问题：帮忙查找磷酸左旋咪唑的质量标准
类型：求助 (悬赏分:3分)
提问：Tom
等级：▲
版块：有机化学问题(jimuwei,fpcwin1211,netpanda,yjgzfl,Ftian,)
信誉：100%
回复：15
阅读：1891
时间：2005-07-14 10:31:25 编辑加入/取消收藏订制/取消短消息举报该贴

磷酸左旋咪唑Levamisole Phosphate

需要英国药典的标准，可能在兽药典上。

急用，谢谢

回复人：Tom,▲ (Pharma) 时间：2005-07-15 11:55:12 编辑	1楼
?

回复人：Tom,▲ (Pharma) 时间：2005-07-25 13:05:32 编辑	2楼
谁能提供？很感谢

回复人：qyl1970,★ (专注于有机合成，接受公斤级化合物定制。) 时间：2005-07-27 10:04:07 编辑	3楼
有EP的标准，是否需要？

回复人：qyl1970,★ (专注于有机合成，接受公斤级化合物定制。) 时间：2005-07-27 10:10:59 编辑	4楼
药典上提供均是盐酸盐，未见到磷酸盐！？

回复人：Tom,▲ (Pharma) 时间：2005-08-01 10:19:22 编辑	5楼
有磷酸盐，Ep的也可以。就想找一个参考，自己不可能定标准，其实很费时、费事，目前我们还不可能。

回复人：qyl1970,★ (专注于有机合成，接受公斤级化合物定制。) 时间：2005-08-01 10:59:16 编辑	6楼
EP上的是盐酸盐，不知是否需要？

回复人：qyl1970,★ (专注于有机合成，接受公斤级化合物定制。) 时间：2005-08-01 11:02:35 编辑

7楼

Levamisole Hydrochloride

　

　

(Ph Eur monograph 0726)

C11H12N2S,HCl 240.8 16595-80-5

Ph Eur

--------------------------------------------------------------------------------

Definition

(6S)-6-Phenyl-2,3,5,6-tetrahydroimidazo[2,1-b]thiazole hydrochloride.

Content

98.5 per cent to 101.0 per cent (dried substance).

Characters

Appearance

White or almost white crystalline powder.

Solubility

Freely soluble in water, soluble in alcohol, slightly soluble in methylene chloride.

Identification

A. It complies with the test for specific optical rotation (see Tests).

B. Infrared absorption spectrophotometry (2.2.24).

Preparation

Discs.

Comparison

Levamisole hydrochloride CRS.

C. It gives reaction (a) of chlorides (2.3.1).

Tests

Solution S

Dissolve 2.50 g in carbon dioxide-free water R and dilute to 50.0 ml with the same solvent.

Appearance of solution

Solution S is clear (2.2.1) and not more intensely coloured than reference solution Y7 (2.2.2, Method II).

pH (2.2.3)

3.0 to 4.5 for solution S.

Specific optical rotation (2.2.7)

-121° to -128° (dried substance), determined on solution S.

Related substances

Liquid chromatography (2.2.29).

Prepare the solutions immediately before use, protect from light and keep below 25°C.

Test solution

Dissolve 0.100 g of the substance to be examined in methanol R, add 1.0 ml of concentrated ammonia R and dilute to 10.0 ml with methanol R.

Reference solution (a)

Dissolve 50 mg of levamisole hydrochloride for system suitability CRS in methanol R, add 0.5 ml of concentrated ammonia R and dilute to 5.0 ml with methanol R.

Reference solution (b)

Dilute 1.0 ml of the test solution to 100.0 ml with methanol R. Dilute 5.0 ml of the solution to 25.0 ml with methanol R.

Column:

size: l = 0.10 m, Ø = 4.6 mm,

stationary phase: base-deactivated octadecylsilyl silica gel for chromatography R (3 mm).

Mobile phase:

mobile phase A: dissolve 0.5 g of ammonium dihydrogen phosphate R in 90 ml of water R; adjust to pH 6.5 with a 40 g/l solution of sodium hydroxide R and dilute to 100 ml with water R,

mobile phase B: acetonitrile R,

Flow rate

1.5 ml/min.

Detection

Spectrophotometer at 215 nm.

