc, khng c c nhng
cht l ca n
2.2.7. nh tnh

chun, thuc cm phi cho cc phn ng ca cc hot cht c trong ch
2.2.8. nh lng

T LNG GI V BI TP
1. rnh by tiu chun v k thut kim nghim chung ca thuc

bt.

cm.

3. y la chn ry khi tin hnh xc nh mn trong trng hp

dng 1 ry ca bt c yu cu v mn nh sau:
a) Bt th
A. 2000 B. 355 C. 710 D.

1400
b) Bt na th
A. 180 B. 355 C. 710 D.

1400
122
c) Bt na mn
A. 1400 B. 125 C. 710 D.

355
4. y la chn ry khi tin hnh xc nh mn trong trng hp

dng 2 ry ca bt c yu cu v mn nh sau:
a) Bt mn
A. 125/90 B. 710/250 C. 180/125 D.

355/180
b) Bt rt mn
A. 125/90 B. 710/250 C. 180/125 D.

355/180
5. Quy nh gii hn cho php v chnh lch khi lng ca ch

phm thuc bt c ng gi nh sau:
a) Bt cam cc 15g
A. 10% B. 3% C. 7% D.
5%
b) Biosubtin 1g
A. 10% B. 7% C. 3% D.
5%
c) Augmentin 0,5g
A. 10% B. 12% C. 8% D.
5%
d) Magnesi sulfat 5g
A. 10% B. 6% C. 8% D.
5%
6. Quy nh gii hn cho php v chnh lch hm lng ca ch

phm thuc cm so vi hm lng ghi trn nhn nh sau:
a) huc cm c cha hot cht paracetamol 325mg trong 1 gi:
A. 10% B. 12% C. 8% D.
15%
123
b) huc cm c cha hot cht acid clavulanic 62,5mg trong 1

gi:
A. 10% B. 12% C. 8% D.
15%
7. huc cm h st tr em ng gi 5g c t tiu chun v

ng u khi lng khng? Bit rng khi cn 5 gi ring bit
c kt qu:
5,2030g; 4,9674g; 5,0923g;

4,7645g;
4,8845 g.
Bi 9
KIM NGHIM THUC VIN NANG,VIN NN
MC TIU

gi cht lng thuc vin nang, vin nn.

- Trnh by c v d v kim nghim cc dng bo ch thuc vin

nang, vin nn.
1. KIM NGHIM THUC VIN NANG
1.1. Khi nim
Vin nang l dng thuc ung cha mt hay nhiu hot cht trong v
nang cng hay mm vi nhiu kiu dng v kch thc khc nhau. V
nang c lm t gelatin v c th c thm cc ph gia khng gy
c hi cho c th. huc cha trong nang c th l dng rn, lng hay
1.2.1. Tnh cht
ang mm cha bt, hoc cm, hoc cht lng.
124
1.2.2. ng u khi lng
Cn khi lng ca mt nang, vi vin nang cng th tho ri hai

na v nang thuc ra, dng bng lau sch v ri cn khi lng ca
v; vi vin nang mm, ct m nang, bp thuc ra ht ri dng ether
hoc dung mi hu c thch hp ra sch v nang, kh t nhin ti
khi ht mi dung mi, cn khi lng v. Khi lng thuc trong nang l
hiu gia khi lng nang thuc v v nang. Lm nh vy vi 19 nang
khc c ly bt k. chnh lch khi lng ca tng vin vi khi
Bng 12. Gii hn cho php chnh lch khi lng i vi vin
nang
Khi lng trung bnh nang Chnh lch cho php

(%)
h hn 300mg 10
Ln hn hoc bng 300mg 7,5
u c yu cu th ng u hm lng th khng phi th
1.2.3. ng u hm lng
Dng ton b bt thuc ca ring tng vin nang, tin hnh th v

nh gi nh i vi thuc bt phn 1.2.5, mc 1.2, bi 8 ( ng
1.2.4. r
u khng c quy nh ring th tin hnh th v nh gi theo

"Php th r vin nn v vin nang"
1.2.5. ho tan
vin nang"
1.2.6. nh tnh
125

chun, vin nang phi cho cc phn ng ca cc hot cht c trong ch
1.2.7. nh lng
Xc nh khi lng trung bnh vin, dng 20 vin (cn c vin, b

thuc ra v lau sch v nang, cn v nang), lm ng nht bng cch
nghin i vi vin nang cha bt; cm hoc trn u i vi nang cha
cht lng. in hnh nh lng theo cc phng php c quy nh
trong tiu chun, hm lng ca tng hot cht trong ch phm phi
nm trong gii hn cho php
1.2.8. Tp cht (nu c)
Bng 13. Gii hn cho php v hm lng i vi thuc vin nang,

vin nn
Lng ghi trn nhn Chnh lch cho php (%)
i 50mg 10
rn 50mg ti 100mg 7,5
Trn 100mg 5
1.3. Cc loi vin nang
iu chun cht lng ca cc loi vin nang phi tun theo yu cu
1.3.1. Thuc nang cng
huc nang cng c v nang gm hai phn hnh tr lng kht vo

nhau, mi phn c mt u kn, u kia h. huc ng trong nang
V d:
1.3.2. Thuc nang mm
huc nang mm c v nang l mt khi mm vi cc hnh dng

khc nhau. huc ng trong nang thng dng dung dch, hn dch
126
V d:
1.3.3. Thuc nang tan trong rut
huc nang tan trong rut l cc nang cng hoc nang mm c v

nang bn vng vi dch d dy, ch tan trong dch rut; hoc cc nang c
ng cm c bao lp ch tan trong dch rut.
V d:
1.4. V d
Vin nang amoxicilin l nang cng c cha amoxicilin trihydrat. Ch
m lng amoxicilin C16H19N3O5S t 92,5 n 110,0% so vi lng

ghi trn nhn (tnh theo loi khan).
a) Yu cu k thut v cht lng thnh phm
Ch tiu Yu cu Phng php th
1. nh cht ang cng, bt thuc trong Cm quan.

nang mu trng ng, khng
mi hay gn nh khng mi.
2. nh tnh Amoxicilin. heo chuyn lun ring.
3. ng Khi lng trung bnh 7,5%. heo chuyn lun chung.

u khi
lng
4. c Khng qu 14,5%. Phng php Karl

Fisher.
5. ho tan Khng c t hn 70,0% heo chuyn lun ring.

amoxicilin C16H19N3O5S so vi
lng ghi trn nhn c ho
tan sau 60 pht.
6. nh lng m lng amoxicilin heo chuyn lun ring.
C16H19N3O5S phi t 92,5 n
110,0% so vi lng ghi trn
nhn (tnh theo loi khan).
127
b) Thuc th (theo DVN III)
Cch pha cc dung dch sau c tin hnh nh ch dn phn

thuc th.
- Dung dch natri hydroxyd 1 .
- Dung dch acid hydrocloric 1 .
- Dung dch ninhydrin 0,3% trong ethanol: o tan 0,3g ninhydrin

trong ethanol v thm ethanol va 100 ml.
- Dung dch formaldehyd trong acid sulfuric: o tan 0,2g

formaldehyd trong 10 ml acid sulfuric m c.
- Dung dch iod 0,01 : o tan 13g iod tinh th vo mt dung dch
cha 20g kali iodid trong 50 ml nc. Pha long vi nc va 1 lt.
Pha long 10 ml dung dch ny thnh 100 ml bng nc.
- Dung dch natri thiosulfat 0,01 : o tan 26g natri thiosulfat v 0,1g
natri carbonat trong nc khng c carbon dioxyd va 1 lt. Pha
long vi nc va 1 lt. Pha long 10 ml dung dch ny thnh 100 ml
bng nc.
- Dung dch amoxicilin chun 1mg/ ml (CC): Cn chnh xc mt lng

amoxicilin trihydrat chun tng ng khong 100mg amoxicilin v cho
vo bnh nh mc 100 ml. o tan v thm nc va 100 ml.
c) Phng php th
nh tnh:
+ Bn mng Silicagelg dy khong 0,25mm, hot ho 100 0C trong

1 gi.
+ dung mi khai trin: Aceton nc toluen acid acetic bng

(65 : 10 : 10: 2,5)
+ Dung dch th: Lc mt lng bt vin tng ng 100mg

amoxicilin trong 20 ml hn hp gm aceton acid hydrocloric 0,1N (4 :
1). Lc.
+ Dung dch chun: o tan 50mg amoxicilin (cht i chiu) trong

10 ml hn hp gm aceton acid hydrocloric 0,1N (4 : 1).
bn mng. rin khai sc k n khi dung mi i c khong 15cm, ly
128
bn mng ra, kh nhit phng. Phun dung dch ninhydrin 0,3%

trong ethanol, ri sy 900C trong 15 pht.
rn sc k , vt ca dung dch th v ca dung dch chun phi

ging nhau v mu sc v gi tr f.
vi 2 ml nc trong 5 pht, lc. a cn lc u vi ethanol, sau vi

ether. Ly khong 2mg cn thu c vo mt ng nghim, lm m bng
0,05 ml nc v thm 2 ml dung dch formaldehyd trong acid sulfuric.
Lc u. Dung dch thu c khng mu. un trong cch thu mt pht,
xut hin mu vng sm.
Nc:
Khng qu 14,5%. Phng php Karl Fisher, dng khong 0,100g

bt thuc
ho tan
ml nc.
pht.
ml dch lc
u, pha long nu cn. o hp th bc sng 272nm (Ph lc 3.1
dung dch amoxicilin trihydrat chun trong nc c nng tng

ng.
Yu cu: Khng c t hn 70,0% amoxicilin C16H19N3O5S so vi

lng ghi trn nhn c ho tan sau 60 pht.
nh lng:
Amoxicilin trong ch phm c nh lng bng phng php o

iod, nhit 25 20C. Cch tin hnh nh sau:
- Dung dch th: Cn 20 nang, tnh khi lng trung bnh thuc trong
nang mTB (mg), nghin mn. Cn chnh xc mt lng bt thuc mT (mg)
tng ng vi khong 100mg amoxicilin, ho tan trong nc va 100
ml. Lc k, lc, b khong 20 ml dch lc u. Ly chnh xc 2,00 ml
dung dch th cho vo bnh nn nt mi c dung tch 100 ml, thm 2,0 ml
dung dch natri hydroxyd 1 , lc u, yn 15 pht. hm 2,4 ml dung
dch acid hydrocloric 1 v 10,0 ml dung dch iod 0,01 , y ngay nt
129
bnh. yn 15 pht, chun iod tha bng dung dch natri thiosulfat
0,01 n khi dung dch c mu vng. hm 2 git ch th h tinh bt v
chun tip n khi mt mu. hi vT ml.
Ly chnh xc 2,00 ml dung dch th cho vo bnh nn nt mi khc

c dung tch 100 ml, thm 0,12 ml dung dch acid hydrocloric 1 v 10,0
ml dung dch iod 0,01 . Chun ngay bng dung dch natri thiosulfat
0,01 n khi dung dch c mu vng. hm 2 git ch th h tinh bt v
chun tip n khi mt mu. hi VT ml.
- Dung dch chun: Cn chnh xc Ag amoxicilin trihydrat chun

tng ng khong 100mg amoxicilin ho tan trong nc va 100 ml.
2,00 ml,... h tch dung dch natri thiosulfat 0,01 dng cho mu chun
l vC ml v mu trng l VC ml.
m lng amoxicilin (%) so vi lng ghi trn nhn c tnh theo

cng thc:
rong : C l lng (g) amoxicilin c trong 100g amoxicilin chun.
B l lng (g) nc c trong 100g amoxicilin trihydrat

chun.
D l lng (g) amoxicilin trong mt nang theo nhn.
2. KIM NGHIM THUC VIN NN
2.1. Khi nim
Vin nn l ch phm rn dng ung, nut hoc nhai, c th ho

vi nc trc khi ung hoc ngm trong ming. Mi vin cha mt liu
ca mt hay nhiu hot cht, c iu ch bng cch nn nhiu khi
ht nh ng u ca cc cht.
2.2.1. Tnh cht
Vin nn thng c dng hnh tr dt, hai y phng hoc cong, c

th khc ch, k hiu hoc rnh. Cnh v thnh vin lnh ln. Mu sc
ng nht.
Cch th: Bng cm quan.
130
2.2.2. r

"Php th r vin nn v vin nang" mc 5, bi 7.
Vin khng cn th r khi php th ho tan c thc hin.
2.2.3. ng u khi lng
Cn chnh xc 20 vin bt k v xc nh khi lng trung bnh ca

vin. Cn ring khi lng tng vin v so snh vi khi lng trung
bnh, tnh lch theo t l phn trm ca khi lng trung bnh, t
tnh ra khong gii hn ca gi tr trung bnh. Khng c qu 2 vin c
khi lng chnh lch qu khong gii hn ca khi lng trung bnh v
khng c c vin no c chnh lch qu gp i lch tnh theo t
l phn trm, theo bng 14.
Bng 14. Gii hn cho php chnh lch khi lng i vi vin nn
Khi lng trung bnh vin Chnh lch cho php

(%)
i 80mg 10
rn 80mg n 250mg 7,5
Trn 250mg 5
u c yu cu th ng u hm lng th khng phi th

ng u khi lng.
V d: h ng u khi lng ca vin nn vitamin C 100mg.

Kt qu thu c nh sau:
124,0 mg 109,6mg 116,2mg

120,1mg 118,0mg
107,8mg 116,9mg 122,3mg

114,5mg 120,3mg
119,4mg 109,2mg 117,2mg

112,6mg 111,9mg
115,3mg 120,8mg 118,3mg

113,9mg 116,1mg
Khi lng trung bnh
131
ii hn cho php mTB 7,5% tc l khi lng vin nm trong

khong: 107,5 124,9mg.
kt qu thu c trn ta thy ch phm t yu cu v ch tiu

ng u khi lng.
2.2.4. ng u hm lng
in hnh th trn 10 vin, ring tng vin v nh gi nh i vi

thuc bt phn 1.2.5, mc 1.2, bi 8 ( ng u hm lng).
2.2.5. ho tan
Ch thc hin khi c yu cu c ch dn trong chuyn lun ring.

"Php th ho tan ca vin nn v vin nang" (mc 6, bi 7).
2.2.6. nh tnh

chun, vin nn phi cho cc phn ng ca cc hot cht c trong ch
phm.
2.2.7. nh lng
Cn 20 vin, xc nh khi lng trung bnh vin. ghin mn. in

hnh nh lng theo cc phng php c quy nh trong tiu chun,
hm lng ca tng hot cht trong ch phm phi nm trong gii hn
cho php, theo bng 12.
2.2.8. Tp cht (nu c)
Khi c yu cu s ch dn trong chuyn lun ring.
2.3. Cc loi vin nn
iu chun cht lng ca cc loi vin nn phi tun theo yu cu

chung ca thuc vin nn v yu cu ring i vi tu tng loi.
2.3.1. Vin nn khng bao
m cc vin nn c bo ch bng cch nn cc ht gm dc

cht, t dc. Vin nn loi ny khng cha mt thnh phn no thay
i s gii phng hot cht trong ng tiu ho. Khi b gy vin nn
mt lp v quan st bng knh lp th thy ng nht, khng c lp bao
ngoi.
V d: Vin nn Acid ascorbic 100mg.
132
Vin nn Paracetamol 500mg.
2.3.2. Vin bao
Vin bao c b mt nhn, thng c mu, c nh bng. Ly mt

phn vin b gy, quan st di knh lp, thy r nhn c bao
bng mt lp hay nhiu lp.
V d: Vin nn Ospen 500mg.
Vin nn Cimetidin 400mg.
2.3.3. Vin bao bn vi dch v d dy
Vin c bao bng lp bao bn vi dch v d dy nhng li tan

c trong dch rut do s dng cc cht bao l cellacephate (cellulose
acetat phtalate) v cc polymer.
V d: Vin nn Aspirin pH 8.500mg.
Vin nn Diclofenac 50mg.
2.3.4. Vin nn si bt
L vin nn khng bao c cha cc acid v carbonat hoc

hydrocarbonat, chng phn ng vi nhau rt nhanh khi c mt ca nc
v gii phng C 2, ng thi ho tan hay phn tn hot cht trong nc
trc khi dng.
V d: Vin nn Efferalgan vitamin C.
Vin nn Plusssz multivitamin.
2.3.5. Vin ngm
Vin ngm thng l vin nn khng bao c iu ch cc

thnh phn v hot cht gii phng dn v tc dng ti ch, gii phng
v hp th di li hoc cc phn khc trong ming.
V d: Vin nn Adalat 5mg.
- Chymotrypsin.
2.3.6. Vin nn tan trong nc
Vin nn tan trong nc l vin nn khng bao, ho tan trong nc.

