Vancomycin Hydroclorid

Vancomycini hydrochloridum

 

 

C66H75Cl2N9O24. HCl P.t.l: 1486,0

Vancomycin hydroclorid la muoi hydroclorid cua hon hp cac glycopeptid co lien quan vi nhau, chu yeu di dang mono hydroclorid cua (3S,6R,7R,22R,23S,26S,aS,36R,38aR)-3-(2-amino-2-oxoethyl)-44-[[2-O-(3-amino-2,3,6-trideoxy-3-C-methyl-a-L-lyxo-hexopyranosyl)-b-D-glucopyra-nosyl]oxy]-10,19-dicloro-7,22,28,30,32-pentahydroxy-6-[[(2R)-4-methyl-2-(methylamino)penta-noyl]amino]-2,5,24,38,39-pentaoxo-2,3,4,5,6,7,23,24,25,26,36,37,38,38a-tetradecahydro-22H-8, 11,18,21-dietheno-23,36-(iminomethano)-13,16:31,35-dimetheno-1H,13H-[1,6,9]oxadiazacyclo-hexadecino[4,5-m][10,2,16]benzoxadiazacyclotetracosin-26-carboxylic acid (vancomycin B). Vancomycin hydroclorid c ieu che t mot so loai Amycolaptosis orientalis hoac bang phng cach khac. Hoat lc khong c t hn 1050 IU/mg, tnh theo che pham a lam kho.

Tnh chat

Bot trang hoac gan nh trang, de hut am. De tan trong nc, kho tan trong ethanol 96%.

nh tnh

A. Kiem tra sac ky o thu c trong phep th gii han vancomycin B. Thi gian lu cua pic chnh trong sac ky o thu c t dung dch th (1) tng ng vi thi gian lu cua pic chnh tren sac ky o cua dung dch oi chieu.

B. Che pham phai cho phan ng A cua phep th nh tnh ion clorid (Phu luc 8.1)

o trong va mau sac cua dung dch

Hoa tan 2,5 g che pham trong nc va pha loang thanh 25 ml vi cung dung moi. Dung dch thu c phai trong (Phu luc 9.2). o hap thụ (Phu luc 4.1) cua dung dch tren o bc song 450 nm khong c ln hn 0,10.

pH

Hoa tan 0,50 g che pham trong nc khong co carbon dioxyd (TT) va pha loang thanh 10 ml vi cung dung moi. pH cua dung dch phai t 2,5 en 4,5 (Phu luc 6.2).

Vancomycin B

Khong c t hn 93,0%

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

Pha ong A: Them 1996 ml nc vao 4,0 ml triethylamin (TT) va chnh pH en 3,2 vi acid phosphoric (TT). Lay 920 ml dung dch va pha, them 10 ml tetrahydrofuran (TT) va 70 ml acetonitril (TT).

Pha ong B: Them 1996 ml nc vao 4,0 ml triethylamin (TT) va chnh pH en 3,2 vi acid phosphoric (TT). Lay 700 ml dung dch va pha, them 10 ml tetrahydrofuran (TT) va 290 ml acetonitril (TT).

Dung dch th (1): Hoa tan 10,0 mg che pham trong pha ong A va pha loang thanh 5,0 ml vi cung dung moi.

Dung dch th (2): Pha loang 2,0 ml dung dch th (1) thanh 50,0 ml bang pha ong A.

Dung dch th (3): Pha loang 0,5 ml dung dch th (2) thanh 20,0 ml bang pha ong A.

Dung dch oi chieu: Hoa tan 5,0 mg vancomycin hydroclorid chuan (C) trong 4 ml nc va pha loang thanh 10 ml vi cung dung moi. un nong 65 oC trong 24 gi. e nguoi.

Dung cac dung dch nay trong vong 4 gi sau khi pha che.

ieu kien sac ky:

Cot: cot thep khong r (0,25m x 4,6 mm), được nhoi pha tĩnh C (5 m).

Toc o dong: 1,0 ml/phut.

Detector quang pho hấp thu tử ngoại at bc song 280 nm.

The tch tiem mau: 20 l.

Cch tiến hnh:

Ra giải cot khi au vi pha ong A. Sau 13 phut, tiến hanh ra giải gradient tang dan nong o pha ong B khoang 11 % v/v cho moi phut. Cuoi cung, ra giải cot trong 4 phut, bằng pha ong B.

Tiem dung dch th (3). Phep th ch co gia tr khi pic chnh trong sac ky o thu c co gia tr t so tn hiệu nhiễu/ường nền nho nhat la 5. Tiem dung dch th (2). Phep th nay ch co gia tr khi he so oi xng cua pic vancomycin toi a la 1,6. Tiem dung dch oi chieu. Phep th nay ch co gia tr khi o phan giai gia 2 pic chnh t nhat la 5,0. Tiem dung dch th (1).

Tnh ket qua ham lng phan tram vancomycin B hydroclorid theo cong thc sau:

Ab = dien tch pic vancomycin B trong sac ky o cua dung dch th (2),

At = tong dien tch tat ca cac pic tap chat trong sac ky o cua dung dch th (1)

Tap chat lien quan

Kiem tra bang sac ky long (Phu luc 5.3), nh mo ta trong th nghiem vancomycin B.

Tiem rieng re dung dch th (1), dung dch th (2) va dung dch th (3).

Tnh ham lng phan tram cho moi tap chat bang cong thc sau:

 

Ai = Dien tch pic cua tap chat tren sac ky o thu c t dung dch th (1),

Ab = Dien tch pic vancomycin B trong sac ky o thu c t dung dch th (2),

At = Tong dien tch tat ca cac pic tap chat trong sac ky o thu c t dung dch th (1)

Ham lng cac chat khong phai la cac tap chat nh mo ta phai ln hn 4,0 % va ham lng tap chat toan phan khong c nhieu hn 7,0 %. Khong tnh en nhng pic co dien tch nho hn dien tch pic chnh trong sac ky o cua dung dch th (3).

Kim loai nang

Khong c qua 30 phan trieu (Phu luc 9.4.8). Dung 1,0 g che pham th theo phng phap 3.

Dung 3,0 ml dung dch ch mau 10 phan trieu (TT) e chuan b mau oi chieu.

Nc

Khong c qua 5,0 % (Phu luc 10.3).

Dung 0,5 g che pham tien hanh th bang phng phap ban vi nh lng.

Tro sulfat

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

Dung 1,0 g che pham.

o vo trung

Neu che pham d nh dung lam nguyen lieu e bao che thuoc tiem ma khong co giai oan tiet trung trong qui trnh san xuat, che pham phai at ch tieu ve o vo trung (Phu luc 15.4).

Noi oc to vi khuan

Khong c qua 0,25 IU/mg (Phu luc 13.2). Neu d nh dung lam nguyen lieu e bao che thuoc tiem phan lieu ma khong co giai oan loai bo noi oc to vi khuan thch hp trong qui trnh san xuat, che pham phai at ch tieu ve noi oc to vi khuan.

nh lng

Tien hanh theo phng phap xac nh hoat lc khang sinh bang phng phap th vi sinh vat (Phu luc 13.9). Dung vancomycin hydroclorid chuan (C) lam chat oi chieu.

Bao quan

Bao quan trong chai lo kn, tranh anh sang. Neu a c tiet trung trc, phai bao quan trong chai lo kn va vo trung.

Nhan

Nhan ghi ro che pham a c tiet trung, khong co noi oc to vi khuan.

Tac dung

Khang khuan.

Che pham

Thuốc tiem, vien nang.