PRIMAQUIN DIPHOSPHAT

Primaquini diphosphas

C15H21N3O. 2H3PO4 P.t.l: 455,3

Primaquin diphosphat la (4RS)-N4-(6-methoxy-quinolin-8-yl)pentan-1,4-diamin diphosphat, phai cha t 98,5 en 101,5% C15H21N3O. 2H3PO4, tnh theo che pham khan.

Tnh chat

Bot ket tinh mau da cam.

Tan trong nc, thc te khong tan trong ethanol 96% va trong ether.

Chay khoang 200 oC kem theo phan huy.

nh tnh

Co the chon mot trong hai nhom nh tnh sau:

Nhom I: A, C, D.

Nhom II: B, D.

A. Hoa tan 15 mg che pham trong dung dch acid hydrocloric 0,01 M (TT) va pha loang thanh 100,0 ml vi cung dung moi. Pho hap thu anh sang (Phu luc 4.1) cua dung dch nay trong khoang bc song t 310 nm en 450 nm phai cho 2 cc ai hap thu 332 nm va 415 nm. o hap thu rieng cac cc ai nay lan lt la t 45 en 52 va t 27 en 35. Pha loang 5,0 ml dung dch nay thanh 50,0 ml bang dung dch acid hydrocloric 0,01 M (TT). Pho hap thu t ngoai cua dung dch pha loang nay trong khoang bc song t 215 nm en 310 nm phai cho 3 cc ai hap thu 225 nm, 265 nm va 282 nm. o hap thu rieng cac cc ai nay lan lt la t 495 en 515, t 335 en 350 va t 330 en 345.

B. Pho hong ngoai (Phu luc 4.2) cua che pham phai phu hp vi pho hong ngoai cua primaquin diphosphat chuan (C). Chuan b a mau e o nh sau: Hoa tan rieng biet 0,1 g che pham va 0,1 g chat chuan trong 5 ml nc, them 2 ml dung dch amoniac 2 M (TT), 5 ml methylen clorid (TT) va lac. Lam khan lp methylen clorid bang cach loc qua 0,5 g natri sulfat khan (TT). Chuan b a mau trang dung 0,3 g kali bromid (TT). Nho tng giot mot 0,1 ml lp methylen clorid len a, e methylen clorid boc hi het gia cac lan nho, roi lam kho a 50 oC trong 2 phut.

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

Ban mong: Silica gel GF254 (TT).

Dung moi khai trien: Amoniac am ac - methanol - cloroform (1 : 40 : 60).

Phep th c tien hanh cang nhanh cang tot trong ieu kien tranh anh sang. Dung dch th va chuan ch pha trc khi dung.

Dung dch th: Hoa tan 0,20 g che pham trong 5 ml nc va pha loang thanh 10 ml vi methanol (TT). Pha loang 1 ml dung dch thu c thanh 10 ml bang hon hp ong the tch gom nc va methanol (TT).

Dung dch oi chieu: Hoa tan 20 mg primaquin diphosphat chuan (C) trong 5 ml nc va pha loang thanh 10 ml vi methanol (TT).

Cach tien hanh: Ra ban mong trc bang dung moi khai trien. e ban mong kho ngoai khong kh. Cham rieng biet len ban mong 5 ml moi dung dch tren va trien khai sac ky en khi dung moi i c khoang 15 cm. Lay ban mong ra e kho ngoai khong kh va quan sat di anh sang t ngoai bc song 254 nm. Vet chnh tren sac ky o cua dung dch th phai tng ng ve v tr va kch thc so vi vet chnh tren sac ky o thu c t dung dch oi chieu.

D. Hoa tan 50 mg che pham trong 5 ml nc, them 2 ml dung dch natri hydroxyd loang (TT) va chiet 2 lan, moi lan vi 5 ml methylen clorid (TT). Lp nc, sau khi a acid hoa bang acid nitric (TT), phai cho phan ng B cua phosphat (Phu luc 9.4.12).

Tap chat lien quan

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

Pha ong: Amoniac am ac - methanol - cloroform - hexan (0,1 : 10 : 45 : 45).

Dung dch th: Hoa tan 50 mg che pham trong nc va pha loang thanh 5,0 ml vi cung dung moi. Them 0,2 ml amoniac am ac (TT) vao 1,0 ml dung dch nay va lac vi 10,0 ml pha ong. Dung lp dch trong pha di.

Dung dch oi chieu (1): Hoa tan 50 mg primaquin diphosphat chuan (C) trong nc va pha loang thanh 5,0 ml vi cung dung moi. Them 0,2 ml amoniac am ac (TT) vao 1,0 ml dung dch nay va lac vi 10,0 ml pha ong. Dung lp trong pha di.

Dung dch oi chieu (2): Pha loang 3,0 ml dung dch th thanh 100,0 ml bang pha ong.

Dung dch oi chieu (3): Pha loang 1,0 ml dung dch th thanh 10,0 ml bang pha ong. Pha loang tiep 1,0 ml dung dch nay thanh 50,0 ml bang pha ong.

ieu kien sac ky:

Cot (20 cm x 4,6 mm) c nhoi silica gel dung cho sac ky (10 mm).

Detector quang pho hap thu t ngoai bc song 261 nm.

Toc o dong: 3,0 ml/phut.

The tch tiem: 20 ml.

Cach tien hanh: Tiem moi dung dch tren va ghi lai sac ky o trong thi gian toi thieu gap oi thi gian lu cua primaquin. Phep th ch co gia tr khi trong sac ky o cua dung dch oi chieu (1) ngay trc pic chnh la mot pic co dien tch pic vao khoang 6% cua dien tch pic chnh va o phan giai gia hai pic nay khong nho hn 2,0; trong sac ky o cua dung dch oi chieu (3), ty so gia tn hieu cua pic chnh va o nhieu ng nen khong nho hn 5. Trong sac ky o thu c t dung dch th, tong dien tch cua tat ca cac pic phu khong c ln hn dien tch pic chnh trong sac ky o thu c t dung dch oi chieu (2) (3,0%). Loai bo pic cua dung moi va cac pic co dien tch nho hn dien tch pic chnh trong sac ky o cua dung dch oi chieu (3).

Mat khoi lng do lam kho

Khong c qua 0,5% (Phu luc 9.6).

(1,000 g; 100 105 oC).

nh lng

Hoa tan 0,200 g che pham trong 40 ml acid acetic khan (TT), bang un nong nhe. e nguoi va chuan o bang dung dch acid percloric 0,1 N (C). Xac nh iem ket thuc bang phng phap chuan o o ien the (Phu luc 10.2).

1 ml dung dch acid percloric 0,1 N (C) tng ng vi 22,77 mg C15H21N3O. 2H3PO4.

Bao quan

Bao quan tranh anh sang.

Tac dung

Tr sot ret.