Dung dch to thnh c th hi c nh.
V d: Vin nn hydrite.
133
2.3.7. Vin nn thay i gii phng hot cht
hng l vin bao hoc khng bao, c iu ch bng cch thm

cc t dc c bit hoc iu ch theo phng php c bit nhm
thay i tc gii phng hoc v tr gii phng ca thuc.
Vin nn thay i gii phng hot cht thng khng yu cu th

r m phi th ho tan.
V d: Vin nn Profenid LP 200mg.
Vin nn Diamicron MR 30mg.
2.4. V d
L vin nn cha acid acetylsalicylic
Ch phm phi p ng cc yu cu chung i vi " huc vin nn"

v cc yu cu ring ca ch phm.
m lng ca acid acetylsalicylic (C9H8O4) t 95,0 n 105,0% so

vi lng ghi trn nhn.

1. nh cht Vin mu trng. Cm quan.
2. nh tnh Acid acetylsalicylic. heo chuyn lun

ring.
3. ng Khi lng trung bnh 5%. heo chuyn lun

u khi chung.
lng
4. ho tan Khng c t hn 70% lng heo chuyn lun

acid acetylsalicylic C9H8O4 so ring.
vi lng ghi trn nhn c
ho tan trong 45 pht.
5. ii hn Khng c qu 0,3%. heo chuyn lun

acid salicylic ring.
t do
6. nh lng m lng ca acid heo chuyn lun
acetylsalicylic (C9H8O4) t 95,0 ring.
n 105,0% so vi lng ghi
134
trn nhn.

thuc th bi 4 v Ph lc 2.8 DV .
- Dung dch natri hydroxyd 10%.
- Dung dch acid sulfuric 10%.
- Dung dch st ( ) clorid 0,5%.
- Natri acetat.
- Acid acetic bng.
- Ethanol 96%.
- Dung dch phn st amoni 0,2%.
- Dung dch chun natri hydroxyd 0,5 .
- Dung dch chun acid hydrocloric 0,5 .
- Dung dch ch th phenol.
c) Phng php th
nh tnh:
un si 0,3g bt vin trong 2 n 3 pht vi 10 ml dung dch natri

hydroxyd 10% ( ). ngui, thm dung dch acid sulfuric 10% (TT) cho
n khi tha acid, s c ta kt tinh v c mi acid acetic. hm 1 ml
dung dch st ( ) clorid 0,5% ( ) s c mu tm.
ho tan
ml dung dch m p 4,5 c pha bng

cch ho tan 29,9g natri acetat trong nc, thm 16,6 ml acid acetic
bng v thm nc va 10.000 ml.
135
ml dung dch mu th, lc. o ngay lp tc

hp th nh sng ca dch lc (nu cn, pha long vi mi trng
1cm, so vi mu trng l mi trng ho tan.
Song song o hp th nh sng ca dung dch acid acetylsalicylic

chun c nng tng ng c pha trong mi trng ho tan.
hm lng C9H8O4 trong acid acetylsalicylic chun, tnh hm

lng C9H8O4 c trong dung dch mu th.
Yu cu: Khng c t hn 70% lng acid acetylsalicylic C9H8O4

so vi lng ghi trn nhn c ho tan trong 45 pht.
Gii hn acid salicylic t do:
vi 4 ml ethanol 96% ( ) v pha long vi nc n 100 ml nhit

khng qu 100C. Lc ngay bng giy lc v ly 50 ml dch lc, thm 1 ml
dung dch phn st amoni 0,2% ( ) mi pha, trn u v yn trong 1
pht. Dung dch ny khng c c mu tm thm hn mu ca dung
dch mu (gm 1 ml dung dch phn st amoni 0,2% mi pha v hn hp
ca 3 ml dung dch acid salicylic 0,010% (KL/ ) mi pha, 2 ml ethanol
96% ( ) v nc va 50 ml). in hnh th trong 2 ng nghim
essler hoc cho vo hai ng nghim ging nhau so snh mu ca
chng.
nh lng:
Cn chnh xc 20 vin, tnh khi lng trung bnh v nghin thnh

bt mn. Cn chnh xc mt lng bt vin tng ng vi 0,5g acid
acetylsalicylic. Thm 30 ml dung dch natri hydroxyd 0,5 un si nh
trong 10 pht, ri chun lng natri hydroxyd 0,5 tha bng dung
dch acid hydrocloric 0,5 , dng dung dch phenol lm ch th (C ).
h mt mu trng nh trn nhng khng c ch phm. iu s gia 2
ln chun biu th lng dung dch natri hydroxyd dng nh
lng.
1 ml dung dch natri hydroxyd 0,5 , tng ng vi 45,04mg

C9H8O4.
T LNG GI V BI TP
1. rnh by tiu chun v k thut kim nghim chung ca vin

nang?
136
2. rnh by cch th ng u khi lng ca vin nang

cephalexin 250mg?

3. Quy nh gii hn cho php v chnh lch khi lng ca vin

nn, vin nang nh sau:
a) Vin nn vitamin C c khi lng trung bnh vin l 0,1532g
A. 10% B. 6% C. 5% D. 7,5%
b) Vin nn paracetamol c khi lng trung bnh vin l 0,6953g
A. 8% B. 7,5% C. 5% D. 6%
c) Vin nang cloramphenicol c khi lng trung bnh vin l

0,2896g
A. 10% B. 12% C. 5% D. 8%
d) Vin nang ampicilin c khi lng trung bnh vin l 0,6385g
A. 12% B. 5% C. 7,5% D. 10%

phm vin nn, vin nang so vi hm lng ghi trn nhn nh
sau:
a) Vin nang nifedipin 5mg
A. 10% B. 12% C. 11% D. 8%
b) Vin nang omeprazol 20mg
A. 12% B. 10% C. 7,5% D. 5%
c) Vin nang cloramphenicol 250mg
A. 10% B. 6% C. 7,5% D. 5%
5. Cc ch phm sau y, ch phm no cn xc nh ng u

hm lng:
A. Vin nn gacdenal 5mg.
B. Vin nang amoxicilin 250mg.
137
C. Vin nang ciprofloxacin 250mg.
D. Vin nn diazepam 1,5mg.
E. Vin nn dopegit 0,5mg.

vin nn.
7. gi ta nh gi ng u hm lng haloperidol ca vin

nn haloperidol 1,5mg. Kt qu (mg/vin) thu c sau khi nh
lng 10 vin ring bit nh sau: 1,537 - 1,480 - 1,245 - 1,632 -
1,571 - 1,602 - 1,516 - 1,493 - 1,618 - 1,587. i ch phm c t
v ng u hm lng khng (tnh theo 10 vin)?
8. Bng tnh ton hy cho bit vin nang cloramphenicol 100mg c

t v hm lng khng?
Bit rng ngi ta ho tan 0,1506g bt vin (vin c khi lng
trung bnh l 0,1583g) trong nc va 500 ml nc, lc. Pha
long 10,00 ml dch lc ti va 100 ml vi nc. o mt
quang ca dung dch ny trong cuvet c chiu dy 1cm, mu trng
l nc bc sng 278nm c kt qu l 0,562.
Cloramphenicol bc sng 278nm c E 1%1cm = 297.
Bi 10
KIM NGHIM CC DNG THUC LNG
MC TIU

gi cht lng thuc tim, thuc nh mt, xir thuc.

- Trnh by c v d v kim nghim cc dng bo ch thuc tim,

thuc nh mt, xir thuc.
1. KIM NGHIM THUC TIM
Ch phm dng tim truyn (parenteral preparations) c 5 loi l:
- huc tim (injections).
138
- Dch truyn (infusions).
- Dung dch m c dng tim hoc truyn (concentrates for

injections and infusions).
- huc bt dng tim hoc truyn (powders for injections and

infusions).
- Thuc cy (implants).
rong phm vi ca chng trnh ch cp ti yu cu k thut v

phng php kim nghim thuc tim.
1.1. Khi nim thuc tim
huc tim l cc dung dch, hn dch, hoc nh tng, v khun

c iu ch bng cch ho tan hoc nh ho, phn tn cc cht v
cc cht ph trong nc pha thuc tim hoc trong cc dung mi v
khun thch hp.
1.2. Yu cu cht lng v phng php th
1.2.1. Tnh cht
Dng dung dch nc hoc du, nh dch hoc dch treo, bt,... tu
theo tng ch phm, c ng trong ng, l, chai thch hp m bo
v khun.
1.2.2. trong
- Dung dch tim khi kim tra bng mt thng iu kin quy
nh phi trong v hu nh khng c tp c hc.
+ Cch xc nh trong ca thuc tim bng mt thng c tin

hnh trong ng nghim ging nhau, bng thu tinh trung tnh, trong,
khng mu, y bng, c ng knh trong t 15 25mm. Chiu dy lp
dung dch khong 40mm. Dng 2 ng, 1 ng ng dung dch cn th, 1
ng ng nc hoc dung mi pha ch thuc tim. Quan st dung dch
trong 2 ng t trn xung trn nn en di nh sng khuch tn ban
ngy.
+ p c hc (tiu phn l) c xc nh bng dng c soi tiu

phn gm 1 bng mu en khng bng, 1 bng mu trng khng lo gn
thng ng, gn nhau v c chiu sng bng ngun sng trng vi
chiu sng cn thit. in hnh th bng cch quay trn nh nhng
139
hoc dc ngc chai hay ng thuc sao cho khng to thnh bt kh

trong dung dch, quan st khong 5 giy pha trc bng mu trng v
lp li php th ny pha trc bng mu en.
+ huc tim th tch khng qu 5 ml: soi 20 ng, khng c c

qu 2 ng c nhiu hn 1 vt th l.
+ huc tim th tch ln hn 5 ml v di 100 ml: soi 10 ng, khng

c c qu 1 ng c nhiu hn 1 vt th l.
+ huc tim v truyn tnh mch th tch t 100 ml tr ln: soi 3 ng

hoc chai, khng c c vt th l.
+ h tng phi khng thy du hiu ca s tch lp.
+ n dch tim c th lng cn nhng phi phn tn ngay khi lc

u v gi c s ng u khi ly liu ra khi ng thuc tim.
1.2.3. Mu sc
Khng mu hoc c mu do hot cht tu theo tng chuyn lun.

in hnh so vi mu mu - Ph lc 5.17, DV .
1.2.4. pH
p phi nm trong gii hn quy nh.
in hnh o p bng my o p .
1.2.5. v khun
mc 3,
bi 13.
1.2.6. Ni c t vi khun
u c quy
nh trong chuyn lun ring. h theo Ph lc 10.3 - DV .
khi c quy nh khc.
1.2.7. Cht gy st
140
nh i vi:
+ huc tim ng liu n l c th tch t 15 ml tr ln v khng

c quy nh php th ni c t.
+ huc tim ng liu n l c th tch nh hn 15 ml nhng trn

nhn c ghi "khng c cht gy st" v khng c quy nh php th ni
c t.
mc 4, bi
13.
1.2.8. Th tch (i vi thuc tim dng lng)
Cch th: huc tim c thng bng ti nhit phng v phi

c phn tn ng u trc khi th.
a) i vi thuc tim n liu
i vi thuc tim c th tch nh hn hoc bng 5 ml:
+ Ly 6 ng thuc, trng bm tim bng 1 ng, th trn 5 ng.
+ Kim tra bng cm quan 5 ng thuc, thy cc ng th cha th

tch ngang nhau.
+ Dng bm tim kh sch c dung tch khng ln hn 2,5 ln so vi

th tch cn o, c gn kim tim thch hp. Ly thuc sao cho trong bm
tim khng c bt kh v trong kim tim vn cha y thuc tim. Ln
lt ly thuc ca tng ng tim theo cch .
ml:
+ Ly 4 ng thuc, trng bm tim bng 1 ng, th trn 3 ng.
+ Cch tin hnh nh i vi thuc tim c th tch khng ln hn 5

ml.
b) i vi thuc tim nhiu liu trong 1 l v thuc tim truyn tnh

mch th th tch phi ln hn so vi s liu quy nh c ly ra.
bng bm tim chun hoc ng ong chun sch, kh, c chnh xc

ph hp ( h tch khng ln hn 2,5 ln th tch cn xc nh).
gii hn cho
php theo bng 15.
Bng 15. Gii hn cho php v th tch i vi thuc tim
141
Th tch ghi trn nhn ( ml) Phn trm chnh lch
i 50 ml + 10
Trn 50 ml +5
nh ln u. u ln th hai c qu mt n v khng t th l thuc

khng t yu cu.
1.2.9. ng u khi lng (i vi ch phm dng bt)
Loi b ht nhn, ra sch v lm kh bn ngoi, loi b ht cc nt

v cn ngay khi lng c thuc v v; ly ht thuc ra, dng bng lau
sch, nu cn th ra bng nc, sau ra bng ethanol 96% ri sy
100 - 1050C trong 1 gi; nu v ng khng chu c nhit th lm
kh iu kin thch hp v cn. iu s khi lng hai ln cn l khi
lng ca thuc. Lm nh vy vi 9 n v khc ly bt k.
Cho php khng qu mt n v c khi lng chnh lch khi bng

10 (Bi 8).
1.2.10. ng u hm lng
2mg hoc di 2% (KL/KL) so vi khi lng thuc ca ton b. huc

tim, thuc tim truyn dng bt ng gi c khi lng nh hn hoc
bng 40mg.
lng v hm lng hot cht trong gii hn quy nh.
nh nht bt k, xc nh hm
lng hot cht tng ng theo phng php ch dn trong chuyn lun.
u nm trong gii hn 85 - 115% ca hm lng trung bnh.
+ Ch phm khng t yu cu nu c qu 1 n v c gi tr hm
lng nm ngoi gii hn 85 - 115% ca hm lng trung bnh, hoc c
mt n v c hm lng nm ngoi gii hn 75 - 125% ca hm lng
trung bnh.
+ u mt n v c gi tr hm lng nm ngoi gii hn 85 -115%

nhng trong gii hn 75 - 125% ca hm lng trung bnh th th li
trn 20 n v khc, ly ngu nhin. Ch phm t yu cu, nu khng
qu 1 n v trong tng s 30 n v em th c gi tr hm lng nm
ngoi gii hn 85 -115% ca hm lng trung bnh v khng c n v
142
no c gi tr hm lng nm ngoi gii hn 75 - 125% ca hm lng

trung bnh.
1.2.11. nh tnh

chun, thuc tim v thuc tim truyn phi cho cc phn ng ca cc
hot cht c tron
1.2.12. nh lng
Ly thuc trong s l thuc nh i vi php th "th tch" (ch

phm dng lng) hoc nh i vi php th " ng u khi lng"
(ch phm dng bt), trn ng nht. in hnh nh lng theo cc
phng php c quy nh trong tiu chun, hm lng ca tng hot
Bng 16. Gii hn cho php v hm lng i vi thuc tim
Lng ghi trn nhn Phn trm chnh lch
Dng dung dch 5
Dng bt 10
1.3. V d
Kim nghim thuc tim Pyridoxin hydroclorid (Thuc tim vitamin

