MT S PHNG PHP SC K DNG TRONG KIM NGHIM

H v tn hc vin:
Nguyn Mai Hng Lp CH 21 M hc vin: 1611060
Nguyn Thnh Nam Lp CH 21 M hc vin: 1611076

BI TP
(Ti liu tham kho: Lun vn, Kha lun)
Cu 1: nh lng bng phng php chun ngoi.
nh lng captopril trong nguyn liu bng phng php HPLC c tin hnh nh sau:
Dung dch chun: Cn chnh xc khong 50,0mg captopril chun i chiu (nng
95,3%, hm m 3%) vo bnh nh mc 50ml, ha tan v nh mc bng dung mi pha
ng, lc u. Ht chnh xc 1,00ml dung dch trn, cho vo bnh nh mc 10ml, ha tan
v nh mc bng dung mi pha ng, lc u. Dung dch trong bnh c lc qua mng
0,45m, dch lc thu c tin hnh tim sc k.
Dung dch th: Cn chnh xc lng bt captopril trong nguyn liu ng vi 50,0mg
captopril cho vo bnh nh mc 50ml, ha tan v nh mc bng dung mi pha ng, lc
u. Ht chnh xc 1,00ml dung dch trn, cho vo bnh nh mc 10ml, ha tan v nh
mc bng dung mi pha ng, lc u. Dung dch trong bnh c lc qua mng 0,45m,
dch lc thu c tin hnh tim sc k.
Bit khi lng captopril chun i chiu cn l 0,0548g; khi lng bt captopril
trong nguyn liu cn l 0,0506g. Tin hnh tim dung dch chun v dung dch th, mi
mu tim lp li 3 ln, din tch pic thu c l:
Dung dch Ln tim Din tch pic (mAU*min)
1 35,452
Dung dch chun 2 35,483
3 35,674
1 35,310
Dung dch th 2 35,334
3 35,319

Vy hm lng captopril trong nguyn liu c t tiu chun khng, bit tiu chun
v hm lng captopril qui nh nm trong khong 98,0% n 101,5%.
p n:
Ta c:
a (%): Hm m ca captopril trong mu chun (a = 3).
Sth v Sch (mAU*min): Din tch pic trung bnh ca dung dch th v dung dch chun.
mth (gam): Khi lng bt nguyn liu cn pha dung dch th.
mch (gam): Khi lng captopril chun cn pha dung dch chun.
Cch (%): Hm lng captopril trong mu chun (Cch = 95,3).
- Din tch pic trung bnh ca dung dch th:
Sth = (35,310 + 35,334 + 35,319)/ 3 = 35,321 (mAU*min)
- Din tch pic trung bnh ca dung dch chun:
Sch = (35,452 + 35,483 + 35,674)/ 3 = 35,536 (mAU*min)
- Khi lng captopril trong chun i chiu l:
M1 = mch (Cch / 100) [(100 a)/100] = 0,0507 (gam)
- Khi lng captopril trong nguyn liu cn l:
M2 = Sth M1/ Sch = 0,0504 (gam)
- Hm lng phn trm ca captopril trong nguyn liu l:
C (%) = (M2/ mth) 100 = 99,51 % (nm trong khong 98,0% n 101,5%)
Kt lun: Mu nguyn liu t tiu chun qui nh v hm lng captopril.
Cng thc tnh hm lng phn trm ca captopril trong nguyn liu:
C (%) = Sth mch Cch (100 a)/ (Sch mth 100)
Trong :
a (%): Hm m ca captopril trong mu chun.
Sth v Sch (mAU*min): Din tch pic trung bnh ca dung dch th v dung dch chun.
mth (gam): Khi lng bt nguyn liu cn pha dung dch th.
mch (gam): Khi lng captopril chun cn pha dung dch chun.
Cch (%): Hm lng captopril trong mu chun.
Cu 2: nh lng bng phng php chun ni.
Xc nh d lng cefixim trong nc thi t c s sn xut dc bng HPLC c tin
hnh nh sau:
Dung dch chun: Tin hnh pha dy dung dch chun c nng cefixim ln lt khong
25; 50; 100; 200; 500; 800; 1000; 1200 ng/ ml v nng cht chun ni (cefdinir) l 500
ng/ ml; lc qua mng 0,45m.
Dung dch th: Ht chnh xc 1ml mu chun ni cefdinir 50g/ml cho vo bnh nh
mc 100ml, nh mc va bng mu nc thi. Acid ha bng HCl 1N n pH khong
3, sau ly chnh xc 5ml mu th v 3ml cloroform cho vo ng nghim, lc xy, ly
tm. Ly lp nc pha trn lc qua mng 0,45m.
Tin hnh phn tch sc k cc dung dch trn thu c kt qu:
Kt qu phn tch cc dung dch chun
Dung dch chun Nng cefixim (ng/ ml) SCFM (mAU*s) SIS (mAU*s)
1 22,98 10174 226167
2 45,96 18753 227215
3 91,93 37426 226790
4 183,86 79688 228426
5 459,64 187997 227636
6 735,43 304697 228576
7 919,29 379618 228854
8 1103,14 456299 228834

