薄层色谱法检查熊去氧胆酸的有关物质

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5 μL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(0.05 mg·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 reagent. Results:Ursodeoxycholic acid and the chenodeoxycholic acid can be separated well;related substances of ursodeoxycholic showed clearly separated principal spots. Conclusions:The established method can be used for the quality control of ursodeoxycholic acid.

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