Equilibration

At least 4 min with the mobile phase at the initial composition.

Injection

10 ml.

Relative retention

With reference to levamisole (retention time = about 3 min): impurity A = about 0.9; impurity B = about 1.4; impurity C = about 1.5; impurity D = about 1.6; impurity E = about 2.0.

System suitability

Reference solution (a):

the chromatogram obtained is similar to the chromatogram supplied with levamisole hydrochloride for system suitability CRS.

Limits:

correction factors: for the calculation of contents, multiply the peak areas of the following impurities by the corresponding correction factor: impurity A = 2.0; impurity B = 1.7; impurity C = 2.9; impurity D = 1.3; impurity E = 2.7,

impurities A, B, C, D or E: for each impurity, not more than the area of the principal peak in the chromatogram obtained with reference solution (b) (0.2 per cent),

any other impurity: not more than half the area of the principal peak in the chromatogram obtained with reference solution (b) (0.1 per cent),

total: not more than 1.5 times the area of the principal peak in the chromatogram obtained with reference solution (b) (0.3 per cent),

disregard limit: 0.25 times the area of the principal peak in the chromatogram obtained with reference solution (b) (0.05 per cent).

Heavy metals (2.4.8)

Maximum 20 ppm.

12 ml of solution S complies with limit test A. Prepare the standard using lead standard solution (1 ppm Pb) R.

Loss on drying (2.2.32)

Maximum 0.5 per cent, determined on 1.000 g by drying in an oven at 100-105°C for 4 h.

Sulphated ash (2.4.14)

Maximum 0.1 per cent, determined on 1.0 g.

Assay

Dissolve 0.200 g in 30 ml of alcohol R and add 5.0 ml of 0.01M hydrochloric acid. Carry out a potentiometric titration (2.2.20), using 0.1M sodium hydroxide. Read the volume added between the 2 points of inflexion.

1 ml of 0.1M sodium hydroxide is equivalent to 24.08 mg of C11H13ClN2S.

Storage

Protected from light.

Impurities

A. 3-[(2RS)-2-amino-2-phenylethyl]thiazolidin-2-one,

B. 3-[(E)-2-phenylethenyl]thiazolidin-2-imine,

C. (4RS)-4-phenyl-1-(2-sulphanylethyl)imidazolidin-2-one,

D. 6-phenyl-2,3-dihydroimidazo[2,1-b]thiazole,

E. 1,1¢-[(disulphane-1,2-diyl)bis(ethylene)]bis[(4RS)-4-phenylimidazolidin-2-one].

--------------------------------------------------------------------------------

Ph Eur

Action and use

Anthelmintic.

回复人：Tom,▲ (Pharma) 时间：2005-08-01 13:44:14 编辑	8楼
感谢qyl1970。《英国药典》由三卷本组成。其中两卷为英国药典、一卷为英国兽药典（兽医药品部分）。我需要左旋咪唑的磷酸盐英国药典规格。可能在比较老的版本上。

回复人：Tom,▲ (Pharma) 时间：2005-08-02 08:50:19 编辑	9楼
往上顶顶

回复人：Tom,▲ (Pharma) 时间：2005-08-04 09:21:39 编辑	10楼
.......

回复人：Tom,▲ (Pharma) 时间：2005-08-05 09:01:59 编辑	11楼
......

回复人：olive,▲ () 时间：2005-09-12 16:27:22 编辑	12楼
请问qyl1970， octadecylsilyl silica gel for chromatography R 是什么啊？我们现在要用到这个东西，但糊里糊涂快愁死了是反碳柱么？

回复人：Tom,▲ (Pharma) 时间：2005-11-10 15:38:23 编辑	13楼
已经打分了。

回复人：qyl1970,★ (专注于有机合成，接受公斤级化合物定制。) 时间：2005-11-10 16:21:40 编辑	14楼
C18柱的一种,十八烷基键合硅胶柱.

回复人：我爱我家,▲ () 时间：2005-12-19 15:07:56 编辑	15楼
其中carbon dioxide-free water 如何翻译？

得分人：qyl1970-1,

问题讨论没有结束...

您尚未进入本论坛,登录之后才可以回贴

8msec