B6), ng ng 1 ml theo DVN III:
pha thuc tim.
uc tim"
8H11NO3. Cl t 95,0 n

1. nh cht Dung dch trong, khng mu. Cm quan.
2. pH 2,5 3,5. o bng my o
143
pH.
3. v Ch phm phi v khun. heo chuyn lun

khun chung.
4. h tch 1,00 1,10 ml. heo chuyn lun
chung.
5. nh tnh Pyridoxin. heo chuyn lun

ring.
Clorid.
6. nh m lng pyridoxin hydroclorid heo chuyn lun
lng C8H11NO3. Cl t 95,0 n 115,0% so ring.
vi lng ghi trn nhn.

thuc th bi 4 v Ph lc 2.8 DV :
- Dung dch m amoniac.
- Dung dch 2,6 dicloroquinon clorimid.
- Butanol.
- Dung dch st ( ) clorid 5%.
- Dung dch acid sulfuric 10%.
- Dung dch acid nitric 16%.
- Dung dch bc nitrat 5%.
- Dung dch amoniac.
- Dung dch chun acid hydrocloric 0,1 .
c) Phng php th
Tnh cht:
Dung dch trong, khng mu.
nh tnh:
0,1g pyridoxin hydroclorid, ho vi nc va 10 ml.
144
ml dung dch A, thm 1 ml nc ct, 2 ml dung dch m

amoniac (TT), 1 ml dung dch 2,6 dicloroquinon clorimid ( ) v 2 ml
butanol ( ), lc 1 pht, yn, lp butanol s hin mu xanh.
ml dung dch A, thm 2 git dung dch st ( ) clorid 5%

( ) s hin mu . hm vi git dung dch acid sulfuric 10% (TT) mu
s phai dn.
ml dung dch A, thm 2 ml nc ct, 5 git dung dch acid

nitric 16% (TT) v 0,5 ml dung dch bc nitrat 5% ( ) s to thnh ta
trng ln nhn, ta ny tan trong dung dch amoniac ( ).
pH:
2,5 n 3,5 (Ph lc 5.9
nh lng:
Ly chnh xc mt lng ch phm tng ng vi 0,100g pyridoxin

hydroclorid cho vo bnh nh mc 500 ml, ho long vi dung dch acid
hydrocloric 0,1 (C) va n vch, trn u. Ly chnh xc 5,0 ml
dung dch trn pha long vi dung dch acid hydrocloric 0,1 (C) thnh
100 ml
DV ), dng dung dch acid hydrocloric 0,1 lm mu trng.
nh hm lng C8H11NO3. Cl theo A (1%, 1cm), ly 427 l gi tr A

(1%, 1cm) bc sng 291nm.
2. KIM NGHIM THUC NH MT
2.1. Khi nim
huc nh mt l dung dch nc, dung dch du hoc hn dch v

khun ca mt hay nhiu hot cht nh vo mt. Khi c yu cu, ch
phm c pha ch dng kh, v khun c th ho tan hoc lm
thnh huyn ph trong mt cht lng v khun thch hp trc khi dng.
huc nh mt c th cha cc cht ph iu chnh tnh ng

trng hoc nht, iu chnh hoc n nh p , tng ho tan ca
hot cht hoc n nh ch phm.
2.2.1. Tnh cht
h cht, mu sc tu theo tng chuyn lun.
145
2.2.2. trong
huc nh mt dng dung dch phi trong, khng c cc tiu phn

khi quan st bng mt thng v t yu cu v trong theo tng
chuyn lun.
huc nh mt dng hn dch c th lng ng, nhng khi lc phi

phn tn d dng v ng nht trong ton khi.
Cch xc nh: trong c xc nh bng cch so snh cc dung

dch vi cc hn dch mu i chiu. h theo Ph lc 5.12 - DV
III.
2.2.3. Th tch
h tch thuc nh mt phi nm trong gii hn 100 - 110% so vi

th tch ghi trn nhn i vi mi th tch ng gi.
Cch th: Ly 5 n v ng gi bt k. Xc nh th tch ca tng

n v bng bm tim chun hoc ng ong chun sch, kh, c
chnh xc ph hp ( h tch khng ln hn 2,5 ln th tch cn xc
nh).
h tch mi n v phi nm trong gii hn cho php.
u c mt n v khng t th phi kim tra li ln th hai ging

nh ln u. u ln th hai c qu mt n v khng t th l thuc
khng t yu cu.
2.2.4. pH
o bng my o p .
2.2.5. v khun
huc nh mt phi v khun.
Cch th: u khng c quy nh ring th tin hnh th v nh gi

theo "Th v trng" mc 3, bi 13.
2.2.6. Gii hn cc tiu phn
h nghim ny ch yu cu i vi thuc nh mt dng hn dch.
Cho mt th tch ch phm thch hp vo cc o hay vt knh ca

g
pha rn.
146
Kt qu:
2.2.7. nh tnh

chun, thuc nh mt phi cho cc phn ng ca cc hot cht c trong
2.2.8. nh lng

2.3. V d
Kim nghim thuc nh mt km sulfat ng l 10 ml DVN III:
L dung dch v khun ca km sulfat trong nc ct c lm

ng trng bng cch cho thm cc mui thch hp.
cc yu cu ca chuyn lun ring.
m lng ca km sulfat ZnS 4.7H2 t 95,0 n 105,0% so vi
1. nh cht Dung dch trong sut, Cm quan.

khng mu.
2. pH 4,5 - 5,5. o bng my o p .
3. v Ch phm phi v khun. heo chuyn lun chung.

khun
4. h tch 10 11 ml. heo chuyn lun chung.
5. nh tnh on km v sulfat. heo chuyn lun ring.
147
6. nh lng m lng ca km sulfat heo chuyn lun ring.

ZnSO4.7H2 t 95,0 n
105,0% so vi lng ghi
trn nhn.

huc th bi 4 v Ph lc 2.8
- Dung dch acid hydrocloric 2M.
- Dung dch bari clorid 5%.
- Dung dch amoniac 6M.
- Dung dch amoni clorid.
- Dung dch dinatri hydrophosphat.
- Dung dch m amoniac p 10.
- Dung dch dinatri dihydro ethylendiamin tetraacetat 0,01 M.
- n hp ch th en eriocrom .
c) Phng php th
Tnh cht:
Dung dch trong sut, khng mu.
nh tnh:
Dung dch ch phm cho cc phn ng ca cc ion km v sulfat
Ly 5 ml dung dch ch phm cho vo ng nghim, thm 1 ml dung

dch acid hydrocloric 2M ( ) v 1 ml dung dch bari clorid 5% ( ), s c
ta trng c to thnh.
Ly 2 ml dung dch ch phm cho vo ng nghim, thm 1 ml dung

dch amoniac 6M ( ) to thnh ta trng, ta ny tan khi thm 1 ml
dung dch amoni clorid ( ). hm 1 ml dung dch dinatri hydrophosphat
( ) s c ta kt tinh mu trng.
pH: 4,5 n 5,5 (Ph lc 5.9 DV ).
v khun:
148
nh lng:
Ly chnh xc mt th tch thuc nh mt tng ng vi khong

25mg km sulfat, thm 50 ml nc v 10 ml dung dch m amoniac p
10,0. Chun bng dung dch dinatri dihydro ethylendiamin tetraacetat
0,01 M, dng hn hp en eriocrom lm ch th (C ).
(1 ml dung dch dinatri dihydro ethylendiamin tetraacetat 0,01 M

tng ng vi 2,875mg ZnS 4.7H2O).
3. KIM NGHIM XIR THUC
3.1. Khi nim
Xir l dung dch m c ca ng trng trong nc, c cha cc

dc cht hoc cc dch chit t dc liu v cc cht thm.
3.2.1. Tnh cht
Ch phm phi trong, khng c c mi l, bt kh hoc bin cht

trong qu trnh bo qun.
Cch th: h bng cm quan.
3.2.2. trong
Xir thuc phi t yu cu v trong theo tng chuyn lun.
Cch xc nh: trong c xc nh bng cch so snh cc dung

dch vi cc hn dch mu i chiu. h theo Ph lc 5.12 - DV
III.
3.2.3. pH
in hnh o p bng my o p .
3.2.4. T trng
trng phi nm trong gii hn quy nh.
in hnh o t trng bng t trng k, picnomet, cn thu tnh Morh

Westphal nh ch dn mc 1, bi 7.
3.2.5. Th tch
149
Cch th: Ch phm c thng bng ti nhit phng v phi

c phn tn ng u trc khi th.
Ly 5 l bt k. Xc nh th tch tng l bng ng ong c th tch

v chnh xc ph hp ( h tch ng ong khng c ln hn 2,5 ln
th tch thuc).
h tch mi l phi nm trong gii hn cho php theo bng 17.
Bng 17. Gii hn cho php v th tch ca xir
Chnh lch cho php

Th tch ghi trn nhn ( ml)
(%)
i 100 ml + 10
rn 100 ml ti 250 ml +8
Trn 250 ml +6
u c 1 l khng t th kim tra ln th hai ging nh ln 1. u

ln hai c qu 1 l khng t th l thuc khng t yu cu v th tch.
3.2.6. nh tnh

chun, xir phi cho cc phn ng ca cc hot cht c trong ch phm
theo tng chuyn lun.
3.2.7. nh lng
Ly thuc trong 5 l thuc, trn ng nht. in hnh nh lng

theo cc phng php c quy nh trong tiu chun, hm lng ca
tng hot cht trong ch phm phi nm trong gii hn cho php theo
bng 18.
Bng 18. Gii hn cho php v hm lng i vi xir thuc
Xir cha dc cht Gii hn chnh lch (%)
huc c A, B 5
huc thng 10
3.2.8. nhim khun
Ch phm phi t nhim khun theo quy nh.
150
gi theo " h gii hn nhim khun" mc 2, bi 13.
3.2.9. ng u hm lng
phn 1.2.5, bi
8.
T LNG GI V BI TP

tim.
2. rnh by cch tin hnh v nh gi kt qu th ng u th

tch ca thuc tim thiamin hydroclorid ng ng 1 ml.
3. rnh by cch tin hnh v nh gi kt qu th ng u khi

lng ca thuc tim benzylpenicilin ng l 1g.
4. in hnh nh lng vitamin B12 trong ng tim vitamin B12 0,5mg/

ml nh sau: Pha long 2,00 ml ch phm trong va 50,0 ml vi
nc. Mt quang ca dung dch ny 361nm trong cc o dy
1cm, dng nc lm mu trng l 0,427.
nh hm lng vitamin B12 trong ch phm. Ch phm c t yu
cu v hm lng khng? Bit vitamin B12 c A (1%, 1cm) bc
sng 361nm l 207.
5. rnh by tiu chun v k thut kim nghim chung ca thuc nh

mt.
6. rnh by phng php tin hnh v tnh kt qu nh lng

cloramphenicol trong thuc nh mt cloramphenicol 0,4%.
7. gi ta tin hnh nh lng natri clorid trong thuc nh mt natri

clorid 0,9% nh sau: Ly chnh xc 10 ml dung dch ch phm cho
vo bnh nn 100 ml, thm 5 git dung dch kali cromat 5%. nh
lng bng dung dch bc nitrat 0,1 c K = 0,9965 ht 15,02 ml.
nh hm lng natri clorid trong ch phm. Ch phm c t yu
cu v hm lng khng? Bit 1 ml dung dch bc nitrat 0,1
tng ng vi 5,844mg aCl.
8. rnh by tiu chun v k thut kim nghim ca xir thuc.
9. gi ta tin hnh nh lng paracetamol trong xir h st tr em

cha 15% paracetamol nh sau: Ly chnh xc 1 ml xir cho vo
bnh nh mc 200 ml, pha long vi dung mi va ti vch.
Lc u, lc (nu cn). Pha long 1,00 ml dch lc thnh 100,0 ml
151
trong bnh nh mc bng dung mi. Mt quang ca dung dch

ny 257nm l 0,524.
i ch phm c t yu cu v hm lng khng? Bit
paracetamol c A (1%, 1cm) bc sng 257nm l 715.
Chn cu tr li ng cho cc cu hi t 10 n 12 bng cch

khoanh trn ch ci u cu c chn:
10. Quy nh gii hn cho php v chnh lch khi lng hoc th
tch ca thuc tim nh sau:
a) huc tim ampicilin dng bt ng l 1g
A. 10% B. 6% C. 7% D. 5%
b) Thuc tim vitamin B1 ng ng 1 ml
A. +8% B. +7,5% C. +5% D. +10%
c) Dung dch tim truyn inger Lactat ng chai 500 ml
A. +10% B. +5% C. +7,5% D. +8%
11. Quy nh gii hn cho php v chnh lch th tch ca thuc nh

mt nh sau:
a) huc nh mt km sulfat 0,5% ng l 8 ml
A. +10% B. +5% C. +7,5% D. +8%
b) huc nh mt natri clorid 0,9% ng l 15 ml
A. +12% B. +11% C. +7,5% D. +10%
c) huc nh mt nemydexan ng l 5 ml
A. +10% B. +15% C. +7,5% D. +8%

phm ca xir thuc so vi hm lng ghi trn nhn nh sau:
a) Xir cha dc cht l thuc c bng A, B
A. 10% B. 2,5% C. 5% D.
7,5%
b) Xir cha dc cht l thuc thng
A. 10% B. 12% C. 11% D. 8%
152
Bi 11
KIM NGHIM THUC M, THUC KEM
MC TIU

gi cht lng thuc m, thuc m tra mt, thuc kem.

