胃得康胶囊质量标准研究

目的主要建立胃得康胶囊质量标准中HPLC测定有效成分延胡索乙素含量的方法和佛手、延胡索乙素、石菖蒲的薄层层析鉴别方法。方法采用色谱柱为Diamonsil(钻石)C18柱(5 um,200×4.6 mm,);流动相在查阅文献的基础上通过优化后确定为:甲醇一0.1%磷酸(三乙胺调pH值=6.0)(62:38);流速:1.0 mL/min;检测波长:254 nm。结果延胡索乙素的线性范围为12~192μg,相关系数R2=0.9999;加样回收率为99.3%(RSD3.2)。佛手、延胡索乙素、石菖蒲薄层层析鉴别采用硅胶254薄层板,展开剂通过实验筛选分别用正已烷一乙酸乙酯(3:1)、正已烷一甲醇一乙酸乙酯一浓氨水(8:2:2:0.1)、石油醚(60~90℃)一乙酸乙酯(3:1)。结论含量测定方法稳定,结果准确,重现性好;薄层层析鉴别方法的色谱中,样品均能在对照品色谱相应的位置上显相同颜色的斑点。可作为本制剂的含量测定方法和薄层层析鉴别方法。

STUDY OF QUALITY STANDARD FOR WEIDEKANG CAPSULE

Objective： To establish HPLC method for measuring the content of the effective component-tetra hydropalmatine and TLC method for identifying Citrus medica var. sarcodactylis, tetrahydropalmatine and Acorus gramineus in Weidekang capsule. Methods： The chromatographic column is Diamonsil Cls （5 μm, 200 × 4.6 mm）, mobile phase is optimized after reviewing references as 62 to 38 for methanol-0.1% phosphate （adjusted PH=6 by triethylamine）, flow rate is 1.0 mL/min, detection wavelength is 254 nm. Results： The linear range of tetrahydropalmatine is 12-192ug, correlation coefficient R2 is 0.9999, recovery rate is 99.3% （RSD 3.2）. The developing solvents are N-hexane-ethyl acetate （3：1）, N-hexane-methanol-ethyl acetate-concentrated aqueous ammonia （8：2：2：0.1）, petroleum ether （60-90 ℃ ）-Ethyl acetate （3 ： l ） for C. medica var. sarcodactylis, tetrahydropalmatine andA. gramineus＇s TLC identification in which silica gel 254 thin layer plates are used respectively. Conclusion： The method is stable, accurate and reproducible well. The samples can display the spots with the same color as the reference standard chromatography in TLC identification. In a word, the HPLC can be used as the content measuring method and identification method for this capsule.