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Dc in Vit Nam III
1-ACID ACETYLSALICYLIC
Acidum acetylsalicylicum
Aspirin
C9H8O4 P.t.l: 180,2
Acid acetylsalicylic l acid 2-acetoxybenzoic, phi cha t 99,5 n
l01,0%
C9H8O4, tnh theo ch phm lm kh.
Tnh cht
Tinh th khng mu hoc bt kt tinh trng, khng mi hoc gn nh
khng mi. Kh tan trong nc, d tan trong ethanol 96%, tan trong
ether v
cloroform.
Chy khong 143oC (Ph lc 5. 19, Phng php 3).
nh tnh
C th chn mt trong hai nhm nh tnh sau:
Nhm I: A, B
Nhm II: B, C, D
A. Ph hng ngoi (Ph lc 3.2) ca ch phm phi ph hp vi ph hng
ngoi ca acid acetylsalicylic chun.
B. un si 0,2 g ch phm vi 4 ml dung dch natri hydroxyd long
(TT)
trong 3 pht, ngui v thm 5 ml dung dch acid sulfuric l0% (TT). Ta
kt tinh
c to thnh. Ta sau khi c lc, ra vi nc v sy kh l00 - l05oC, c
im chy t 156 n 161oC (Ph lc 5.19).
C. Trong mt ng nghim, trn 0,1 g ch phm vi 0,5 g calci
hydroxyd
(TT).
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un hn hp v cho khi sinh ra tip xc vi ming giy lc tm 0,05 ml
dung dch nitrobenzaldehyd (TT) s xut hin mu xanh l cy hi vng,
hoc
xanh l cy hi xanh lam. Lm m t giy lc vi dung dch acid
hydrocloric
long (TT), mu s chuyn thnh xanh lam.
D. Ha tan bng cch un nng khong 20 mg ta thu c t php th B
trong l0 ml nc v lm ngui. Dung dch thu c cho phn ng ca
salicylat
(Ph lc 7.l).
trong v mu sc ca dung dch
Ha tan l,0 g ch phm trong 9 ml ethanol 96% (TT). Dung dch phi
trong
(Ph lc 5.12) v khng mu (Ph lc 5.17, phng php 2).
Tp cht lin quan
Trong bnh nh mc dung tch l00 ml, ha tan 0,15 g ch phm trong l0
ml
dung dch tetrabutylamoni hydroxyd 0,1 M trong 2 - propanol, yn
10 pht.
Thm 8,0 ml dung dch acid hydrocloric 0,1 N v 20,0 ml natri
tetraborat l,9% v
trn u. Thm 2,0 ml dung dch aminopyrazolon l,0% v 2,0 ml dung dch
kali
fericyanid l,0%, trong qu trnh thm cc dung dch ny lc lin tc. Sau
2 pht,
pha long n 100,0 ml bng nc. yn 20 pht. o hp th ca dung dch
bc sng 505 nm trong cc o dy 2 cm, dng nc lm mu trng. hp th
thu c khng c ln hn 0,25 (khong 0,l% biu th bng acid
acetylsalicylic).
Acid salicylic
Khng c qu 0,05%.
Ha tan 0,l0 g ch phm trong 5 ml ethanol 96% (TT), thm ngay 15
ml
nc c lm lnh trong nc v 0,05 ml dung dch st (III) clorid
0,5%.
Sau 1pht dung dch ny khng c c mu thm hn mu ca dung dch i
chiu chun b ng thi bng cch cho hn hp gm 0,05 ml dung dch st
(III)
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clorid 0,5%, 0,1 ml acid acetic (TT), 4 ml ethanol 96% (TT) v 15
ml nc vo 1
ml dung dch ca 5,0 mg acid salicylic trong 100 ml ethanol 96%
(TT).
Clorid
Khng c qu 0,015% (Ph lc 7.4.5)
Dung dch S: un si 4,0 g ch phm vi l00 ml nc trong 5 pht,
ngui, thm nc va 100 ml v lc.
Ly 8,3 ml dung dch S, pha long vi nc va 15 ml v tin hnh th.
Sulfat
Khng c qu 0,040% (Ph lc 7.4.12).
Ly 9,4 ml dung dch S, pha long vi nc va 15 ml v tin hnh th.
Kim loi nng
Khng c qu 20 phn triu (Ph lc 7.4.7).
Ha tan 0,75 g ch phm trong 9 ml aceton (TT) v pha long vi nc
va
15 ml. Ly 12 ml dung dch ny th theo phng php 2. Pha long dung
dch
ch mu l00 phn triu bng hn hp gm 9 th tch aceton (TT) v 6 th tch
nc
c dung dch ch mu 1 phn triu chun b mu i chiu.
Mt khi lng do lm kh
Khng c qu 0,5% (Ph lc 5.16).
(l,00 g; p sut gim; phosphor pentoxyd).
Tro sulfat
Khng c qu 0,l% (Ph lc 7.7, phng php 2)
Dng l,0 g ch phm.
nh lng
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Ha tan 1,000 g ch phm trong 10 ml ethanol 96% (TT) trong bnh
nn
nt mi. Thm 50,0 ml dung dch natri hydroxyd 0,5 M. y nt bnh v
yn
trong 1 gi. Chun bng dung dch acid hydrocloric 0,5 M, dng 0,2 ml
dung
dch phenolphtalein (CT) lm ch th.
Song song lm mu trng.
1 ml dung dch natri hydroxyd 0,5 M tng ng vi 45,04 mg
C9H8O4.
Bo qun
Ch phm c bo qun trong chai l nt kn, trnh nh sng.
Cng dng
H nhit, gim au, khng vim.
Ch phm
Vin nn aspirin.
2 -ACID ASCORBIC
Acidum ascorbicum
Vitamin C, Acid L-ascorbic
C6H8O6 P.t.l: 176,1
Acid ascorbic l
(R)-5-[(S)-1,2-dihydroxyethyl]-3,4-dihydroxy-5H-furan 2-
on, phi cha t 99,0 n 100,5% C6H8O6.
Tnh cht
Tinh th khng mu hay bt kt tinh trng hoc gn nh trng, b bin mu
khi tip xc vi khng kh, nh sng v m. Khng mi hoc gn nh khng
mi.
D tan trong nc, tan trong ethanol 96%, thc t khng tan trong
cloroform v
ether. Chy khong 1900C cng vi phn hu.
nh tnh