- Trnh by c v d v kim nghim cc dng bo ch thuc m.
1. KIM NGHIM THUC M
1.1. Khi nim
huc m l dng thuc c th cht mm, dng bi ln da hay

nim mc nhm bo v da hoc a thuc thm qua da. Bt nho bi da
l loi thuc m c cha mt t l ln cc dc cht khng tan.
1.2.1. Tnh cht
h cht: huc m phi mn, ng nht, khng cng li hoc tch

lp iu kin thng, khng chy lng nhit 37oC v phi bt
dnh c trn da hay nim mc khi bi.
Mu sc, mi: u tng ch phm.
1.2.2. ng u khi lng
Cch th: Cn tng n v trong s 5 n v ng gi nh nht c

ly bt k.
Khi lng tt c cc n v phi nm trong gii hn quy nh theo

bng 19.
u c mt n v c khi lng lch ra ngoi quy nh ny th th

thuc khng t yu cu.
153
Bng 19. Gii hn cho php chnh lch khi lng i vi thuc
m
Khi lng ghi trn nhn Chnh lch cho php (%)
Di 10,0 g 15
10,0 - 20,0 g 10
Trn 20,0 - 50,0 g 8
Trn 50,0 g 5
1.2.3. ng nht
Cc tiu phn phi phn tn ng u.
Cch th: ly 4 n v ng gi, mi n v khong 0,02 -0,03g, tri

ch phm ln 4 tiu bn, bn trn t mt phin knh. y mi phin
knh bng mt phin knh khc v p mnh cho n khi to thnh mt
vt c ng knh khong 2cm. Quan st vt thu c bng mt
thng, 3 trong 4 tiu bn khng c nhn thy cc tiu phn. u c
cc tiu phn nhn thy trong phn ln s cc vt th phi lm li vi 8
n v ng gi. rong s cc tiu bn ny, cc tiu phn cho php nhn
thy khng c vt qu 2 tiu bn.
1.2.4. nh tnh
Tin hnh nh tnh theo cc phng php c quy nh trong tiu

chun, thuc m phi cho cc phn ng ca cc hot cht c trong ch
1.2.5. nh lng
Cn thuc trong 5 n v ng gi nh nht, tnh khi lng trung

bnh, trn ng nht. Cn mt lng ch phm nh ch dn trong
chuyn lun, tin hnh nh lng. m lng hot cht phi nm trong
Bng 20. Gii hn cho php v hm lng i vi thuc m
Nng hm lng ghi trn Chnh lch cho php

nhn (%)
i 200mg 15
Trn 200mg - 1g 10
154
Trn 1g - 5g 7,5
Trn 5g 3
1.3. Thuc m tra mt
iu chun cht lng ca thuc m tra mt phi t cc yu cu
1.3.1. v khun
khun v khng c c
Staphylococcus aureus v Pseudomonas aeruginosa
gi theo " h v trng"
1.3.2. Cc phn t kim loi
tng a petri ring c ng knh 6cm, y bng, khng c cc vt

xc v cc phn t l nhn thy c. y cc a, un nng n 80 -
85oC trong 2 gi v cho thuc m phn tn ng u. Lm ngui v
lm ng lnh thuc m, lt ngc mi a t ln bn soi ca knh hin
vi thch hp; chiu sng t trn xung bng mt ngn n chiu t
gc 450 so vi mt phng ca bn soi. Quan st v m cc phn t kim
loi sng bng,
qu mt ng trong 10 ng thuc em th cha nhiu hn 8 phn t v
khng c qu 50 phn t tm thy trong 10 ng. u ch phm khng
t ln th th nht th lm li ln th hai vi 20 ng thuc khc. Mu
th c coi l t yu cu nu khng c qu 3 ng cha qu 8 phn t
1.3.3. Gii hn kch thc cc phn t
: ri mt lng nh ch phm thnh mt lp mng trn

bn soi ca knh hin vi, ph phin knh ln trn v soi.
1.4. V d
Kim nghim thuc m acid boric 10%, ng gi 15g - DVN III:
155
yu cu ca chuyn lun ring.
3BO3 t 9,0 n 11,0%.
1. nh cht huc m mu trng hoc Cm quan.

vng nht.
2. ng 15g 10%. heo chuyn lun chung.

u khi
lng
3. ng Ch phm phi ng nht, heo chuyn lun chung.

nht khng c tiu phn, vt l.
4. nh tnh Acid boric. heo chuyn lun ring.
5. nh lng m lng ca acid boric heo chuyn lun ring.

H3BO3 t 9,0 n 11,0%.
b) Thuc th

huc th, bi 4, Ph lc 2.8 - DV .
- Ethanol.
- Dung dch acid sulfuric m c.
- Dung dch chun natri hydroxyd 0,1 .
- Dung dch ch th phenolphtalein.
c) Phng php th
Tnh cht:
huc m mu trng hoc vng nht.
nh tnh:
Ly 1g ch phm cho vo mt bt un, thm 4 ml ethanol (TT) v 1

git acid sulfuric m c ( ). Chm la t, va t va khuy bng
mt a thu tinh. gn la c vin mu xanh l m.
156
nh lng:
Cn chnh xc khong 1g ch phm cho vo cc c m, thm 20 ml

nc v 20 ml phenolphtalein. un cch thu (C ) cho tan. Lc u.
Chun bng dung dch natri hydroxyd 0,1 n khi xut hin mu
hng bn vng (ch th phenolphtalein).
(1 ml dung dch natri hydroxyd 0,1 tng ng vi 6,183mg

H3BO3).
2. KIM NGHIM THUC KEM
2.1. Khi nim
Kem (Cream) l dng ch phm mm, nht, ng nht, thng bao

gm mt hay nhiu hot cht ho tan hay phn tn trong t dc, hoc
hn hp t dc. Cc t dc ny thng dng nh tng du/nc,
hoc nc/du. Kem bi da thng c th cht mm v mn mng.
i chung yu cu k thut v phng php th ca kem ging nh

i vi thuc m.
T LNG GI V BI TP

m.
2. iu chun v k thut kim nghim ca thuc m tra mt c g

khc so vi thuc m ni chung? y trnh by nhng im khc
nhau .
3. rnh by cch tin hnh v nh gi kt qu th ng u

khi lng ca kem ngh ng gi 5g trong 1 tuyp.

4. Quy nh gii hn cho php v chnh lch khi lng ca thuc

m, thuc kem nh sau:
a) huc m tra mt clorocid ng gi 4g
A. 10% B. 15% C. 12,5% D. 20%
b) huc m profenid gel ng gi 50g
157
A. 5% B. 7,5% C. 8% D. 6%
c) huc m km oxyd ng gi 15g
A. 10% B. 12% C. 15% D. 8%
d) huc m kem acyclovir ng gi 3g
A. 12% B. 7,5% C. 15% D. 10%

phm thuc m, thuc kem so vi hm lng ghi trn nhn nh
sau:
a) huc m tra mt tetracyclin 1% ng gi 5g
A. 10% B. 12% C. 11% D. 8%
b) huc kem acyclovir 5% ng gi 3g
A. 12% B. 10% C. 7,5% D. 5%
c) huc m acid boric 10% ng gi 15g
A. 10% B. 6% C. 5% D.
7,5%
6. huc m tra mt yu cu th cc ch tiu:
A. v khun.
B. r nhit t.
C. ii hn nhim khun.
D. Cc phn t kim loi.

kem.
158
Bi 12
KIM NGHIM THUC NG DC
MC TIU

gi cht lng thuc hon, ru thuc, cao thuc.
- nh gi c kt qu kim nghim i vi mt mu kim nghim

thnh phm c th ca cc dng bo ch trn.
- Trnh by c v d v kim nghim cc dng bo ch thuc hon,

ru thuc, cao thuc.
1. KIM NGHIM THUC HON
1.1. Khi nim
on l dng thuc rn hnh cu, mm hoc cng, khi lng c th

thay i thng t 4mg n 12mg. hnh phn ca hon gm cc bt
mn ca dc liu, hoc cc dch chit dc liu, cc cht dnh, hoc
cc t dc thch hp. on dng ung, nhai hoc ngm.
1.2.1. Hnh thc
mm mt ong phi mn, trn bng, nhuyn do vi cng thch hp
ng cm quan.
1.2.2. m
- on mm mt ong khng c cha nhiu hn 15% nc.
- on cng: on mt ong nc khng c cha nhiu hn 12%

nc; hon nc, hon h khng c cha nhiu hn 9% nc.
u theo tng ch phm m c yu cu s dng phng php xc

nh m khc nhau nh:
159
+ on cng: in hnh theo phng php xc nh mt khi lng
+ on mm v hon cng trong thnh phn c cha nhiu tinh du

hoc ng: Xc nh nc bng phng php ct vi dung mi (Ph
1.2.3. r
"Php th r vin nn v vin nang" mc 5, bi 7.
gi cho cc loi
hon, ring hon h c php r khng qu 2 gi.
1.2.4. ng u khi lng
vin.
Cn khi lng ca 10 hon, xc nh khi lng trung bnh ca 1

hon. Cn ring r tng hon v so snh vi khi lng trung bnh
hon.
C 10 hon c coi l 1 phn. Cn ring r 10 phn v tnh khi

lng trung bnh ca mt phn, sau so snh vi khi lng trung
bnh, tnh lch theo t l phn trm ca khi lng trung bnh, t
tnh ra khong gii hn ca gi tr trung bnh.
hoc ng gi theo liu ung mt ln hoc ung hng ngy.
Ly 10 n v ng gi, cn ring bit tng n v ng gi v so

snh vi khi lng trung bnh, tnh lch theo t l phn trm ca khi
lng trung bnh, t tnh ra khong gii hn ca gi tr trung bnh.
nh bng 21.
Bng 21. Gii hn cho php chnh lch khi lng i vi vin
hon
Phng php 1 Phng php 2 Phng php 3
KLTB* % chnh KLTB* % chnh KLTB* ca 1 %
160
ca 1 lch ca 1 lch n v ng gi chnh

hon phn lch
0,05g 12% 0,05g 12% 0,5g tr 12%

n 1,5g n 0,1g xung
rn 0,5g n 11%
1g
Trn 1,5g 10% Trn 0,1g 10% rn 1g n 2g 10%

n 5g n 1g
rn 2g n 3g 8%
Trn 5g 7% Trn 1g 7% rn 3g n 6g 6%
n 9g
rn 6g n 9g 5%
Trn 9g 5% Trn 9g 4%
KL B*: Khi lng trung bnh
Khi lng ca tng hon (phng php 1), tng phn (phng
php 2), tng n v ng gi (phng php 3) ng vi khi lng trung
bnh phi nm trong gii hn sai s quy nh bng 21. Khng c c
qu hai n v vt qu gii hn sai s cho php. Khng c c n v
no vt gp i gii hn cho php.
1.2.5. nh tnh

chun, thuc hon phi cho cc phn ng ca cc hot cht c trong
ch phm.
1.2.6. nh lng
in hnh nh lng theo cc phng php c quy nh trong

tiu chun, hm lng ca tng hot cht trong ch phm phi nm
trong gii hn cho php theo tng chuyn lun ring.
1.2.7. nhim khun
u cu v gii hn nhim khun.
nh gi theo " h gii hn nhim khun" mc 2, bi 13.
1.2.8. c tnh bt thng
161
u khng c quy nh ring th tin hnh th v

nh gi theo quy nh ca chuyn lun " h c tnh bt thng" (Ph
1.3. Cc loi vin hon
iu chun cht lng ca cc loi vin hon phi tun theo yu cu

chung ca thuc vin hon v yu cu ring i vi tu tng loi.
12% nc.
9% nc.
1.4. V d
Kim nghim Hon lc v (hon cng, ng gi 25g) - DVN III:
oi sn 80g
hc a 160g
n b 60g
rch t 60g
Phc linh 60g
Sn th 80g
Mt ong 1000g
1. Tnh cht on cng hnh cu, mu en Cm quan.

nhnh. Mi thm dc liu. V
ngt hi chua.
2. m Khng c qu 9%. heo chuyn lun
162
chung.
3. ng u KLTB 10%. heo chuyn lun

khi lng chung, phng
php 2.
4. r Khng c qu 1 gi. Theo chuyn lun

chung.
5. nh tnh - Bng ct ko hi nc. heo chuyn lun

ring.
- Sinh a.
6. nhim t yu cu v gii hn nhim heo chuyn lun

khun khun. chung.
b) Phng php th
Tnh cht:
Ch phm l hon hnh cu, mu en nhnh. Mi thm dc liu. V

ngt hi chua.
nh tnh:
- Ct ko bng hi nc 10g hon v hng ly 20 ml dch ct, ly 2

ml dch ct, thm 0,5 ml acid benzosulfonic diazo ho, 1 - 2 git natri
carbonat ( ) xut hin dn dn mu da cam.
- nh tnh hc a:
+ Bn mng: Silicagel hot ho 110 oC trong 1 gi.
+ Dung mi khai trin: Cloroform - ethylacetat (9: 1).
+ Dung dch th: ly khong 10g ch phm, tn thnh bt th, chit

bng cch un si cch thu 15 pht vi methanol 3 ln, mi ln 30 ml.
p dch chit methanol, c trn cch thu n cn. Cn c chit
bng n- butanol 3 ln, mi ln 5 ml, gp dch chit n butanol ri lc, c
dch lc trn cch thu n cn. o cn trong 1 ml ethanol.
+ Dung dch i chiu: Ly 1,5g hc a thi nh, ri tin hnh chit

nh dung dch th, bt u t chit bng cch un si,... ho cn trong 1
ml ethanol.
th v dung dch i chiu. rin khai dung mi khong 12 15cm. Ly
163
bn mng ra kh nhit phng, phun dung dch acid sulfuric 10%

trong ethanol ( ). Sy bn mng 110 oC n khi hin r vt. rn sc
k ca dung dch th phi cho vt c cng mu v gi tr f vi cc
vt trn sc k ca dung dch i chiu.
2. KIM NGHIM CAO THUC
2.1. nh ngha
Cao thuc l ch phm iu ch bng cch c hoc sy n th cht

quy nh cc dch chit thu c t dc liu thc vt hay ng vt vi
cc dung mi thch hp.
t yu cu quy nh trong chuyn lun ring v cc yu cu chung

sau y:
2.2.1. Cao lng
a) ho tan
Cao lng phi tan hon ton trong dung mi dng iu ch

cao.
b) trong, ng nht v mu sc
ng mu sc m t trong chuyn lun ring,

khng c vng mc, khng c cn b dc liu v vt l.
khong 10 15 ml. Chuyn phn cn li trong chai vo mt bt s men

trng, nghing bt cho thuc chy t t trn thnh bt to thnh mt lp
d quan st. Quan st di nh sng t nhin, thuc phi t cc yu
cu quy nh. u khng t phi th li ln th hai vi chai thuc khc,
nu khng t coi nh l thuc khng t ch tiu ny.
c) nh tnh

chun, ch phm phi cho cc phn ng ca cc hot cht c trong ch
phm.
d) nh lng

164
2.2.2. Cao c, cao kh
a) Mt khi lng do lm kh
u khng c ch dn khc th:
- Cao c: khng qu 20%.
- Cao kh: khng qu 5%.
b) nhim khun
t y
III.
c) nh tnh

chun, ch phm phi cho cc phn ng ca cc hot cht c trong ch
phm.
d) nh lng

2.3. V d
Kim nghim Cao hy thim (Cao lng) - DVN III:
Hy thim 1000g
hin nin kin 50g
Ethanol 90% 235 ml
ng trng 130g
c 1000 ml
165
1. nh cht Cht lng mu nu en, mi Cm quan.

thm hin nin kin, v ngt.
2. nh tnh Hy thim. heo chuyn lun

ring.
3. trong v Snh, ng nht, khng c Cm quan.

ng nht c vng mc, b dc liu v
vt l.
4. m lng 19% 1%. heo chuyn lun

ethanol chung.
5. trng 20oC: 1,05 1,10. heo chuyn lun

chung, dng t trng
k.
b) Phng php th
Tnh cht:
Cht lng mu nu en, mi thm hin nin kin, v ngt.
nh tnh:
nh tnh y thim:
o
C trong 1 gi.
methanol (9: 1).
Ly 25 ml ch phm, pha long vi 25 ml nc,

chit bng ethyl acetat 2 ln, mi ln 25 ml. p cc dch chit, c trn
cch thu ti cn. o tan cn trong 1 ml ethanol.
Dung dch i chiu: Ly khong 25g y thim, ct nh, un si vi