Kt qu phn tch dung dch th

Dung dch th SCFM (mAU*s) SIS (mAU*s)
13008 212994

Trong :
SCFM (mAU*s): din tch pic ca cefixim.
SIS (mAU*s): din tch pic ca chun ni cefdinir.
Tnh nng cefixim trong mu nc thi qua x l.
p n:
- T l din tch pic (gia cefixim v chun ni): S = SCFM/ SIS trong cc mu phn tch
c th hin nh trong bng:
Dd chun N. cefixim (ng/ ml) SCFM (mAU*s) SIS (mAU*s) S = SCFM/ SIS
1 22,98 10174 226167 0,04498
2 45,96 18753 227215 0,08253
3 91,93 37426 226790 0,16502
4 183,86 79688 228426 0,34886
 5 459,64 187997 227636 0,82587
6 735,43 304697 228576 1,33302
7 919,29 379618 228854 1,65878
8 1103,14 456299 228834 1,99402
Dd th 13008 212994 0,06107

- Da vo nng ca cc dung dch chun v t l din tch pic (gia cefixim v chun
ni), xy dng phng trnh biu din s ph thuc ca t l din tch pic (gia cefixim v
chun ni) vo nng cefixim (ng/ml) ta thu c kt qu:
y = 0,0018.x + 0,0037 (R2 = 0,9999).
Trong :
y l t l din tch pic (gia cefixim v chun ni).
x l nng cefixim (ng/ml).
- H s R2 = 0,9999 (xp x 1), c s ph thuc tuyn tnh cht ch ca t l din tch pic
(gia cefixim v chun ni) vo nng cefixim trong khong nng t 22,98 1103,14
(ng/ml). V vy, ta c th xc nh nng cefixim trong mu nc thi bng phng php
chun ni s dng k thut ng chun da trn ng chun xy dng.
- T l din tch pic ca mu nc thi l SX = 0,06107 nm trong khong tuyn tnh ca
ng chun xy dng.
Nng CFM c trong mu nc thi qua x l c tnh theo cng thc:
X(ng/ml) = (SX b)/ a = 31,87.
- Vy nng cefixim trong mu nc thi qua x l l 31,87 (ng/ml).
Cu 3: nh lng bng phng php chun ha din tch.
a. Xc nh tp cht lin quan trong nghin cu chit sut v tinh ch conessin t dc
liu lm cht chun i chiu thu c kt qu nh sau:
Thi gian lu (pht) Din tch pic (mAU*s)
Tp cht 1 7,04 72206
Tp cht 2 7,76 18145
Tp cht 3 10,38 16320
Tng pic 6333860

Bit tng hm lng tp cht trong nguyn liu khng c qu 3% tnh theo ch phm
nguyn trng, loi nhng pic c t l din tch di 0,05%.
Xc nh hm lng tng tp cht. Mu th c t yu cu v tp cht khng.
 b. Kt qu nh lng s b kaempferol nguyn liu thit lp chun i chiu bng
phng php chun ha din tch thu c nh sau:
Mu th Khi lng (mg) Din tch pic (mAU*s)
Pic chnh Tng pic
1 18,12 1870557 1937397
2 18,54 1915220 1982198
3 18,75 1912984 2004804

Bit hm lng hot cht yu cu khng c thp hn 95,0% tnh theo nguyn trng.
Vy cc mu th trn c t yu cu v hm lng thit lp cht chun i chiu
khng.
p n:
a.
- Hm lng tp cht (%) c tnh theo cng thc: Stp/ Stng x 100. Hm lng % tng
tp c th hin trong bng:
Hm lng (%)
Tp cht 1 1,14 (> 0,05%)
Tp cht 2 0,29 (> 0,05%)
Tp cht 3 0,26 (> 0,05%)
Tng tp cht 1,69

- Do cc tp 1, 2, 3 u c hm lng (hay t l din tch pic) trn 0,05%. Vy tng hm

lng tp cht bng tng hm lng cc tp 1, 2, 3 l: 1,14 + 0,29 + 0,26 = 1,69 (%)

Tng hm lng tp cht l 1,69% (< 3%). Vy mu th t yu cu v tp cht.

b.

- Hm lng kaempferol trong cc mu nguyn liu (%) c tnh theo cng thc:
Skaempferol/ Stng x 100. Hm lng kaempferol trong cc mu c th hin trong bng:
Mu th Hm lng (%)

1 96,55 (> 95%)

2 96,62 (> 95%)
3 95,42 (>95%)

- Cc mu th u c hm lng kaempferol ln hn 95,0% (tnh theo nguyn trng). Vy

cc mu t yu cu thit lp cht chun i chiu.