TERPIN HYDRAT

Terpinum hydratum

 

 

 

 

 

 

C10H20O2. H2O P.t.l: 190,3

Terpin hydrat la cyclohexan methanol, 4-hydroxy-a, a, 4-trimethyl monohydrat hay p-menthan 1, 8-diol monohydrat, phai cha t 98,0 en 100,5% C10H20O2, tnh theo che pham khan.

Tnh chat

Tinh the trong suot, khong mau hay bot ket tinh trang, khong mui. Say can than 100 oC, che pham se thang hoa va tao thanh nhng tinh the hnh kim. e khong kh nong va kho, che pham se dan dan b mat nc ket tinh va nhiet o nong chay giam. Hi tan trong nc, tan trong nc nong va ethanol 96%, de tan trong ethanol 96% nong, hi tan trong ether, cloroform.

nh tnh

Co the chon mot trong hai nhom nh tnh sau:

Nhom I: A, D.

Nhom II: B, C, D, E.

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

B. iem chay: 115 117 C (Phu luc 6.7). un nong dung cu ti 110 C roi mi cho ong mao quan vao va tiep tuc un nong vi toc o 4 6 C trong 1 phut.

C. Tren sac ky o thu c trong phep th "Tap chat lien quan": Vet chnh cua dung dch th phai giong ve v tr, mau sac va kch thc vi vet cua dung dch oi chieu (1).

D. Lay 5 ml dung dch che pham (1/50), un nong roi cho them vai giot acid sulfuric am ac (TT). Dung dch se b van uc va co mui thm cua terpineol.

E. Nho vao 0,01 g che pham khoang 5 giot dung dch sat (III) clorid trong ethanol (TT), em boc hi en kho trong chen s, se thay xuat hien cung mot luc cac cho khac nhau trong chen nhng mau o son, tm va luc.

o trong va mau sac cua dung dch

Dung dch S: Hoa tan 2,50 g che pham trong ethanol 96% (TT), va pha loang thanh 50 ml vi cung dung moi.

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

Gii han acid - kiem

Lay 10 ml dung dch S, them 0,1 ml dung dch xanh bromothymol (TT). Khong c dung qua 0,2 ml dung dch acid hydrocloric 0,02 N (C) hoac dung dch natri hydroxyd 0,02 N (C) e lam chuyen mau cua ch th.

Tap chat lien quan

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

Ban mong: Silica gel G (TT).

Dung moi khai trien: Cloroform - ethyl acetat (1 : 9).

Dung dch th: Hoa tan 0,25 g che pham trong methanol (TT), va pha loang thanh 5 ml vi cung dung moi.

Dung dch oi chieu (1): Hoa tan 0,25 g terpin hydrat chuan trong methanol (TT) va pha loang thanh 5 ml vi cung dung moi.

Dung dch oi chieu (2): Pha loang 1 ml dung dch oi chieu (1) thanh 100 ml bang methanol (TT).

Cach tien hanh: Cham rieng biet len ban mong 3 ml moi dung dch tren. Trien khai sac ky en khi dung moi i c khoang 15 cm. Say ban mong nhiet o 100 105 C trong 5 phut. e nguoi ban mong sau khi say, phun dung dch vanilin 1% trong acid sulfuric (TT). Tren sac ky o cua dung dch th, bat ky vet phu nao khac vi vet chnh khong c co mau am hn mau cua vet chnh tren sac ky o cua dung dch oi chieu (2).

Nc

T 8,0 - 10,0% (Phu luc 10.3).

Dung 0,20 g che pham.

Tro sulfat

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

Dung 1,0 g che pham.

nh lng

Phng phap sac ky kh (Phu luc 5.2).

Dung dch chuan noi: Hoa tan mot lng chnh xac biphenyl trong cloroform (TT) e c dung dch cha khoang 20 mg/ml.

Dung dch chuan: Can chnh xac khoang 170 mg terpin hydrat chuan (C), hoa tan bang 5 ml ethanol 96% (TT) trong bnh nh mc 100 ml, them 5,0 ml dung dch chuan noi va them cloroform (TT) en vach.

Dung dch th: Can chnh xac khoang 170 mg che pham, tien hanh nh cach chuan b dung dch chuan, bat au t "hoa tan bang 5 ml...".

ieu kien sac ky:

Cot thep khong g hoac thuy tinh (1,2 m x 3,5 mm) c nhoi at diatomit a ra acid en trung tnh va a silan hoa (chromosorb AW - 80 - 100 mesh) (TT) vi 6% chat hap phu dimethylpolysiloxan dung cho sac ky kh (TT).

Kh dan la nit dung cho sac ky kh (TT) vi lu lng can thiet e at c thi gian lu cua terpin khoang 7 phut va cua biphenyl khoang 11 phut.

Detector ion hoa ngon la.

Nhiet o cot 120 C, nhiet o cua buong tiem va detector 260 C.

The tch tiem: 1 ml.

Cach tien hanh:

Tiem dung dch chuan. o phan giai gia pic terpin va biphenyl khong c nho hn 2,0 va o lech chuan tng oi gia cac lan tiem nhac lai khong c ln hn 2,0%.

Tiem dung dch th. Tnh ham lng C10H20O2 theo ty le dien tch gia pic cua terpin va chuan noi co c t sac ky o cua dung dch th va dung dch chuan.

Bao quan

ng trong lo nut kn, tranh anh sang.

Loại thuốc

Tang tiet dch kh quan (long m).

Che pham

Thng c ket hp trong cac che pham tr ho nh: Vien uong terpin benzoat, vien uong terpin codein.