100 ml nc trong khong 1 gi (lun b nc bc hi), gn, lc dch
chit, c cn khong 50 ml ri tip tc chit bng ethyl acetat nh dung
dch th.
th v dung dch i chiu. Sau khi trin khai xong, kh bn mng

nhit phng ri phun dung dch acid sulfuric 10% ( ), sy bn mng
110oC ti khi xut hin cc vt. rn sc k ca dung dch th phi
cho vt c cng mu v gi tr f vi cc vt trn sc k ca dung
dch i chiu.
166
trong v ng nht:
Snh, ng nht, khng c c vng mc, b dc liu v vt l.
Hm lng ethanol:
19%
T trng:
20oC: 1,05
trng k).
3. KIM NGHIM RU THUC
3.1. nh ngha
u thuc l dng thuc lng c mi thm v v ngt, iu ch

bng cch ngm dc liu thc vt hoc ng vt ( ch bin) trong
ru hoc ethanol long trong mt thi gian nht nh (tu theo quy nh
ca tng cng thc) ri gn ly ru thuc. m lng ethanol trong
ru thuc khng qu 45%.
3.2.1. Mu sc
5 ml, cho vo 2 ng nghim (thu tinh khng mu, ng c). Quan st

mu ca hai ng nh sng thin nhin bng cch nhn ngang, mu sc
ca hai ng phi nh nhau v ng nh mu sc quy nh trong tng
chuyn lun.
3.2.2. Mi v
t yu cu theo quy nh trong chuyn lun ring.
3.2.3. trong v ng nht
vt l.
mc. t 5 ml ru thuc v tr cch y chai khong 2cm, cho vo

ng nghim (thu tinh khng mu, dung tch 10 20 ml, quan st nh
sng thin nhin bng cch nhn ngang. u thuc phi trong v ng
167
nht. u khng t yu cu, th li ln th hai vi mt chai ru thuc

khc. Ln ny khng t th l thuc coi nh khng t tiu chun.
3.2.4. Hm lng ethanol
t yu cu theo quy nh trong chuyn lun ring.
Cch xc nh: m lng ethanol trong ch phm c xc nh

theo ch dn Ph lc 6.15 DV .
3.2.5. T trng
t yu cu theo quy nh trong chuyn lun. Xc nh t trng theo

Ph lc 5.15 DV .
3.2.6. lng cn
yn khong 48 gi, sau m nt v thn trng dng ng cao su hay

ng nha lm xiphng, ht phn ru pha trn, cn li 15 20 ml
(i vi ru c th tch cn khng qu 0,5 ml), hoc 40 50 ml (i vi
ru c th tch cn trn 0,5 ml). Lc cn trong chai cho tan, rt ht sang
ng ong 25 ml (chia 0,5 ml) hoc 50 ml (chia 1 ml) c nt. Ly
phn ru trong ht xiphng trng chai, vo ng ong ri thm
ru thuc va 25 ml hoc 50 ml. lng 48 gi, c kt qu trn
vch chai.
3.3. V d
Kim nghim Ru b huyt tr phong - DVN III:
h phc linh 10g

Cu
tch 20g
uyt gic 10g
g gia
c on 20g
b 10g
Hy thim 30g
Tang
chi 30g
ng
trng 130g
gu
168
tt 10g K huyt
ng 40g
th
40g Ethanol 130
ml
Thin nin
kin 30g
Hong
tinh 20g
1. nh cht Cht lng trong, mu nu, Cm quan.

mi c bit, v ngt cay.
2. trong Ch phm phi trong. Cm quan.
3. Hm lng 19 - 23% heo chuyn lun

ethanol chung.
4. trng 20oC: 1,02 - 1,04. heo chuyn lun

chung, dng t trng
k.
5. lng cn Lp cn khng c qu 0,5 heo chuyn lun

ml. chung.
b) Phng php th
Tnh cht:
Cht lng trong, mu nu, mi c bit, v ngt cay.
trong:
1.17 - DV ).
Hm lng ethanol:
19 - 23% (Ph lc 6.15 - DV ).
T trng:
200C: t 1,02 -
t trng k).
169
lng cn:
Lp cn khng c qu 0,5 ml (Ph lc 1.17 - DV ).
T LNG GI V BI TP

hon.
2. rnh by tiu chun v k thut kim nghim ca cao thuc.
3. Trnh by tiu chun v k thut kim nghim ca ru thuc.
Chn cu tr li ng cho cc cu hi t 4 n 6 bng cch khoanh trn

ch ci u cu c chn:
4. Quy nh gii hn cho php v chnh lch khi lng ca thuc

hon c ung theo s lng vin nh sau:
a) huc i trng hon c khi lng trung bnh 0,1258g
A. 10% B. 15% C. 12% D.

7%
b) huc hon phong t thp c khi lng trung bnh 1,5632g
A. 5% B. 10% C. 7% D.
6%
c) huc hon b thn dng c khi lng trung bnh 5,2687g
A. 10% B. 12% C. 7% D.
8%
5. Quy nh v thi gian r cho php i vi thuc hon nh sau:
a) huc i trng hon (hon nc) l khng qu:
A. 60 pht B. 45 pht C. 90 pht D. 120

pht
b) huc hon phong t thp (hon nc) l khng qu:
A. 105 pht B. 45 pht C. 60 pht D. 90

pht
c) huc hon b thn dng (hon h) l khng qu:
170
A. 105 pht B. 120 pht C. 60 pht D. 90

pht
6. Quy nh gii hn cho php v hm lng nc i vi cao thuc

nh sau:
a) Cao c, khng qu:
A. 5% B. 15% C. 20% D. 10%
b) Cao kh, khng qu:
A. 5% B. 15% C. 20% D. 10%
Bi 13
MT S PHNG PHP SINH HC
TRONG KIM NGHIM THUC
MC TIU
- Trnh by c phng php lm mi trng nui cy vi sinh vt v

nu c cc phng php kh trng.
- Trnh by c mc ch, nguyn tc, phng php th cht gy

st, v khun v gii hn nhim khun ca ch phm bo ch v
nguyn liu lm thuc.
rong Ph lc 10 ca Dc in Vit am c trnh by phng

php kim nghim thuc bng phng php sinh hc. rong khun kh
ca ti liu ny, chng ti trnh by ba php th nh gi cht lng
thuc l th cht gy st, th gii hn nhim khun v th v trng.
1. YU CU C BN CA PHNG KIM NGHIM VI SINH VT
1.1. Quy tc an ton trong phng kim nghim vi sinh vt
Cn b lm vic ti phng kim nghim vi sinh phi c kin thc

v kinh nghim v cng tc kim nghim vi sinh v phi tun theo cc
quy tc an ton trong khi lm vic.
1.1.1. Yu cu v phng kim nghim vi sinh
Din tch lm vic, cc khu vc trong phng c phn chia v b tr

ph hp, khong cch lm vic hp l hn ch ti a s di chuyn
trong phng (lm xo ng khng kh v lm tng nguy c nhim).
thng chiu sng y , c h thng thng kh trnh s ng bi v
171
lan truyn cc vi sinh vt,... Khu vc thao tc nui cy nn c lp t

n t ngoi tit trng khng kh v khng gian thao tc. Ch trnh
hoc khng dng qut trong phng kim nghim vi sinh, trnh mi
trng, ho cht trc tip di nh sng mt tri.
1.1.2. Cc quy tc an ton trong phng kim nghim vi sinh
tip vi cc vi sinh vt, ng thi c nhiu chng vi sinh vt gy bnh

nn khi tin hnh lm vic phi ht sc cn thn vi cc chng ang
thao tc. Ch phi nm vng nguyn tc, phng php lm vic vi vi
sinh vt. Khng n ung, ht thuc trong phng kim nghim. rong khi
lm vic phi mc o blouse, mang khu trang khi thao tc vi vi sinh
vt. rc khi bt u th nghim cn st trng mt bn, st trng tay
bng cn 70oC hoc dung dch cht dit khun khc, kh. Sau khi
hon thnh cng vic li tin hnh st trng nh trn. rng hp v
tnh b , nhim vi sinh vt ra ni lm vic, dng khn giy tm cht dit
khun lau k, sau kh trng li bn lm vic.
hp Petri, ng nghim mi trng, bnh nui cy.
hoc nhim vi sinh vt cn

c hp kh trng trc khi thi i.
dung dch cht dit khun (nc Javel) trc khi ra v ti s dng.
1.2. Dng c, thit b
- Cc dng c bng thu tinh: ng nghim, a petri, n cn, cc

thu tinh, bnh cu y bng v trn, bnh tam gic, cc loi ng ong,
ng ht,...
- Que cy: que cy thng, que cy vng, que cy mc.
-
ng knh vi khun. VSV s b gi li trn mng lc cn dung dch i
qua s v trng. Mng lc c th bng cellulose hay hn hp cellulose
v mui este ca cellulose.
- hit b: nhit k, my o p , t sy, t m, my lc, b iu nhit,

t lnh, n t ngoi (UV), ni hp, knh hin vi, bnh k kh,...
- cy v trng: t cy v trng c s dng m bo tnh v

trng cao khi thao tc vi vi sinh vt. Khng kh trong t cy v trng
c cung cp qua h thng lc khng kh. n t ngoi c tc dng
kh trng b mt bn thao tc trong t cy v b mt cc dng c thit b
khc. rc khi s dng t cy v trng, cn bt n t ngoi trc 30 -
172
60 pht. Khi bt u thao tc, tt n t ngoi v bt h thng lc khng

kh.
1.3. K thut c bn trong phn tch kim nghim vi sinh vt
1.3.1. Phng php pha ch mi trng
thnh phn v ngun carbon, m, cht khong, cc yu t sinh

trng,... ngoi ra cn cha mt lng nc cn thit (khong 70 -
85%), c pH xc nh thch hp cho s pht trin ca vi sinh vt. rong
mt s mi trng c bit c th thm cc cht khng sinh, cc cht c
ch s sinh trng ca mt s vi sinh vt theo yu cu mc tiu ca th
nghim,...
da vo tnh cht vt
l mi trng v chia thnh 3 dng: lng (liquid media), rn (solid media)
v bn rn (semisolid media).
in nay, nhiu hng sn xut mi trng chuyn nghip sn

xut cc mi trng dng ng kh. Cc mi trng ny thng c
iu ch t cc ho cht tng hp tinh khit vi hm lng xc nh.
trng, v vy vic pha ch mi trng cn c thc hin chnh xc, cn

thn. Cch pha ch nh sau:
+ chun b mi trng cn phi cn ong chnh xc tng thnh

phn ca mi trng. Mt s thnh phn bt buc phi cn chnh xc
trn cn phn tch nh cc thnh phn vi lng,...
+ Vi mi trng lng: cn cc thnh phn, ho tan vo trong nc.
+ Vi mi trng rn: b sung thm cht lm rn nh thch, ng

thi phi gia nhit lm tan mi trng.
+ Yu cu mi trng phi trong d quan st, trng hp cn

thit phi lc qua giy lc, gc hoc than hot. u theo i tng yu
cu ca th nghim, mi trng c iu chnh n p quy nh bng
Cl 1 hoc a 1 . Mi trng c kh trng nhit v thi
gian thch hp ph thuc vo thnh phn ca mi trng. Vi cc mi
trng bnh thng, thng kh trng 121 oC (1atm) trong 15 - 20
pht.
- Mi trng ng kh: c pha ch n gin bng cch phi hp

mt lng cn thit mi trng ng kh vo nc, iu chnh p , ng
ng v kh trng. rong nhiu trng hp, c th khng cn iu chnh
pH.
173
rng hp c bit, phi ra ng nghim bn trong bng nc m v

x phng c s dng chi c ng nghim. X li 2 ln nc, ln u
bng nc my, sau bng nc ct loi tr x phng cn st li.
p ngc cc ng nghim ln r t ro nc, ch khng lau bng
khn.
ca dng c cha. hng thng vi cc bnh cha nh bnh cu, bnh

tam gic ch 1/3 - 1/2 dung tch, ng 5 ml mi trng lng trong ng
nghim, 5 - 7 ml i vi ng thch nghing.
1.3.2. Cc k thut kh trng dng c v mi trng
C nhiu phng php kh trng vi sinh vt: bng cc tc nhn l

ho nh nhit , bc x, lc,... c nhn kh trng c chn tu mc
ch v vt liu cn kh trng.
a) Kh trng bng nhit
Nhit cao c th tiu dit c cc vi sinh vt do tc dng lm

enzym ca vi sinh vt b bin tnh, lm mt nc v oxy ho cc t bo.
- Kh trng bng nhit kh: thng thng sy 170 oC trong 2 gi

hoc t. Dng c thu tinh (a petri, ng ht thu tinh,...) bn vi nhit
nn thng c kh trng bng phng php sy 180 oC trong 2 gi
trong t sy (ch cc ng ht cn c nht nt bng khng thm
nc u ht). Dng c thu tinh cn c gi kn trong giy hoc
giy nhm; ng ht c cho vo ng inox trc khi sy. Cc thanh gt
thu tinh c kh trng bng cch t vi cn 70 oC v cc que cy kim
loi c kh trng bng cch t trc tip trn ngn la.
- Kh trng bng nhit m: un si 100oC trong 10 pht dit t

bo sinh dng hoc hp bng hi nc 1atm, 121oC trong 15 - 30
pht tit trng hon ton. Phng php ny thng c dng
kh trng mi trng nui cy v dng c phu thut.
Phng php nhit m bng ni hp p lc 121 oC trong 15 - 30

pht thng c s dng cc thnh phn hu c ca mi trng
khng b chy, bin tnh v mi trng khng b mt nc. Phng php
ny da trn nguyn tc lm tng nhit bng hi nc bo ho di
p sut ln hn p sut bnh thng ca kh quyn.
- Phng php kh trng gin on (phng php yndall): mi

trng c hp 3 - 4 ln nhit khng qu 100 oC trong 30 - 40
pht, cch nhau 24 gi. ia 2 ln hp mi trng 28 - 32oC trong
24 gi cho bo t ny mm. Cc bo t no cn li sng st ny mm
s b dit ln hp tip theo.
174
- Phng php kh trng nhit thp (phng php Pasteur): un

cch thu mi trng 60oC trong 30 pht hoc 80oC trong 15 pht; sau
lm lnh t ngt di 10oC. Phng php ny khng dit c bo
t.
Mt s trng hp mi trng c cha cc cht khng bn vi nhit

nh vitamin, acid amin,... thng c kh trng bng 0,5atm trong
20 - 30 pht.
b) Kh trng bng mng lc
lng i qua, gi li cc vi khun v vi sinh vt c kch thc ln hn.

Phn chy qua phu c ng trong cc dng c v trng. rc khi
dng thit b lc v mng lc phi c kh trng. Phng php ny
thng c s dng kh trng trong cc trng hp c cc cht d
b oxy ho hoc khng bn vi nhit.
c) Kh trng bng bc x
C th dng tia X, tia gama, tia t ngoi kh trng. ia t ngoi

c dng nhiu nht kh trng cc bung pha ch, t cy vi sinh
vt; trong trng hp ny ch n t ngoi phi c chiu trc tip,
thng gc vi ni lm th nghim, cng sut v s lng n ph hp
vi din tch bung cy. n t ngoi t c tc dng vi nm, do
mun kh trng bung pha ch cn phi hp thm dng ho cht dit
nm.
d) Kh trng bng ho cht
hiu ho cht c th kim sot s tng trng ca vi sinh vt.

