PHENYTOIN

Phenytoinum

 

 

 

 

C15H12N2O2 P.t.l: 252,3

Phenytoin la 5,5-diphenylimidazolidin-2, 4-dion, phai cha t 99,0 en 101,0% C15H12N2O2, tnh theo che pham a lam kho.

Tnh chat

Bot ket tinh trang hoac gan nh trang, khong mui hoac gan nh khong mui.

Thc te khong tan trong nc, hi tan trong ethanol 96%, kho tan trong cloroform va ether. Rat kho tan trong methylen clorid. Tan trong cac dung dch hydroxyd kiem loang.

nh tnh

Co the chon mot trong hai nhom nh tnh sau:

Nhom I: A.

Nhom II: B, C, D.

A. Pho hong ngoai (Phu luc 4.2) cua che pham phai phu hp vi pho hong ngoai cua phenytoin chuan (C).

B. Trong muc th Tap chat lien quan, vet chnh trong sac ky o thu c cua dung dch th (2) phai co v tr va kch thc giong vi vet chnh trong sac ky o thu c cua dung dch oi chieu (1).

C. Cho vao 10 mg che pham 1 ml nc va 0,05 ml amoniac (TT). un en soi, them 0,05 ml dung dch ong sulfat 5% trong dung dch amoniac 2 M (TT) va lac eu. Tua ket tinh mau hong xuat hien.

D. Phai ap ng cac yeu cau cua phep th Tro sulfat.

o trong va mau sac cua dung dch

Dung dch cua 1,0 g che pham trong hon hp gom 20 ml nc va 5 ml dung dch natri hydroxyd 1 M phai trong (Phu luc 9.2) va khong c co mau am hn mau cua mau mau VN6 (Phu luc 9.3, phng phap 2).

Gii han acid - kiem

Them 45 ml nc vao 1,0 g che pham, un soi khoang 2 phut, e nguoi va loc. Ra pheu loc bang nc khong co carbon dioxyd (TT). Pha loang dch loc va nc ra pheu loc bang nc khong co carbon dioxyd (TT) thanh 50 ml. Lay 10 ml dung dch thu c va them 0,15 ml dung dch o methyl (TT), mau cua ch th phai chuyen sang mau o khi them khong qua 0,5 ml dung dch acid hydrocloric 0,01 M (C). Lay 10 ml dung dch thu c va them 0,15 ml dung dch xanh bromothymol (TT), mau cua ch th phai chuyen sang mau xanh lam khi them khong qua 0,5 ml dung dch natri hydroxyd 0,01 M (C).

Tap chat lien quan

Xac nh bang phng phap sac ky lp mong (Phu luc 5.4).

Ban mong: Silica gel GF254 (TT). Trc khi dung, ra ban mong bang hon hp gom 30 ml dioxan (TT) va 75 ml hexan (TT). e ban mong kho ngoai khong kh.

Dung moi khai trien: Dioxan - hexan (30 : 75).

Dung moi hoa tan mau: Hon hp ong the tch cua aceton (TT) va methanol (TT) .

Dung dch th (1): Hoa tan 0,40 g che pham trong dung moi hoa tan mau va pha loang thanh 10 ml vi cung dung moi.

Dung dch th (2): Pha loang 1 ml dung dch th (1) thanh 20 ml bang dung moi hoa tan mau.

Dung dch oi chieu (1): Hoa tan 20 mg phenytoin chuan (C) trong dung moi hoa tan mau va pha loang thanh 10 ml bang cung dung moi.

Dung dch oi chieu (2): Hoa tan 8 mg benzophenon (TT) trong dung moi hoa tan mau va pha loang thanh 100 ml bang cung dung moi.

Dung dch oi chieu (3): Hoa tan 8 mg benzil (TT) trong dung moi hoa tan mau pha loang thanh 100 ml bang cung dung moi.

Dung dch oi chieu (4): Pha loang 1 ml dung dch th (1) thanh 100 ml bang dung moi hoa tan mau.

Dung dch oi chieu (5): Tron eu 1 ml dung dch oi chieu (2) va 1 ml dung dch oi chieu (3).

Cach tien hanh:

Cham rieng biet len ban mong 10 ml moi dung dch tren, dung luong kh lanh e lam kho ban mong trong khoang 2 phut. Trien khai sac ky en khi dung moi i c 15 cm. e ban mong kho ngoai khong kh va quan sat di anh sang t ngoai bc song 254 nm. Tren sac ky o cua dung dch th (1) cac vet tng ng vi vet cua benzophenon va benzil khong c am mau hn vet thu c tren sac ky o cua dung dch oi chieu (2) va (3) (0,2%), cac vet phu khac tr vet chnh va vet tng ng vi benzophenon va benzil khong c am mau hn vet thu c tren sac ky o cua dung dch oi chieu (4) (1%). Phep th ch co gia tr khi sac ky o thu c cua dung dch oi chieu (5) cho thay 2 vet tach ro rang.

Kim loai nang

Khong c qua 10 phan trieu (Phu luc 9.4.8).

Lay 2,0 g che pham th theo phng phap 3. Dung 2 ml dung dch ch mau 10 phan trieu (TT) e chuan b mau oi chieu.

 

Mat khoi lng do lam kho

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

(1,000 g; 100 105 oC).

Tro sulfat

Khong c qua 0,1% (Phu luc 9.9, phng phap 2).

Dung 1,0 g che pham.

nh lng

Hoa tan 0,200 g che pham trong 50 ml dimethyl formamid (TT). Chuan o bang dung dch natri methoxid 0,1 N. Xac nh iem ket thuc bang phng phap chuan o o ien the (Phu luc 10.2).

1 ml dung dch natri methoxid 0,1 N (C) tng ng vi 25,23 mg C15H12N2O2.

Bao quan

ng trong bnh kn.