CODEIN PHOSPHAT

Codeini phosphas

 

 

 

 

 

 

 

 


C18H21NO3. H3PO4. 1/2H2O (hemihydrat) P.t.l: 406,4

C18H21NO3. H3PO4. 3/2H2O (sesquihydrat) P.t.l: 424,4

Codein phosphat la

4,5a-epoxy-3-methoxy-17-methyl-7,8-didehydromorphinan-6a-ol phosphat hemihydrat .

hoac sesquihydrat, phai cha t 98,5 en 101,0% C18H21NO3. H3PO4, tnh theo che pham a lam kho.

Tnh chat

Tinh the nho khong mau hoac bot ket tinh trang, khong mui.

De tan trong nc, kho tan trong ethanol 96%, thc te khong tan trong ether.

nh tnh

Co the chon mot trong 2 nhom nh tnh sau:

Nhom I: B, E.

Nhom II: A, C, D, E, F.

Dung dch S: Hoa tan 1,00 g che pham trong nc khong co carbon dioxyd (TT) va pha loang thanh 25,0 ml bang cung dung moi.

A. Pha loang 1,0 ml dung dch S vi nc thanh 100,0 ml. Them 25 ml nc, 10 ml dung dch natri hydroxyd 1 M vao 25,0 ml dung dch nay va pha loang thanh 100,0 ml bang nc. o pho t ngoai (Phu luc 4.1) cua dung dch tren dai song t 250 en 350 nm. Dung dch ch co duy nhat mot cc ai hap thu 284 nm. o hap thu rieng bc song cc ai khoang 38, tnh theo che pham a lam kho.

B. Hoa tan 0,20 g che pham trong 4 ml nc, them 1 ml hon hp ong the tch dung dch natri hydroxyd 10 M (TT) va nc. e khi mao ket tinh, co the co vao thanh ong nghiem bang mot ua thuy tinh va lam lanh trong nc a. Ra tua va say kho 100 en 105 oC. Pho hong ngoai (Phu luc 4.2) cua tua thu c phai phu hp vi pho hong ngoai oi chieu cua codein.

C. iem chay cua tua thu c phep th B t 155 en 159 oC (Phu luc 6.7).

D. Them 1 ml acid sulfuric (TT) va 2 giot dung dch sat (III) clorid 1,3% vao khoang 10 mg che pham va un nong tren cach thuy, se xuat hien mau xanh lam. Them 2 giot acid nitric (TT), mau chuyen sang o.

E. Dung dch S cho phan ng A cua ion phosphat (Phu luc 8.1).

F. Che pham cho phan ng cua cac alcaloid (Phu luc 8.1).

o trong va mau sac cua dung dch

Dung dch S phai trong (Phu luc 9.2) va mau khong c am hn mau mau V6 (Phu luc 9.3, phng phap 2).

pH

pH cua dung dch S phai t 4,0 en 5,0 (Phu luc 6.2).

Goc quay cc rieng

T -98o en -102o, tnh theo che pham a lam kho (Phu luc 6.4).

Pha loang 5,0 ml dung dch S vi nc thanh 10,0 ml e o.

Morphin

Khong c qua 0,13%.

Hoa tan 0,10 g che pham trong dung dch acid hydrocloric 0,1 M (TT) va pha loang thanh 5 ml vi cung dung moi. Them 2 ml dung dch natri nitrit 1% (TT), e yen 15 phut va them 3 ml dung dch amoniac 6 M (TT). Mau cua dung dch thu c khong c am hn mau mau N4 (Phu luc 9.3, phng phap 2).

Alcaloid la

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

Ban mong: Silica gel G (TT).

Dung moi khai trien: Amoniac am ac - cyclohexan - ethanol (6 : 30 : 72).

Dung dch th: Hoa tan 0,50 g che pham trong mot hon hp ethanol - dung dch acid hydrocloric 0,01 M (1 : 4), roi pha loang thanh 10 ml bang cung hon hp dung moi.

Dung dch oi chieu (1): Pha loang 1,5 ml dung dch th vi hon hp ethanol - dung dch acid hydrocloric 0,01 M (1 : 4) thanh 100 ml.

Dung dch oi chieu (2): Pha loang 1 ml dung dch th vi hon hp ethanol - dung dch acid hydrocloric 0,01 M (1 : 4) thanh 100 ml

Cach tien hanh: Cham rieng biet len ban mong 10 ml moi dung dch tren. Trien khai sac ky en khi dung moi i c khoang 15 cm, lay ban mong ra e kho ngoai khong kh va phun dung dch kali iodobismuthat (TT). Tren sac ky o, ngoai vet chnh, bat ky vet phu nao cua dung dch th, khong c am mau hn vet cua dung dch oi chieu (1) (1,5%) va ch c mot vet phu ( pha tren vet chnh) am mau hn vet cua dung dch oi chieu (2) (1%).

Sulfat

Khong c qua 0,1% (Phu luc 9.4.14).

Lay 5 ml dung dch S pha loang thanh 20 ml bang nc, lay 15 ml dung dch nay e tien hanh th.

Mat khoi lng do lam kho

T 1,5 en 3,0% oi vi dang hemihydrat va t 5,0 en 7,5% oi vi dang sesquihydrat (Phu luc 9.6).

(0,50 g; 100 105 oC).

nh lng

Hoa tan 0,350 g che pham trong hon hp gom 10 ml acid acetic khan (TT) va 20 ml dioxan (TT) dung 0,05ml dung dch tm tinh the (TT). Chuan o bang dung dch acid percloric 0,1 N (C). Song song lam mau trang.

1 ml dung dch acid percloric 0,1 N (C) tng ng vi 39,74 mg C18H21NO3. H3PO4.

Bao quan

Trong bao b kn, tranh anh sang. oc bang B, gay nghien.

Loại thuốc

Giam au, chong ho, tr tieu chay.

Che pham

Vien nen, dung dch uong, dung dch tiem.