Ethylen oxyd, triethylen glycol,... c s dng kh trng, c ch s
pht trin ca vi sinh vt. S dng dung dch Cloramin B; Cloramin 2%
hoc dung dch phenol 0,5% x l bung v khun. it khun khng
kh bng dung dch formaldehyd (500 ml cho 1 lt nc).
1.3.3. Cc k thut thao tc v trng
rong kim nghim vi sinh vt, cc chng vi sinh vt cn c cy

vo nhiu mi trng khc nhau tng sinh, kho st c tnh sinh
trng ca vi sinh vt, cc th nghim sinh ho,... Vic cy chng cn
ch thc hin khng a cc vi sinh vt khc vo hay vi sinh vt
nhim vo mi trng, v vy cc thao tc cn ht sc cn thn loi
tr cc vi sinh vt gy nhim. m bo c c trng thi v trng
trc khi s dng, mi trng v cc dng c cn c kh trng thch
hp.
Cc thao tc v trng c thc hin trong khng gian v trng

c to ra bi ngn la n cn, hoc trong t cy v trng. goi ra
175
ngi tin hnh th nghim cn mang gng tay hoc st trng tay vi
cn 70o hoc cc dung dch tit khun, ng thi st trng mt bn thao
tc. Sau khi thc hin xong vic cy chng li tin hnh st trng tay,
mt bn tng t nh trn.
t nng u que cy trong ngn la v t

nh phn cn. Cm thng ng que cy ln cho que nng u. M nt
bng v a ngay que cy kh trng vo dng c cha ging. p
u que cy vo thnh ng nghim, bnh cha hoc t nh ln phn
mi trng khng cha vi sinh vt lm ngui que cy trc khi ly vi
sinh vt.
+ ng thch nghing: gay sau khi kh trng, t u cc ng

nghim ng mi trng rn cao to nghing sao cho chiu di
ca mi trng trong ng khng qu 2/3 chiu cao ng, thch khng
c chm vo nt bng. ngui.
+ a: nhit 45 - 55oC va hn ch s ngng t hi

nc trn np a petri, va to c b mt mi trng phng. a
trong t cy v trng, b dy mi trng trong a l 3 - 4mm.
2. TH GII HN NHIM KHUN
h gii hn nhim khun (hay th gii hn vi sinh vt) l mt th

nghim bt buc cho cc dc phm t nguyn liu n thnh phm
khng c tit trng trong qu trnh sn xut.
2.1. Mc ch
h nhim vi sinh vt nhm mc ch xc nh gii hn ti a ca

s lng vi khun hiu kh, vi nm c trong 1g (hoc 1 ml) ch phm
th. ng thi pht hin cc vi khun ch im v sinh quy nh khng
c c trong thuc l: Staphylococcus aureus, Pseudomonas
aeruginosa, Escherichia coli, cc loi Salmonella, vi khun k kh
Clostridia.
2.2. Nguyn tc
m s vi khun hiu kh, nm mc, nm men c trong dc phm

c th hin bng cc khun lc c trng trn a thch dinh dng
thch hp. Cn c vo cc c tnh hnh thi, sinh l, sinh ho ca tng
loi vi khun xc nh vi khun gy bnh. rn c s kt qu th
nghim nh gi cht lng ca thuc theo iu chun Dc in hoc
iu chun c s.
2.3. Phng php th xc nh gii hn ti a vi sinh vt
176
2.3.1. Chun b mi trng
a) Mi trng xc nh gii hn vi khun
Mi trng thch Casein - u tng:
Pepton casein 15,0g
Pepton u tng 5,0g
NaCl 5,0g
hch 15,0g
c ct 1000 ml
Mi trng thch thng:
Cao tht 5g
Pepton 10g
NaCl 5g
hch 18g
c ct va 1000 ml
b) Mi trng xc nh gii hn vi nm
Mi trng thch Sabouraud - Khng sinh:
Pepton 10g
Glucose 20g
hch 20g
c ct 1000 ml
hm 50mg cloramphenicol trong 1 lt mi trng trc khi tit trng

hoc dng benzyl penicillin, hoc tetracylin cho vo mi trng sau khi
tit trng.
177
2.3.2. Chun b mu th
Mu th theo quy nh chung c ly 10g (hoc 10 ml) th

nghim.
2.3.3. m s lng vi sinh vt
ml cht th nng thch hp sao cho

khng qu 300 khun lc vi khun v 100 khun lc vi nm trong 1 ml.
Thm 15 20 ml mi trng thch casein - u tng hoc mi trng
thch thng i vi a xc nh s lng vi khun v 15 20 ml thch
Sabouraud - khng sinh i vi a xc nh s lng vi nm
ngui di 45oC. ui cy 30 350C trong 1 2 ngy i vi a xc
nh s lng vi khun v 25 28oC trong 4 5 ngy i vi a xc
nh s lng vi nm.
V d: Xc nh s lng vi khun hiu kh, vi nm trong 1 ml b ph

ch khi l.
in hnh: Dng cn 70o st trng bn ngoi l. Ly 10 ml ch phm

pha vo 90 ml dung dch aCl 0,9% c nng pha long 10-1.
Pha long tip c nng 10-2. Cho vo mi hp petri 1 ml dung dch
cht th ca mi nng . hm 15 ml dung dch mi trng thch
thng un chy ngui khong 45 oC i vi a xc nh s lng
vi khun, v mi trng Sabouraud khng sinh i vi a xc nh s
lng vi nm. Xoay nh a cht th trn u vo mi trng. Mi
nng lm 2 a th song song. iu kin nui cy nh trn.
trn cc a th.
2.3.4. Tnh kt qu
ng s vi khun hiu kh, vi nm trong 1g (1 ml) c tnh theo

cng thc:
(Php th thc hin vi 2 nng ).
A1: s khun lc vi sinh vt trung bnh nng pha long k1.
A2: s khun lc vi sinh vt trung bnh nng pha long k2.
k1, k2: pha long.
Cc Dc in c quy nh: mu th c t hn 10 vi sinh vt/1g (1

ml) nu khng c khun lc mc trn a th nng 10-1.
178
Bng 22. Yu cu gii hn nhim khun
Mc Loi ch phm Yu cu
1 Cc ch phm dng cho Khng c cc vi khun c th sng li
bng v cc vt lot trong 1g ( ml) mu th.
su.
2 Cc ch phm dng ti ng s vi khun hiu kh khng qu 100

ch nh cha sng ty, trong 1g ( ml).
tn thng v cc mng
nhy (mi, hng, tai, m Mu th phi khng c nm v mc trong
o),... 1g ( ml).
3 Cc ch phm dng ti ng s vi khun hiu kh khng qu 500

ch cho da nh kem trong 1g ( ml).
bi, nc thm, du,
dung dch, bt,... Mu th phi khng c nm v mc trong
1g ( ml).
4 Cc ch phm dng ng s vi khun hiu kh khng qu 10 4

ung; qua trc trng; trong 1g ( ml).
thm qua da.
m v mc khng qu 100 trong 1g (
ml).
5 Cc ch phm c cha ng s vi khun hiu kh sng li c
cc nguyn liu c khng qu 5.104 trong 1g ( ml).
ngun gc thc vt,
ng vt khng th x l m v mc khng qu 500 trong 1g (
theo quy trnh lm gim ml).
lng vi khun.
3. TH V TRNG
3.1. Mc ch
Mc ch ca th v trng nhm pht hin s c mt ca vi khun, vi

nm trong cc ch phm nh dch tim truyn, mt s loi thuc tim,
thuc tra mt v cc dng c y t (dng c phu thut m theo tiu
chun ring cn phi v trng).
3.2. Nguyn tc
Vi sinh vt c trong ch phm th s pht trin trn cc mi trng

dinh dng thch hp; trong mi trng lng, vi sinh vt lm c mi
trng, to vng trn b mt hoc lng cn y ng nghim; trn mi
trng c vi khun, vi nm mc thnh cc khun lc c trng.
179
3.3. Mi trng
rong nhiu Dc in, pht hin vi khun hiu kh, k kh

thng dng mi trng hioglycolat lng v pht hin vi khun, vi
nm dng mi trng Casein - u tng lng. uy nhin, c th dng
cc mi trng khc cho th nghim, vi iu kin cc mi trng ny
thch hp cho s pht trin ca loi vi sinh vt cn pht hin nh mi
trng canh thang cao tht - pepton pht hin vi khun hiu kh; mi
trng Wilson - Blair pht hin vi khun k kh; mi trng Sabouraud
lng pht hin vi nm.
V d:
- Mi trng Thioglycollat:
Agar 0,75g
Yeast extract 5,0g
Pepton casein 15,0g
Glucose 5,5g
Na thioglycollat 0,5g
NaCl 2,5g
L-Cystine 0,5g
Resazurin 0,001g
c ct 1 lt
p tit trng 120oC trong 20 pht, ly ra lm lnh ngay, p = 6,9
- Mi trng canh thang casein- u tng lng:
Pepton casein 17,0g
Pepton u tng 3,0g
NaCl 5,0g
K2HPO4 2,5g
Glucose 2,5g
c ct 1000 ml
180
it trng 121o
3.4. Phng php th
h v trng bng phng php nui cy trc tip c k thut n

gin, nhng kh nng pht hin vi sinh vt gim khi s lng vi sinh vt
c t v phn phi trong mt th tch cht th ln. Phng php ny
khng thc hin c vi cc ch phm c tc dng c ch v cc cht
khng sinh, v khi th nghim cht th c cy trc tip vo cc mi
trng nui cy thch hp cho cc vi khun, vi nm.
3.4.1. Lng mu th dng trong th nghim
Lng mu th cn cy vo cc mi trng tu thuc vo tng loi

mu (bng 23).
Bng 23. Lng mu th dng cho th nghim nui cy trc tip
Lng ch phm
Lng ti thiu cho mt Th tch mi
trong mt n v ng
mi trng nui cy trng
gi
Cht lng:
h tch V < 1 ml on b mt ng 10 ml
1 ml ml 1/2 ng 15 ml
4 ml ml 2 ml 20 ml
20 ml ml 5 ml 40 ml
50 ml ml 10 ml 80 ml
ml hng 10% 100 ml
Cht rn:
Khi lng P < 50mg on b mt n v ng gi 20 ml
50mg < P < 200mg 1/2 khi lng ca mt n

v ng gi 40 ml
100mg 80 ml
ch du phi thm vo mi trng nui

cy 1% ween 80 hoc cc cht nh ho khc vi nng thch hp.
181
pepton 0,1% v trng theo t l 1/10 trc khi cy vo mi trng (dung

dch pepton cn thm ween 80 vi t l 1 ml/1lt).
3.4.2. K thut th
Kim tra v khun mu th l dc phm th dng dng c v

trng cy trc tip ch phm th vo cc mi trng pht hin vi khun,
vi nm theo s lng quy nh. Cht rn l dng bt c th cho trc tip
vo mi trng hoc lm thnh dung dch hay nh dch 1% sau cy
vo mi trng.
V d: h v trng thuc tim vitamin B1.
- Dng c th nghim: pipet 1 ml, ng nghim, kp st, n cn. Cc

dng c ra sch, tit trng kh 160 oC trong 2 gi trc khi dng.
- Pha ch mi trng: s dng mi trng canh thang v mi trng

Sabouraud lng. o tan tng cht vo nc, un nng cho tan hon
ton, iu chnh p bng a 1 hoc Cl 1 . iu chnh cho th
tch, phn chia mi trng vo ng nghim, mi ng 10 ml. it trng
bng ni hp autoclave 121oC, 1atm trong 15 - 20 pht.
- in hnh: St trng ng tim bng cn 70 o. B u ng tim bng

kp st v trng. t ton b thuc trong 1 ng cho vo 10 ml mi
trng canh thang v 1 ng khc c cy vo mi trng Sabouraud
(mi mi trng lm 2 ng). ng pht hin vi khun nui cy 30 - 35oC
t nht trong 4 ngy v ng pht hin vi nm nui cy 25 2oC t nht
trong 7 ngy. Mi loi mi trng lm 2 3 ng th song song.
3.4.3. Nhn nh kt qu
Trong sut thi gian nui cy, hng ngy phi kim tra cc ng nui
cy. u sau thi gian nui cy khng c s xut hin vi sinh vt, mu
th c coi l v trng. u c mt hoc nhiu ng c vi sinh vt phi
lm ln hai. ln hai, nu khng c vi sinh vt mc, ta kt lun l ch
phm v trng, trng hp c nhim vi sinh vt phi tin hnh phn lp
so snh vi vi sinh vt b nhim ln mt. u c vi sinh vt ging
ln mt th mu th khng v trng; nu c vi sinh vt khc ln mt, th
nghim c lm li ln ba vi s mu gp i. rong ln ba nu khng
c vi sinh vt, mu v trng; nu c vi sinh vt, mu th khng v trng.
4. TH CHT GY ST
rong kim nghim thuc tim hoc dung dch tim truyn u phi
nh gi ch tiu ny. in nay c 2 phng php th.
182
Lysat), thuc th ny khi gp cht gy st s to ra mt ta gel c th

pht hin c bng mt thng.
trn s tng thn nhit ca th sau khi tim vo tnh mch th dung dch
ca mu th. y l phng php th cht gy st hin nay Dc in
Vit am quy nh.
4.1. ng vt th nghim
Dng th kho mnh, trng thnh, c hoc ci khng c cha,

cn nng t 1,5kg tr ln, cha dng vo th nghim khc. C th dng
li nhng th th cht gy st nhng phi cho ngh hai ngy, nu ln
th trc m tnh; hoc hai tun l, nu ln th trc dng tnh. h
c nui dng ring trong chung bng thc n tng hp khng c
cht khng sinh. h chn nui phi sch s, thong, yn tnh v c
nhit n nh, chnh lch vi nhit phng th nghim khng qu
30C.
4.2. Thit b, dng c
hit k hay thit b in o nhit phi c chnh xc

0
0,1 C. Khi o nhit , nhit k c t su trong trc trng th t nht
5cm v ti thiu 5 pht. u l thit b in, phi yn trong trc trng
t nht 60 pht trc khi o nhit v gi nguyn v tr trong sut
thi gian th nghim.
Cc dng c thu tinh, bm tim, kim tim phi ra sch, trng nc

ct v loi cht gy st bng cch sy 2500C trong 30 pht, hoc
2000C trong 60 pht.
4.3. Tin hnh
h nghim c tin hnh ni yn tnh, trnh cc yu t kch

ng. m v nhit ca phng phi n nh. i th trn bn bng
cc gi kp c sao cho th vn t th thoi mi nht. Khng cho th
n trong thi gian th nghim.
1 - 3 ngy trc ngy tim mu th, kim tra s b vi nhng th

t tiu chun nhng khng c dng th cht gy st trong vng 2
tun trc . Sau khi th v tr n nh, o nhit th 3 ln, mi ln
0,60C khng dng vo th nghim.
rong ngy tim mu th, th n nh trong phng th nghim t

nht 90 pht trc khi tim. gay trc lc tim 40 pht, o nhit th
2 ln cch nhau 30 pht. hit ban u ca th l gi tr trung bnh
ca hai ln o ny. Ch nhng th c nhit chnh lch gia hai ln o
183
khng qu 0,20C v nhit ban u trong khong t 380C 390C mi

dng tim mu. Mi ln th c tim cho mt nhm 3 th c nhit
khc nhau khng qu 10C.
o nhit th cch nhau khong 30 pht/ln, trong 3 gi sau khi

tim. hit ti a sau khi tim l nhit cao nht o c trong
khong thi gian ny.
Liu lng v cch x l mu c quy nh trong cc chuyn lun

ring. u mu th l dung dch nhc trng th phi ng trng
bng natri clorid khng c cht gy st. h tch dng tim c th
thay i t 0,5 - 10 ml/kg th. Khi tim vi th tch ln, nn nng dung
dch n 380C.
hi gian tim cho mt th khng ko di qu 4 pht. rng hp

dng cc thit b o nhit c gi t chng trnh, gi nhit k trong
trc trng th trong sut thi gian th nghim. o nhit th nhng
khong thi gian t nht 30 pht v nh gi kt qu thu c.
4.4. nh gi kt qu
p ng ca mi th l hiu s ca nhit ti a sau khi tim mu

th v nhit ban u.
p ng ca th bng 0 nu nhit ti a sau khi tim thuc em

th ch bng hoc thp hn nhit ban u.
u khng c th no c p ng bng hoc ln hn 0,6 0C v nu

tng s p ng ca 3 th khng vt qu 1,40C th mu th t yu
cu v th cht gy st.
u 1 th tr ln c p ng bng hoc ln hn 0,60C, hoc nu

tng s p ng ca 3 th ln hn 1,4 0C th phi lm li th nghim trn
5 con th khc.
u khng qu 3 trong s 8 th ca hai ln th nghim c p ng

