Bo chuyen luan nay

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, de tan trong dung dch kiem, ethanol 96%, methylen clorid.

nh tnh

Co the chon mot trong hai nhom nh tnh sau:

Nhom I: A va C.

Nhom II: A, B, D va E.

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

B. Hoa tan 0,1 g che pham trong methanol (TT) va pha loang thanh 100,0 ml bang cung dung moi. Lay 1,0 ml dung dch, them 0,5 ml dung dch acid hydrocloric 10,3 g/l (TT), them methanol (TT) thanh 100,0 ml. Bao quan dung dch nay tranh anh sang va em o o hap thu (Phu luc 4.1) ngay tc khac bc song 249 nm. A (1%, 1 cm) phai trong khoang 860 - 980.

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

D. un nong 0,1 g che pham trong 1 ml acid hydrocloric (TT) trong 3 phut, them 10 ml nc, lam lanh trong a, khong co tua tao thanh. Them 0,05 ml dung dch kali dicromat 4,9 g/l (TT), 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.

Kim loai nang

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

Hoa tan 1,0 g che pham trong hon hp gom 15 the tch nc(TT) va 85 the tch aceton (TT) 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 vi hon hp dung moi tren e chuan b mau oi chieu.

4 - Aminophenol

Khong c qua 50 phan trieu.

Hoa tan 0,50 g che pham trong hon hp methanol (TT) - nc (50: 50) va pha loang thanh 10,0 ml bang cung dung moi. Them 0,2 ml dung dch co cha natri nitroprusiat (TT) 10 g/l va natri carbonat khan (TT) 10 g/l mi pha. Tron eu va e yen 30 phut. Song song chuan b mau oi chieu trong cung ieu kien, tien hanh vi 10,0 ml hon hp methanol (TT) - nc (50 : 50) cha 0,50 g paracetamol khong co 4-aminophenol va 0,5 ml dung dch 4-aminophenol 0,05 g/l trong hon hp methanol (TT) - nc (50 : 50). Mau xanh cua dung dch th khong c am hn mau cua dung dch oi chieu.

Tap chat lien quan

Phng phap sac ky lp mong (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 4,6 g/l cua dung dch tetrabutylamonium hydroxyd 400 g/l (TT) va pha loang thanh 10,0 ml vi hon hp ong the tch cua dung dch dinatri hydrophosphat 17,9 g/l (TT) va dung dch natri hydrophosphat 7,8 g/l (TT).

Dung dch oi chieu (1)

Lay 1,0 ml dung dch th, pha loang thanh 50,0 ml vi pha ong. Lay 5,0 ml dung dch nay pha loang thanh 100,0 ml vi pha ong.

Dung dch oi chieu (2)

Lay 1,0 ml dung dch oi chieu (1) pha loang thanh 10,0 ml vi pha ong.

Dung dch oi chieu (3)

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

Dung dch oi chieu (4)

Hoa tan 20,0 mg 4-aminophenol (TT) trong methanol (TT). Pha loang thanh 50,0 ml vi cung dung moi. Lay 1,0 ml dung dch nay pha loang thanh 20,0 ml vi pha ong.

ieu kien sac ky

Cot : 25 cm, 4,6 mm.

Pha tnh : octylsilyl silica gel dung cho sac ky (TT) (5 m)

Pha ong : hon hp 375 the tch cua dung dch dinatri hydrophosphat 17,9 g/l (TT), 375 the tch cua dung dch natri hydrophosphat 7,8 g/l (TT) va 250 the tch cua methanol (TT) co cha 4,6 g/l cua dung dch tetrabutylamoni hydroxid 400 g/l (TT).

Toc o dong : 1,5 ml/phut

Phat hien bc song 245 nm

The tch tiem mau 20 l.

Thi gian chay sac ky : 12 lan thi gian lu cua paracetamol.

Thi gian lu tng oi

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

Tnh tng thch cua he thong

Dung dch oi chieu (3):

o phan giai : toi thieu la 4 gia nh cua tap chat K va paracetamol

T le tn hieu nhieu : toi thieu 50 cho nh cua tap chat J

Gii han

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

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

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

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

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

Gii han bo qua e tnh toan tong cac lng tap chat khac : dien tch cua nh chnh tren sac ky o thu c cua dung dch oi chieu (2) (0,01%).

 

 

 

 

 

 

 


Sac ky o (xin scan va paste vao dum)

 

 

 

 

 

 

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

Mat khoi lng do lam kho

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

Hnh Sac ky o cua paracetamol va cac tap chat lien quan

 
Dung 1,000 g che pham; say 100-105OC).

 

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 (TT) va 30 ml dung dch acid sulfuric loang (TT). un soi hoi lu trong 1 gi, lam lanh va pha loang vi nc (TT) va u 100,0 ml. Lay 20,0 ml dung dch, them 40 ml nc (TT), 40 g nc a, 15 ml dung dch acid hydrocloric loang (TT) va 0,1 ml dung dch feroin (CT). 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.

Che pham

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

Cong dung

Ha nhiet, giam au

Cac tap chat

 

 

 

 

 

 


  1. R1 = R3 = R4 = H, R2 = OH : N-(2-hydroxyphenyl) acetamid
  2. R1 = CH3, R2 = R3 = H, R4 = OH : N-(4-hydroxyphenyl) propanamid
  3. R1 = R2 = H, R3 = Cl, R4 = OH : N-(3-cloro-4-hydroxyphenyl) acetamid
  4. R1 = R2 = R3 = R4 = H : N-phenylacetamid
  1. R1 = R2 = R3 = H, R4 = O-CO-CH3 : 4-(acetylamino) phenyl acetat

J. R1 = R3 = R4 = H, R4 = Cl : N-(4-clorophenyl) acetamid (cloroacetanilid)

 

 

 

 

 

 


  1. X = O, R2 = H, R4 = OH : 1-(4-hydroxyphenyl) ethanon

G. X = N-OH, R2 = H, R4 = OH : 1-(4-hydroxyphenyl) ethanon oxim

I. X = O, R2 = OH, R4 = H : 1-(2-hydroxyphenyl) ethanon

 

 

 

 

F. R = NO2 : 4-nitrophenol

K. R = NH2 : 4-aminophenol