PARACETAMOL

Paracetamolum

 

 

 

 

C8H9NO2 P.t.l: 151,2

Paracetamol la N-(4-hydroxyphenyl) acetamid, phai cha t 99,0 en 101,0% C8H9NO2, tnh theo che pham a lam kho.

Tnh chat

Bot ket tinh trang, khong mui. Hi tan trong nc, rat kho tan trong cloroform, ether, methylen clorid, de tan trong dung dch kiem, ethanol 96%.

nh tnh

Co the chon mot trong hai nhom nh tnh sau:

Nhom I: A, C.

Nhom II: B, C, D, E.

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

B. Hoa tan 0,1 g che pham trong methanol (TT) va pha loang thanh 100,0 ml vi cung dung moi. Lay 1,0 ml dung dch, them 0,5 ml dung dch acid hydrocloric 0,1 M (TT), them methanol (TT) thanh 100,0 ml. Bao quan dung dch nay tranh anh sang va em o ngay o hap thu (Phu luc 4.1) bc song cực đại 249 nm. A(1%, 1 cm) phai trong khoang 860 - 980.

C. iem chay (Phu luc 6.7): 168 172 oC

D. un nong 0,1 g che pham trong 1 ml acid hydrocloric (TT) trong 3 phut, them 1 ml nc, lam lanh trong a, khong co tua tao thanh. Them 0,05 ml dung dch kali dicromat (TT) 0,49%, xuat hien mau tm va khong chuyen sang mau o.

E. Che pham phai co phan ng cua nhom acetyl (Phu luc 8.1). Thc hien phan ng bang cach un trc tiep tren la.

Tap chat lien quan

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

Cac dung dch c chuan b ngay khi tien hanh th nghiem

Dung dch th: Hoa tan 0,200 g che pham trong 2,5 ml methanol (TT) co cha 0,46% dung dch tetrabutylamoni hydroxyd 40% va pha loang thanh 10,0 ml vi hon hp ong the tch cua dung dch dinatri hydrophosphat 1,79% va dung dch natri dihydrophosphat 0,78%.

Dung dch oi chieu (1): Pha loang 1,0 ml dung dch th thanh 50,0 ml vi pha ong. Pha loang 5,0 ml dung dch nay thanh 100,0 ml vi pha ong.

Dung dch oi chieu (2): Pha loang 1,0 ml dung dch oi chieu (1) thanh 10,0 ml vi pha ong.

Dung dch oi chieu (3): Hoa tan 5,0 mg 4-aminophenol (TT), 5 mg paracetamol chuan (ĐC) va 5,0 mg cloroacetanilid (TT) trong methanol (TT) va pha loang thanh 20,0 ml vi cung dung moi. Pha loang 1,0 ml dung dch nay thanh 250,0 ml vi pha ong.

Dung dch oi chieu (4): Hoa tan 20,0 mg 4-nitrophenol (TT) trong methanol (TT) va pha loang thanh 50,0 ml vi cung dung moi. Pha loang 1,0 ml dung dch nay thanh 20,0 ml vi pha ong.

Pha ong: Hon hp gom 375 the tch dung dch dinatri hydrophosphat 1,79%, 375 the tch dung dch natri dihydrophosphat 0,78% va 250 the tch methanol (TT) co cha 0,46% cua dung dch tetrabutylamoni hydroxid 40%.

ieu kien sac ky:

Cot: Cot thep khong g (25 cm x 4,6 mm) c nhoi pha tnh B (5 m). Duy tr nhiet o cot 35 C

Toc o dong: 1,5 ml/phut

Detector quang pho t ngoai bc song 245 nm

The tch tiem: 20 l.

Cach tien hanh: Tiem cac dung dch oi chieu.

Lay paracetamol lam oi chieu (thi gian lu khoang 4 phut): Thi gian lu tng oi cua tap chat K khoang 0,8; tap chat F khoang 3; tap chat J khoang 7.

