QUININ BISULFAT

Quinini bisulfas

 

C20H24N2O2. H2SO4. 7H2O P.t.l: 548,6

Quinin bisulfat la (8S, 9R)-6'-methoxycinchonan-9-ol hydrosulfat heptahydrat, phai cha t 98,5 en 101,5% C20H24N2O2.. H2 SO4, tnh theo che pham khan.

Tnh chat

Tinh the khong mau hay bot ket tinh trang, khong mui, v ang, len hoa ngoai khong kh kho. De tan trong nc, hi tan trong ethanol 96%.

nh tnh

A. Phng phap sac ky lp mong (Phu luc 5.4).

Ban mong: Silica gel G (TT).

Dung moi khai trien: Diethylamin - ether - toluen (15 : 36 : 60).

Dung dch th: Dung dch che pham 1,0% trong methanol (TT).

Dung dch oi chieu (1): Dung dch quinin sulfat chuan (ĐC) 1,0% trong methanol (TT).

Dung dch oi chieu (2): Dung dch cha 1,0% cua moi chat quinidin sulfat chuan va quinin sulfat chuan (ĐC) trong methanol (TT).

Cach tien hanh: Cham rieng biệt len ban mong 4 ml moi dung dch tren. Sau khi trien khai sac ky, lay ban mong ra, lam kho bang luong khong kh trong 15 phut va chay sac ky nhac lai. Say kho ban mong 105 oC trong 30 phut, e nguoi va phun thuoc th iodoplatinat (TT). Vet chnh tren sac ky o cua dung dch th phai tng t ve v tr, mau sac va kch thc vi vet chnh tren sac ky o cua dung dch oi chieu (1). Phep th ch co gia tr khi sac ky o cua dung dch oi chieu (2) cho 2 vet tach ro rang.

B. Che pham ap ng phep th pH.

C. Che pham cho phan ng ac trng cua sulfat (Phu luc 8.1).

pH

pH cua dung dch che pham 1%: 2,8 - 3,4 (Phu luc 6.2).

Goc quay cc rieng

T -208 en -216o, tnh theo che pham khan (Phu luc 6.4).

Dung dung dch che pham 3% trong dung dch acid hydrocloric 0,1 M (TT) e o.

Cac alcaloid cinchona khac

Xac nh bang phng phap sac ky long (Phu luc 5.3).

Pha ong: Hoa tan 6,8 g kali dihydrophosphat va 3,0 g hexylamin trong 700 ml nc, ieu chnh pH en 2,8 bang dung dch acid phosphoric 1 M (TT), them 60 ml acetonitril (TT) va pha loang thanh 1000 ml bang nc.

Dung dch th: Hoa tan 20 mg che pham trong 5 ml pha ong, un nong nhe neu can thiet, pha loang thanh 10 ml vi pha ong.

Dung dch oi chieu (1) va dung dch oi chieu (2) c chuan b tng t nh dung dch th, nhng thay che pham bang quinin sulfat chuan (C) thu c dung dch oi chieu (1) va quinidin sulfat chuan (C) thu c dung dch oi chieu (2).

Dung dch oi chieu (3): Pha loang 1,0 ml dung dch oi chieu (1) thanh 10,0 ml vi pha ong. Pha loang 1,0 ml dung dch thu c thanh 50,0 ml vi pha ong.

Dung dch oi chieu (4): Hoa tan 10 mg thioure trong pha ong thanh 10 ml.

Dung dch phan giai: Hon hp ong the tch cua dung dch oi chieu (1) va dung dch oi chieu (2).

ieu kien sac ky:

Cot thep khong g (25 cm x 4,6 mm) c nhoi pha tĩnh C (5 mm) (Hypersil ODS 5 mm la thch hp).

Detector quang pho hap thu t ngoai at bc song 250 nm cho sac ky o cua dung dch oi chieu (4) va 316 nm cho sac ky o cua cac dung dch khac.

Toc o dong: 1,5 ml/phut.

The tch tiem: 10 ml.

Cach tien hanh:

Tiem dung dch oi chieu (2) va (4), neu can thiet ieu chnh nong o cua acetonitril trong pha ong e sac ky o thu c t dung dch oi chieu (2) co he so dung lng cua pic quinidin la 3,5 en 4,5, Vo c tnh t pic cua thioure trong sac ky o cua dung dch oi chieu (4).

Tiem dung dch oi chieu (1), (2), (3) va dung dch phan giai. Sac ky o cua dung dch oi chieu (1) cho 1 pic chnh cua quinin va 1 pic cua dihydroquinin co thi gian lu tng oi so vi quinin la khoang 1,4. Sac ky o cua dung dch oi chieu (2) cho 1 pic chnh cua quinidin va 1 pic cua dihydroquinidin co thi gian lu tng oi so vi quinindin la khoang 1,2. Sac ky o cua dung dch phan giai cho 4 pic: quinin, dihydroquinin, quinidin, dihydroquinidin c nh tnh bang so sanh thi gian lu cua chung vi cac pic tng ng trong sac ky o cua dung dch oi chieu (1) va dung dch oi chieu (2).

Phep th ch co gia tr khi sac ky o cua dung dch phan giai co o phan giai gia pic cua quinin va quinidin t nhat la 1,5 va o phan giai gia pic cua dihydroquinidin va quinin t nhat la 1,0 va ty so tn hieu cua pic chnh va nhieu ng nen trong sac ky o cua dung dch oi chieu (3) t nhat la 5.

Tiem dung dch th. Tien hanh sac ky trong khoang thi gian gap 2,5 lan thi gian lu cua pic chnh. Tnh ham lng phan tram cua tap chat lien quan bang phng phap chuan hoa, bo qua bat ky pic nao co dien tch nho hn dien tch cua pic trong sac ky o cua dung dch oi chieu (3) (0,2%). Ham lng cua dihydroquinin khong c qua 10%, ham lng cua bat ky tap chat lien quan nao ra giai trc quinin khong c qua 5% va ham lng cua bat ky tap chat lien quan nao khac khong c qua 2,5%.

Tro sulfat

Khong c qua 0,1% (Phu luc 9.9, phng phap 1).

Nc

T 19,0 en 25,0% (Phu luc 10.3).

Dng 0,20 g chế phẩm.

Cation chuan o c

Phai t 75,3 en 79,6%, tnh theo che pham khan, c xac nh bang phng phap sau: Them vao dung dch nc a thu c muc nh lng 0,1 ml dung dch phenolphtalein (TT) va nh lng bang dung dch acid hydrocloric 0,1 N (C).

1 ml dung dch natri hydroxyd 0,1 N (C) tng ng vi 16,32 mg [C20H26N2O2]2+

nh lng

Hoa tan 0,450 g che pham trong 15 ml nc. Them 25 ml dung dch natri hydroxyd 0,1 M (C) va chiet bang cloroform (TT) 3 lan, moi lan 25 ml. Tap trung dch chiet cloroform (TT) va ra bang 20 ml nc. Gop cac dung dch nc thu c e em th cation chuan o c. Lam khan dch chiet cloroform (TT) bang natri sulfat khan (TT), boc hi ti kho ap suat 2 kPa, hoa tan can con lai trong 50 ml acid acetic khan (TT). Tien hanh chuan o theo phng phap nh lng trong moi trng khan (Phu luc 10.6, phng phap 1), dung dung dch tm tinh the (TT) lam ch th.

1 ml dung dch acid percloric 0,1 N (C) tng ng vi 21,13 mg C20H24N2O2. H2SO4.

Bao quan

Trong lo kn, tranh anh sang.

Loại thuốc

Tr sot ret.

Che pham

Vien nen.