薄层色谱法检查熊去氧胆酸的有关物质  

TLC examination of related substances in ursodeoxycholic acid

作　　者：佟爱东[1] 劳瑞珍[1] 李思源[1] 

机构地区：[1]广州市药品检验所,广州510160

出　　处：《药物分析杂志》2012年第9期1654-1657,共4页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立熊去氧胆酸有关物质检查的薄层色谱方法。方法:以丙酮-水(9∶1)为溶剂,制备熊去氧胆酸溶液(10 mg.mL-1),鹅去氧胆酸对照溶液+熊去氧胆酸对照溶液(各0.4 mg.mL-1)、鹅去氧胆酸对照溶液(0.1 mg.mL-1)、胆石酸对照溶液(0.01 mg.mL-1)、胆酸对照溶液(0.05 mg.mL-1)、系列自身对照溶液(0.01,0.02,0.05 mg.mL-1);各点样5μL于硅胶G薄层板上,以二氯甲烷-丙酮-冰醋酸(60∶30∶3)为展开剂,以4.5%磷钼酸硫酸溶液-冰醋酸(1∶20)溶液为显色剂。结果:熊去氧胆酸与鹅去氧胆酸分离较好;熊去氧胆酸可能含有的各有关物质的斑点清晰可见。结论:本法适用于熊去氧胆酸的质量控制。Objective：To establish a TLC method for determination of the related substances in ursodeoxycholic acid. Methods： Acetone - water （ 9 ： 1 ） was used as the solvent for preparation of ursodeoxycholic acid （ 10 mg ·mL-1 ）, ursodeoxycholic acid plus chenodeoxycholic acid solution（ each at 0.4 mg·mL-1 ）, chenodeoxycholic acid control solution（0. 1 mg·mL-1）, lithocholic acid solution （0. 01 mg·mL-1）, cholic acid control solution （0.05mg·mL-1 ） ,and series of self - control solutions（0.01,0.02,0.05 mg·mL-1 ）. 5 μL of each solution was added in G plate, a mixture of methylene chloride, acetone and glacial acetic acid （60： 30：3 ）was adopted as developer, and phosphomolybdic acid- sulphuric acid solution （4.5%, w/v） -glacial acetic acid（1：20） was used as color rea- gent. Results：Ursodeoxycholic acid and the chenodeoxycholic acid can be separated well;related substances of ur- sodeoxycholic showed clearly separated principal spots. Conclusion：The established method can be used for the quality control of ursodeoxycholic acid.

关 键 词：薄层色谱法 胆石溶解药 熊去氧胆酸 有关物质限量 鹅去氧胆酸 胆酸 杂质限度检查 

分 类 号：R917[医药卫生—药物分析学]