bng hoc ln hn 0,60C v nu tng s p ng ca 8 th khng vt
qu 3,70C th mu th t yu cu v th cht gy st.
T LNG GI V BI TP
1. rnh by cc quy tc an ton trong phng kim nghim vi sinh.
2. rnh by phng php pha ch mi trng nui cy vi sinh vt.
3. M t cc phng php kh trng.
4. rnh by cch kh trng bng ni hp p lc.
184
5. rnh by cch tin hnh th cht gy st.
6. rnh by th nghim th v trng bng phng php nui cy

trc tip.
7. u mc ch, nguyn tc ca th nghim th v trng v th gii

hn vi sinh vt.
8. rnh by th nghim m s lng vi sinh vt trong 1g (1 ml)

dc phm bng phng php a thch.
9. rnh by phng php xc nh s lng ti a vi khun hiu kh,

vi nm trong mt gam vin lc v hon.
10. rnh by phng php th v trng thuc tim vitamin B1.
11. Chn cu tr li ng bng cch khoanh trn ch ci u cu

c chn i vi quy nh gii hn cho php v nhit ca
th khi kim tra ch tiu ch nhit t i vi dung dch tim truyn:
a) Ca tng th:
A. Ln hn 0oC v khng qu 0,6oC.
B. Khng qu 0,6oC.
C. Khng qu 0,5oC.
D. 0 0,6oC.
b) Ca ba th:
A. Ln hn 0oC v khng qu 1,6oC.
B. Khng qu 1,5oC.
C. Khng qu 1,4oC.
D. Khng qu 1,6oC.
P N
Bi 1 Bi 4
5. a) A, D 7. 1,0619
185
b) B, C 8. 1,0848
6. a) C 13. a) A: cam; B: vng
b) B b) A: ; B: vng
Bi 2 c) A: vng; B:
7. a) cao hn d) A: trng; B:
b) c tnh thc t 14. a) A
c) chnh xc b) B
8. a) A c) D
b) D 15. a) A
c) B b) D
d) D Bi 5
9. a) B 4. a) pha lng
b) C b) lc ly tm
c) A c) dung mi
10. a) C 13. 0,74V v 0,62V
b) A 14. 0,22V
Bi 3 15. 0,276%
4. m lng: 0,02756g/l 16. ml
Sai s tng i: 2,217% 17. a) A
Kt qu x l thng k: b) B
= 0,92756 0,000611(g/l) 18. a) B
5. A: phn hu mu bng acid mnh b) C
B: cht hu c c) B
C: t 19. a) A
186
D: nung b) C
c) B
Bi 7 Bi 10
9. 1,134 4. 0,5157mg/ ml. t
10. 1,458 7. 0,875%. t
11. 19,89 9. t (14,65%)
12. a) C 10. a) C
b) B b) D
c) C c) B
13. a) A 11. a) A
b) B b) D
14. a) gii phng c) A
b) tan r 12. a) C
Bi 8 b) A
3. a) D Bi 11
b) C 4. a) B
c) D b) C
4. a) C c) A
b) A d) C
5. a) B 5. a) A
b) B b) B
c) A c) D
d) D 6. A
6. a) A Bi 12
187
b) D 4. a) C
7. t b) B
Bi 9 c) C
3. a) D 5. a) A
b) C b) C
c) C c) B
d) B 6. a) C
4. a) A b) A
b) B Bi 13
c) D 11. a) A
5. D, E b) C
7. Khng t
8. t (99,45%)
188
Ph lc 1
BNG NGUYN T LNG CC NGUYN T
heo ti liu ca Lin on quc t v ho hc thun tu v ng

dng xut bn nm 1989 (Pure App.Chem.1991,63,978.)
Tn nguyn t * K hiu Nguyn t s Nguyn t lng
Argon Ar 18 39,948
Arsen As 33 74,9216
Bc (Argentum) Ag 47 107,8682
Bari Ba 56 137,327
Beryli Be 4 9,0122
Bismuth Bi 83 208,9804
Bor B 5 10,811
Brom Br 35 79,904
Cadmi Cd 48 112,411
Cesi Cs 55 132,9054
Calci Ca 20 40,078
Carbon C 6 12,011
Ceri Ce 58 140,115
Ch (Plumbum) Pb 82 207,2
Clor Cl 17 35,4527
Crom Cr 24 51,9961
Cobalt Co 27 58,9332
ng (Cuprum) Cu 29 63,546
Dysprosi Dy 66 162,50
Erbi Er 68 167,26
Europi Eu 63 151,965
Fluor F 9 18,9984
gadolini gd 64 157,25
189
gali ga 31 69,723
germani ge 32 72,61
Hafni Hf 72 178,49
Heli He 2 4,0026
Holmi Ho 67 163,9303
Hydrogen H 1 1,0079
Indi In 49 114,82
Iod I 53 126,9045
Iridi Ir 77 192,22
Kali K 19 39,0983
Km (Zincum) Zn 30 65,39
Krypton Kr 36 83,80
Lanthan La 57 138,9055
Lithi Li 3 6,941
Luteti Lu 71 174,967
Lu hunh (Sulfur) S 16 32,066
Magnesi Mg 12 24,3050
Mangan Mn 25 54,9381
Molybden Mo 42 95,94
Natri Na 11 22,9898
Neodymi Nd 60 144,24
Neon Ne 10 20,1797
Nhm (Aluminium) Al 13 26,9815
Nickel (Niccolum) Ni 28 58,6934
Niobi Nb 41 92,9064
Nitrogen N 7 14,0067
Osmi Os 76 190,2
190
Oxygen O 8 15,9994
Paladi Pd 46 106,42
Phosphor P 15 30,9738
Platin Pt 78 195,08
Praseodymi Pr 59 140,9077
Rheni Re 75 186,207
Rhodi Rh 45 102,9055
Rubidi Rb 37 85,4678
Rutheni Ru 44 101,07
Samari Sm 62 150,36
St ( ron) Fe 26 55,847
Scandi Sc 21 44,9559
Selen Se 34 78,96
Silic (Silicium) Si 14 28,0855
Stibi (Stibium) Sb 51 121,757
Stronti Sr 38 87,62
Tantal Ta 73 180,9479
Techneti Tc 43 (97)
Telur Te 52 127,60
Terbi Tb 65 158,9253
Thali Tl 81 204,3833
hic (Stanium) Sn 50 118,70
Thori Th 90 232,0381
Thuli Tm 69 168,9342
hu ngn Hg 80 200,59
(Hydrragyrum)
Titan Ti 22 47,88
Uran U 92 238,0289
191
Vanadi V 23 50,9415
Vng (Aurum) Au 79 196,9665
Wolfram W 74 183,85
Xenon Xe 54 131,29
Yterbi Yb 70 173,04
Ytri Y 39 88,9059
Zirconi Zn 40 91,224
Ph lc 2
CC PHN NG NH TNH MT S ION
Acetat
A. un nng ch phm vi cng mt lng acid oxalic ( ). i xng ra

c mi acid acetic.
B. o tan khong 30 ml ch phm trong 3 ml nc, hoc ly 3 ml dung

dch theo ch dn trong chuyn lun. hm 0,25 ml dung dch lanthan
nitrat ( ), 0,1 ml dung dch iod 0,1 v 0,05 ml dung dch amoniac 2
M ( ). un nng hn hp cn thn n si, sau vi pht xut hin
ta mu xanh hay mu xanh thm.
Amoni (mui)
A. o tan khong 0,2g ch phm trong 2 ml nc, hoc ly mt lng

dung dch theo ch dn trong chuyn lun, thm 2 ml dung dch natri
hydroxyd 2 M ( ), un nng, s xng ra kh c mi c bit v lm
xanh giy qu thm nc.
B. o tan khong 10mg ch phm trong 5 ml nc, hay mt lng

dung dch theo ch dn trong chuyn lun, thm 0,2 ml thuc th
essler ( ), hn hp c mu vng hay ta vng nu.
Bc (mui)
A. o tan khong 10 ml ch phm trong 5 ml nc, hoc ly mt lng

dung dch theo ch dn trong chuyn lun, thm 3 git dung dch acid
hydrocloric 10% ( ) s xut hin ta trng ln nhn, ta ny khng
tan trong acid nitric long ( ) nhng tan trong dung dch amoniac
(TT).
192
B. o tan 20mg ch phm trong 5 ml nc, hoc ly mt lng dung

dch theo ch dn trong chuyn lun, thm mt lng dung dch
amoniac ( ) s c ta mu nu xm, tip tc thm dung dch
amoniac ( ), ta s tan. Sau thm vi git formalin ( ), un
nng dung dch s c ta bc kim loi bm vo thnh ng nghim
(phn ng trng gng).
Bari (mui)
A. Ly mt lng dung dch mui bari nh ch dn trong chuyn lun,

thm vi git acid sulfuric long ( ) s xut hin ta trng, ta ny
khng tan trong acid hydrocloric 10% (TT) v acid nitric long (TT).
B. Dng mt dy bch kim hoc a thu tinh ly mt lng cht th t

trn ngn la khng mu, ngn la s nhum thnh mu xanh lc hi
vng, khi nhn qua knh thu tinh mu lc ngn la s c mu xanh.
Benzoat
A. Ly 1 ml dung dch trung tnh 10% ca ch phm, hoc mt lng

ch phm theo ch dn trong chuyn lun, thm 0,5 ml dung dch st
( ) clorid 10% ( ) s xut hin ta vng thm, ta ny tan trong
ether (TT).
B. Ly khong 0,2g ch phm hoc mt lng ch phm theo ch dn

trong chuyn lun, lm m bng 0,2 ml n 0,3 ml acid sulfuric ( )
v un nng nh y ng nghim, s c cc tinh th thng hoa
trng bm thnh trong ca ng.
C. o tan 0,5g ch phm trong 10 ml nc hoc dng 10 ml dung dch

theo ch dn trong chuyn lun, thm 0,5 ml acid hydrocloric ( ), s
cho ta. Kt tinh li ta trong nc ri lm cho kh di p sut gim,
ta thu c c nhit chy t 120oC n 124oC.
Bismuth (mui)
A. hm 10 ml acid hydrocloric 10% ( ) vo 0,5g ch phm, hoc dng

10 ml dung dch theo ch dn trong chuyn lun. un si trong 1 pht,
ngui ri lc nu cn. hm 20 ml nc vo 1 ml dung dch thu
c trn, xut hin ta trng hay hi vng, ta ny s chuyn
thnh nu khi thm 0,05 n 0,1 ml dung dch natri sulfid ( ).
B. hm 10 ml dung dch acid nitric 2M ( ) vo 40 n 50mg ch phm,

hoc dng 10 ml ch phm c x l theo ch dn trong chuyn
lun. un si trong 1 pht, ngui ri lc nu cn. hm 2 ml dung
dch thioure 10% ( ) vo 5 ml dch lc thu c trn, xut hin
mu vng da cam hay ta da cam. hm 4 ml dung dch natri fluorid
2,5% ( ), dung dch khng c mt mu trong vng 30 pht.
193
Borat
A. o tan khong 0,1g ch phm vo 0,1 ml acid sulfuric ( ) trong mt

chn s, thm 3 ml methanol ( ), trn u ri chm la vo hn
hp, hn hp chy vi ngn la mu lc.
B. Ly 5 ml dung dch ch phm 10%, thm 0,5 ml acid hydrocloric long

( ) v 0,5 ml cn ngh (C ), s cho mu nu; thm 1 ml dung dch
natri hydroxyd 10% ( ), mu nu chuyn thnh lam hay lc.
Bromid
A. o tan mt lng ch phm c cha khong 3mg ion bromid trong 2

ml nc, hoc dng 2 ml dung dch theo ch dn trong chuyn lun.
Acid ho bng acid nitric long ( ) v thm 0,4 ml dung dch bc
nitrat 4% ( ). Lc v yn s to ta ln nhn mu vng nht. Lc
ly ta, ra ta ba ln, mi ln vi 1 ml nc. Phn tn ta trong 2 ml
nc, thm 1,5 ml dung dch amoniac 10 M ( ) ta kh tan.
B. o tan mt lng ch phm c cha khong 5mg ion bromid trong 2

ml nc, hoc ly mt lng dung dch theo ch dn trong chuyn
lun, acid ho dung dch bng acid sulfuric long (TT), thm 1 ml
nc clo ( ) v 2 ml cloroform ( ), lc. Lp cloroform s c mu
nu.
Calci (mui)
A. Ly khong 20mg ch phm, hoc mt lng ch phm theo ch dn

trong chuyn lun, ho tan trong 5 ml dung dch acid acetic 5 M ( ),
thm 0,5 ml dung dch kali ferocyanid ( ), dung dch vn trong, thm
khong 50mg amoni clorid ( ), to thnh ta kt tinh trng.
B. hm vo dung dch ch phm theo ch dn trong chuyn lun vi git

dung dch amoni oxalat 4% ( ), to thnh ta trng, ta ny t tan
trong acid acetic 6 M ( ), nhng tan trong acid hydrocloric ( ).
Ch (mui)
A. o tan 0,1g ch phm trong 1 ml dung dch acid acetic 5 M ( ),

hoc ly 1 ml dung dch theo ch dn trong chuyn lun, thm 2 ml
dung dch kali cromat ( ), ta vng s to thnh, ta ny tan trong
dung dch natri hydroxyd 10 M ( ).
B. o tan 50mg ch phm trong 1 ml dung dch acid acetic 5 M, hoc 1

ml dung dch theo ch dn trong chuyn lun. hm 10 ml nc v 0,2
ml dung dch kali iodid 10% ( ), ta vng s to thnh; un si 1 n
2 pht cho ta tan ra, ngui, ta li xut hin nh nhng mnh
vng.
194
Citrat
A. o tan khong 0,1g ch phm trong 2 ml nc, nu cn c th trung

tnh ho dung dch bng amoniac ( ), hoc dng mt lng dung
dch theo ch dn trong chuyn lun. hm 1 ml dung dch calci clorid
10% ( ), dung dch vn trong. un si dung dch s xut hin ta
trng, tan trong acid acetic 6 M ( ).
B. o tan khong 0,1g ch phm trong 2 ml nc, hoc ly 2 ml dung

dch theo ch dn trong chuyn lun, thm vi git dung dch acid
sulfuric long ( ), un n si, sau thm vi git dung dch kali
permanganat ( ), lc, mu tm s bin mt. Chia dung dch lm hai
phn, mt phn dung dch thm vi git dung dch thu ngn ( ) sulfat
( ), phn th hai thm vi git dung dch nc brom ( ), ta trng
c to thnh c hai dung dch.
Clorid
A. o tan mt lng ch phm tng ng vi 2mg ion clorid trong 2 ml

nc hoc dng 2 ml dung dch theo ch dn trong chuyn lun. Acid
ho bng dung dch acid nitric 2 M ( ), thm 0,4 ml dung dch bc
nitrat 2% ( ). Lc v yn, s to ta trng ln nhn. Lc ly ta,
ra ta 3 ln, mi ln vi 1 ml nc, thm vo ta trong 2 ml nc, v
thm 1,5 ml dung dch amoniac 10 M, ta tan ra d dng.
B. Cho vo ng nghim mt lng ch phm tng ng khong t 10

n 50mg ion clorid ( ), un nng, s gii phng kh clo c mi c
bit, kh ny lm xanh giy tm h tinh bt c kali iodid (C ) thm
nc.
ng (mui)
A. o tan khong 10mg ch phm trong 2 ml nc, hoc dng 2 ml

dung dch theo ch dn trong chuyn lun, thm vi git dung dch kali
ferocyanid ( ), s c ta mu nu khng tan trong acid acetic
(TT).
B. o tan khong 10mg ch phm trong 2 ml nc, hoc dng 2 ml

dung dch theo ch dn trong chuyn lun. hm vi git dung dch
amoniac ( ), s c ta mu xanh, ta ny tan trong thuc th qu
tha to thnh dung dch mu xanh lam thm.
Iodid
A. o tan mt lng ch phm tng ng khong 4mg ion iodid trong

