Professional Documents
Culture Documents
T 3- Nhm III Lp Dc 3B
Ngy thc hnh : 16/5/2013
H
N
NH
N
O
O
CH3
Ptl: 295,3
nh lng:
Cn chnh xc khong 50mg mebendazole, thm 50ml HCl 0,5M pha trong
methanol, khuy tan trong 30 pht, chuyn vo bnh nh mc dung tch
100ml, thm HCl 0,5M trong methanol n vch trn u
(dung dch 1)
Ly chnh xc 1ml dung dch 1 cho vo bnh nh mc 100ml th 2, thm
HCl 0,5M trong methanol n vch (dung dch 2). o hp th quang ca
dung dch 2 234nm, cuvet 1cm, mu trng l dung dch HCl 0,5M trong
methanol.
Tin hnh tng t nh trn vi mebendazole chun
Tnh hm lng C16H13N3O3 ca mu mebendazol th
Khi lng mu chun m1= 0,0523g
hp th mu chun E1 = 0,6140
Khi lng mu th m2 = 0,0503 g
hp th mu th E2= 0,5277
C1= 0,0523/(295,30*0,1*0,1)= 0,01771 M
E1/E2 = C1/C2
Suy ra C2= C1* E2/ E1 = 0,01771* 0,5277/ 0,6140 = 0,01522 M
Vy khi lng thc t ca mebendazole cha trong mu th l
M= 0,01522*295,3*0,1*0,1= 0,04495 gam
Hm lng phn trm ca mebendazole trong mu th
% C16H13N3O3 = 0,04495/ 0,0503= 89,36%
Hm lng ca mebendazole theo quy nh phi t t 98-101%
Kt qu thu c khng nm trong khong ny, c th v nhng l do sau:
- Mu th khng t yu cu
- Thao tc trong qu trnh cn, ong, o cha t chun
- Tnh ton sai s
B. NHN THC, NH TNH METRONIDAZOLE, ARTESUNATE
I. Metronidazole
Cng thc: C6H9O3N3
Ptl: 171,20
OH
O
N
O
CH3
N
Ha tnh v nh tnh:
1. Tnh base
Tin hnh: Ha tan 0,1g cht th vo 4ml acid sulfuric 3%, thm 2ml acid
picric 1%
Hin tng: xut hin kt ta mu vng
Gii thch: Metronidazole c tnh base, tan trong acid v c long, khi kt
hp vi thuc th alcaloid th cho kt ta c mu vng c trng
2. Phn ng ca nitro thm
Tin hnh:
ng nghim 1: un nng trn n cn trong 5-10 pht hn hp gm: 10mg
cht th, 10mg km bt, 1ml nc, 0,5ml HCl long, lc ly dch lc, thm
1-2 git NaNO2 0,1 M vo dch lc, trn u
ng nghim 2: Ha tan khong 0,1 g beta-naphtol vo 2ml dung dch NaOH
long. t t dch ng 2 vo ng 1.
Hin tng: xut hin mu
Gii thch:
HCl v bt Zn l to H mi sinh, H mi sinh ny s kh nhm NO2- thnh
nhm amin bc 1 thm, HCl v NaNO2 to ra HNO2 tham gia phn ng
diazo ha. Sn phm l mui diazoni
ng 2 thm NaOH long l ha tan beta-naphtol thnh dng mui d tan.
O Na
OH
O
N
O
OH
CH3
H2N
+ HCl + Zn
CH3
N
OH
OH
H2N
CH3
N
+ NaNO2 + HCl
CH3
N
OH
N
O Na
CH3
OH
N
CH3
N
(mu cam)
II. ARTESUNATE
Cng thc: C19H29O8
Ptl : 384,40
Phn ng mu:
Ha tan 50mg cht th trong khong 1ml dung dch hydroxylamine
hydrochloride 7% trong ethanol. Thm 3ml KOH 0,5M trong ethanol, un
si cch thy ri ngui, acid ha bng HCl 10% n pH khong 6-7.
Thm vi git FeCl3 5%
Hin tng : xut hin mu tm
Gii thch:
Nhm ceton ca artesunate tc dng vi hydroxylamin hydroxhlorid trong
ethanol to dn cht oxim, dn cht ny b thy phn, sn phm to ra tc
dng vi mui st III to phc mu tm.