Phep th ch co gia tr khi tren sac ky o cua dung dch oi chieu (3):

o phan giai gia pic cua tap chat K va pic cua paracetamol t nhat la 4;

T le gia tn hieu va nhieu cho pic cua tap chat J t nhat la 50.

Tiem dung dch th va tien hanh chay sac ky vi thi gian gap 12 lan thi gian lu cua pic paracetamol.

Tren sac ky o cua dung dch th:

Dien tch pic tap chat J: khong qua 0,2 lan dien tch cua pic tng ng tren sac ky o thu c cua dung dch oi chieu (3) (10 phan trieu)

Dien tch pic tap chat K: khong ln hn dien tch cua pic tng ng tren sac ky o thu c cua dung dch oi chieu (3) (50 phan trieu).

Dien tch pic tap chat F: khong ln hn 0,5 lan dien tch cua pic tng ng tren sac ky o thu c cua dung dch oi chieu (4) (0,05%).

Dien tch pic cua bat ky tap chat nao khac: khong ln hn 0,5 lan dien tch cua pic chnh tren sac ky o thu c cua dung dch oi chieu (1) (0,05%).

Tong dien tch pic cua cac tap chat khac: khong ln hn dien tch cua pic tng ng tren sac ky o thu c cua dung dch oi chieu (1) (0,1%).

Bo qua cac pic co dien tch nho hn dien tch cua pic chnh tren sac ky o thu c cua dung dch oi chieu (2) (0,01%).

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 


Hnh .....Sac ky o cua th nghiem cac tap chat lien quan

 

1. Tap chat K 5. Tap chat C 9. Tap chat F

2. Paracetamol 6. Cac tap chat E va D 10. Tap chat I

3. Tap chat B 7. Tap chat G 11. Tap chat J

4. Tap chat A 8. tap chat H

Ghi chu:

Tạp chất A: N-(2-hydroxyphenyl)acetamid

Tạp chất B: N-(4-hydroxyphenyl)propanamid

Tạp chất C: N-(3-cloro-4-hydroxyphenyl)acetamid

Tạp chất D: N-phenylacetamid

Tạp chất E: 1-(4-hydroxyphenyl)ethanon

Tạp chất F: 4-nitrophenol

Tạp chất G: 1-(4-hydroxyphenyl)ethanon oxim

Tạp chất H: 4-(acetylamino)phenyl acetat

Tạp chất I: 1-(2-hydroxyphenyl)ethanon

Tạp chất J: N-(4-clorophenyl)acetamid (cloroacetanilid)

Tạp chất K: 4-aminophenol.

Kim loai nang

Khong c qua 20 phan trieu (Phu luc 9.4.8).

Hoa tan 1,0 g che pham trong hon hp nc - aceton (15 : 85) roi pha loang thanh 20,0 ml bang cung dung moi. Lay 12 ml dung dch nay th theo phng phap 2. Dung dung dch ch mau 1 phan trieu thu c bang cach pha loang dung dch ch mau 100 phan trieu (TT) vi hon hp dung moi tren e chuan b mau oi chieu.

Mat khoi lng do lam kho

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

Dung 1,000 g che pham; say 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 0,300 g che pham trong hon hp gom 10 ml nc va 30 ml dung dch acid sulfuric loang (TT). un soi hoi lu trong 1 gi, lam lanh va pha loang thanh 100,0 ml bang nc. Lay 20,0 ml dung dch, them 40 ml nc, 40 g nc a, 15 ml dung dch acid hydrocloric loang (TT) va 0,1 ml dung dch feroin (TT). nh lng bang dung dch amoni ceri sulfat 0,1 M (C) cho en khi xuat hien mau vang xanh. Song song tien hanh mau trang trong cung ieu kien.

1 ml dung dch amoni ceri sulfat 0,1 M (C) tng ng vi 7,56 mg C8H9NO2.

Bao quan

Trong lo kn, tranh anh sang.

Loai thuoc

Ha nhiet, giam au.

Che pham

Vien nen, vien bao phim, hon dch uong, dung dch uong, vien nen sui bot.