2 ml nc, hoc dng 2 ml dung dch theo ch dn trong chuyn lun.
Acid ho bng dung dch acid nitric 2 M ( ), thm 0,4 ml dung dch
bc nitrat 4% ( ). Lc v yn, c ta to thnh mu vng nht,
195
ln nhn. Lc ly ta. Phn tn ta trong 2 ml nc, thm 1,5 ml dung

dch amoniac 10 M ( ), ta khng tan.
B. o tan mt lng ch phm tng ng vi 4mg ion iodid trong 2 ml

nc, hoc dng 2 ml dung dch st ( ) clorid 3% ( ), 2 git acid
hydrocloric ( ), 1 ml cloroform ( ) v lc, yn. Lp cloroform c
mu tm.
Kali (mui)
A. o tan 0,1g ch phm trong 2 ml nc, hoc dng 2 ml dung dch

theo ch dn trong chuyn lun. hm 1 ml dung dch natri carbonat
10% ( ) ri un nng, khng to thnh ta. hm vo trong lc nng
0,05 ml dung dch natri sulfid ( ), khng to thnh ta. Lm ngui
trong nc v thm 2 ml dung dch acid tartric 15% ( ). yn,
to thnh ta kt tinh trng.
B. o tan khong 40mg ch phm trong 1 ml nc hoc dng 1 ml

dung dch theo ch dn trong chuyn lun. hm 1 ml dung dch acid
acetic 2 M ( ) v 1 ml dung dch natri cobal trinitrit 10% ( ) mi
pha, to thnh ta vng hay da cam.
Km (mui)
o tan 0,1g ch phm trong 5 ml nc, hoc dng 5 ml dung dch

theo ch dn trong chuyn lun. hm 0,2 ml dung dch natri hydroxyd
10 M ( ), to thnh ta trng, ta ny tan khi thm 2 ml natri
hydroxyd 10 M ( ). hm 10 ml dung dch amoni clorid ( ), dung
dch vn trong, thm 0,1 ml dung dch natri sulfid ( ), ta bng trng
c to thnh.
Magnesi (mui)
o tan khong 15mg ch phm trong 2 ml nc, hoc ly 2 ml dung

dch theo ch dn trong chuyn lun. hm 1 ml dung dch amoniac 6
M ( ), to thnh ta trng, ta ny tan khi thm 1 ml dung dch
amoni clorid ( ). hm 1 ml dung dch dinatri hydrophosphat ( ), s
c ta kt tinh trng.
Natri (mui)
A. Dng mt dy bch kim hay a thu tinh, ly mt ht cht th hay

mt git dung dch ch phm, a vo ngn la khng mu, ngn la
s nhum thnh mu vng.
B. o tan khong 50mg ch phm trong 2 ml nc, hoc ly 2 ml dung

dch theo ch dn trong chuyn lun. Acid ho dung dch bng acid
acetic long ( ), thm 1 ml dung dch magnesi uranyl acetat ( ), c
196
thnh ng nghim bng mt a thu tinh (nu cn), s c ta kt tinh

vng.
Nhm (mui)
o tan khong 0,1g ch phm trong 2 ml nc, hoc dng 2 ml dung

dch ch dn trong chuyn lun. hm tng git dung dch amoniac
( ) cho ti khi to ta keo trng, ta ny chuyn thnh khi thm
vi git dung dch alizarin S ( ).
Nitrat
A. o tan 0,1g ch phm trong 2 ml nc, hoc dng 2 ml dung dch

theo ch dn trong chuyn lun. hm t t 2 ml acid sulfuric ( ),
trn v ngui.
Cho cn thn (khng trn) dc theo thnh ng nghim 1 ml dung dch
st ( ) sulfat ( ). min tip gip gia hai cht lng c mt vng
mu nu.
B. rn 0,1 ml nitrobenzen ( ) vi 0,2 ml acid sulfuric ( ), thm mt

lng ch phm tn nh tng ng vi khong 1mg ion nitrat
hoc mt lng dung dch theo ch dn trong chuyn lun, yn 5
pht, lm lnh trong nc vi pht, va lc va thm t t 5 ml
nc, sau 5 ml dung dch natri hydroxyd 10 M ( ) v 5 ml aceton
( ), lc ri yn. Lp cht lng trn c mu tm thm.
Oxalat
A. o tan khong 0,1g ch phm trong 5 ml nc, hoc dng 5 ml

dung dch theo ch dn trong chuyn lun. hm 0,5 ml dung dch
calci clorid 10% ( ), to ta trng, ta tan trong acid v c, khng tan
trong dung dch acid acetic 6 M ( ).
B. o tan khong 0,1g ch phm trong 5 ml nc, hoc dng 5 ml

dung dch theo ch dn trong chuyn lun. Acid ho dung dch bng
acid sulfuric 10% ( ), dung dch ny s lm mt mu dung dch kali
permanganat ( ) khi un nng.
Peroxyd
A. h 1 git dung dch ch phm vo 10 ml dung dch acid sulfuric 2%

( ), thm 2 ml ether ( ) v 1 git dung dch kali dicromat ( ), lc.
lp ether hin mu xanh.
B. Ly 1 ml dung dch ch phm, acid ho nh bng acid sulfuric 10%

( ), thm tng git dung dch kali iodid ( ), s gii phng iod, lm
xanh h tinh bt (C ).
Phosphat
197
A. o tan khong 50mg ch phm trong 3 ml nc, hoc dng 3 ml

dung dch theo ch dn trong chuyn lun. Acid ho dung dch bng
acid nitric long ( ), thm 2 ml dung dch amoni molybdat ( ) s
hin ta vng.
B. o tan khong 0,1g ch phm trong 2 ml nc, hoc dng 2 ml

dung dch theo ch dn trong chuyn lun. rung tnh ho dung dch
bng acid nitric long ( ) hoc dung dch natri hydroxyd ( ). hm
1 ml dung dch bc nitrat 4% ( ) s to ta vng, mu ca ta khng
thay i khi un si, ta tan khi thm dung dch amoniac 10 M ( ).
St (II) (mui)
o tan mt lng ch phm tng ng vi 10mg st ( ) trong 1 ml

nc, hoc dng 1 ml dung dch theo ch dn trong chuyn lun.
hm 1 ml dung dch kali fericyanid ( ), to ta xanh lam, ta ny
khng tan trong dung dch acid hydrocloric 2 M ( ).
St (III) (mui)
A. o tan mt lng ch phm c cha khong 0,1mg st ( ) trong 3

ml nc, hoc dng 3 ml dung dch theo ch dn trong chuyn lun.
hm 1 ml dung dch acid hydrocloric 2 M ( ) v 1 ml dung dch kali
thiocyanat ( ), dung dch c mu . Dng 2 ng nghim, cho vo
mi ng 1 ml dung dch thu c trn. Mt ng cho thm 5 ml alcol
amylic ( ) hoc ether ( ), lc v yn, lp dung mi c mu
hng. Cho vo ng nghim kia 3 ml dung dch thu ngn ( ) clorid
( ), mu s bin mt.
B. o tan mt lng ch phm tng ng vi 1mg st ( ) trong 1 ml

nc, hoc dng 1 ml dung dch theo ch dn trong chuyn lun.
hm 1 ml dung dch kali ferocyanid ( ) s to ta xanh lam, ta ny
khng tan trong dung dch acid hydrocloric 2 M ( ).
Sulfat
A. Ho tan 45mg ch phm trong 5 ml nc, hoc dng 5 ml dung dch

theo ch dn trong chuyn lun, thm 1 ml dung dch acid hydrocloric
2 M ( ) v 1 ml dung dch bari clorid 5% ( ), s c ta trng c
to thnh.
B. hm 0,1 ml iod 0,1 vo hn dch thu c phn ng trn, hn

dch c mu vng (phn bit vi sulfid v dithionit) nhng mt mu khi
thm tng git dung dch thic ( ) clorid ( ) (phn bit vi iodat).
un si hn hp, khng c to thnh ta c mu (phn bit vi
selenat v tungstat).
Sulfid
198
o tan 0,1g ch phm trong 2 ml nc, hoc dng 2 ml dung dch

theo ch dn trong chuyn lun. hm 1 ml acid hydrocloric 10%( ),
kh bay ra c mi ca hydrosulfid, kh ny s lm nu hoc en giy
tm ch acetat (C ) thm nc.
Thu ngn (mui)
A. h 2 - 3 git dung dch th ln mt ming ng phi ( ) c c

sch, s xut hin vt hoen mu xm ti; vt ny sng ra khi c lau
nh. t nng phi ng trong ng nghim th vt hoen s mt.
B. o tan khong 0,10g ch phm trong 2 ml nc, nu l thu ngn

oxyd th ho tan trong 2 ml acid hydrocloric 10% ( ), hoc dng 2 ml
dung dch theo ch dn trong chuyn lun. hm tng git dung dch
kali iodid ( ) s cho ta , ta tan trong thuc th qu tha (i vi
mui thu ngn ( )).
u l mui thu ngn ( ), khi thm tng git dung dch kali iodid ( )
s cho ta vng, sau chuyn sang mu lc.
Ph lc 3
PHN Ng MU CA CC PENICILIN
V CEPHALOSPORIN
A. Cho 2mg ch phm vo mt ng nghim (kch thc 15cm 1,5cm),

lm m vi 0,05 ml nc, thm 2 ml acid sulfuric ( ). Lc u hn
hp v quan st mu ca dung dch. t ng nghim trong cch thu
si trong mt pht v li quan st mu. Mu sc ca dung dch c
quy nh trong bng di y.
B. Lp li cch th nh phn ng A, nhng thay 2 ml acid sulfuric (TT)

bng 2 ml dung dch formaldehyd trong acid sulfuric ( ). Mu sc
ca dung dch c quy nh trong bng di y.
Phn ng mu ca cc penicilin v cephalosporin
Acid
Dung dch
sulfuric
Acid Dung dch formaldehyd
(TT)
Tn mu sulfuric formaldehyd trong trong acid
sau 1
(TT) acid sulfuric (TT) sulfuric (TT) sau
pht
1 pht 100oC
100oC
Amoxicilin natri u nh khng Vng sm
mu
Amoxicilin u nh khng Vng sm
199
trihydrat mu
Ampicilin u nh khng Vng sm

mu
Ampicilin natri u nh khng Vng sm

mu
Ampicilin u nh khng Vng sm

trihydrrat mu
Benzathin u nh khng u
penicilin mu
Benzylpenicilin u nh khng u
kali mu
Benzylpenicilin u nh khng u
natri mu
Cephalexin Vng nht Vng sm
Cephaloridin Vng u nu
nht nh
khng
mu
Cephalothin Vng ng nu
natri (mu nu
chuyn
nhanh)
Cloxacilin natri Vng xanh l nht Vng
Dicloxacilin Vng xanh l nht Vng

natri
Flucloxacilin Vng xanh l nht Vng

natri
Phenoxymethyl u u sm
penicilin
Phenoxymethyl u u sm
penicilin kali
Procain u u u nh khng u
penicilin nh nh mu
khng khng
mu mu
200
TI LIU THAM KHO
1. rng i hc Dc i (1998). Ho phn tch II.
2. rng i hc Y dc thnh ph Ch Minh (2001). gio trnh

kim nghim thuc.
3. B Y t (2002). Dc in Vit Nam III. XB Y hc. i
4. B Y t (2002). Cc vn bn qun l nh nc trong lnh vc Dc.

XB Y hc. i.
5. rng i hc Dc i (2004). Kim nghim thuc.
6. guyn Linh hc (2002). Phng php phn tch vi sinh vt trong

nc, thc phm v m phm. h xut bn gio dc.
7. B mn o phn tch - rng i hc Dc i (1998). Thc

tp Ho phn tch. i liu lu hnh ni b - rung tm thng tin th vin
i hc Dc i.
8. British Pharmacopoeia (2005).
9. Harold J. Benson (1998). Microbiological applications laboratory

manual in general microbiology. 7th edition. Mcgraw Hill.
10. United Stated Pharmacopoeia XXIX (2006).
201

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Trng Trung Cp Bch khoa Si Gn Gio trnh KIM NGHIM

KIM NGHIM THUC

Thc hin mt s iu ca Lut Gio dc, B Y t ban hnh

Sch KIM NGHIM THUC c bin son da trn chng trnh

Sch KIM NGHIM THUC c Hi ng chuyn mn thm nh

sch phi c chnh l, b sung v cp nht.

B Y t xin chn thnh cm n cc tc gi v Hi ng chuyn mn

Ln u xut bn, chng ti mong nhn c kin ng gp ca

- Trnh by c s cn thit phi kim tra cht lng thuc.

- Bit c ni dung, h thng t chc kim tra cht lng thuc ca

1. CHT LNG V KIM TRA CHT LNG

1.1. Thuc v yu cu cht lng

1.1.1. Khi nim v thuc

- Phng bnh, cha bnh.

- Phc hi, iu chnh chc nng c th.

- Lm gim triu chng bnh.

- Phc hi hoc nng cao sc kho.

- Lm mt cm gic mt b phn hay ton thn.

- Lm nh hng qu trnh sinh sn.

- Lm thay i hnh dng c th.

huc lu hnh trn th trng a phn l cc tn dc v thuc y

1.1.2. Cht lng thuc v yu cu cht lng

Cht lng ca mt thuc l tng hp cc tnh cht c trng ca

- C hiu lc phng bnh v cha bnh.

- Khng c hoc t c tc dng c hi.

- n nh v cht lng trong thi hn xc nh.

huc l sn phm hng ho c bit, c quan h trc tip n sc

Mc tiu ca m bo cht lng trn ch c coi l t khi no

- huc c cha ng cc thnh phn theo t l quy nh ca cng

- huc c php sn xut v sn xut theo ng cc quy trnh

- C tinh khit t yu cu quy nh.

- huc c ng gi trong cc ng v bao gi vi nhn

- huc c bo qun, phn phi, qun l theo quy nh cht

t cc mc tiu trn, cn phi c nhiu yu t, trong 3 yu t

a) Thc hnh sn xut thuc tt (GMP - Good Manufacture Practice)

hm sn xut ra c thuc theo d kin v t tiu chun k

5) guyn liu ban u.

8) thng kim tra cht lng.

10) s phn phi.

11) Cc khiu ni v bo co tai bin dng thuc.

b) Thc hnh kim nghim thuc tt (GLP - Good Laboratory

2) thng cht lng.

4) hit b phn tch v hiu chnh thit b phn tch.

5) huc th v cht i chiu.

6) iu chun cht lng v phng php phn tch.

10) An ton trong phng th nghim.

c) Thc hnh bo qun thuc tt (GSP - Good Storage Practice)

hm gim st, kim tra cht ch thuc m bo cht lng n

2) h kho v trang thit b.

4) Cc quy trnh bo qun.

6) i hng (vn chuyn bng cch gi hng).

1.2. Kim tra cht lng thuc (Drug quality control)

1.2.1. Khi nim

Kim tra cht lng thuc l qu trnh o, xem xt, th nghim mt

- y c phi l thuc cn kim tra khng?

- C m bo hot lc hay hm lng ng k khng?

- C t tinh khit theo yu cu khng?

- C b phn hu hay bin cht khng?

- bao gi, nhn c ng quy cch khng?

h vy, mc tiu c bn ca cng tc kim tra cht lng thuc l:

- ngi s dng c dng thuc m bo cht lng, t hiu

rong ngnh Y t quy nh: t c cc thuc v nguyn liu lm

1.2.2. Khi nim v thuc t v khng t tiu chun, thuc gi