目的:建立黄白止痢颗粒的质量标准。方法:采用薄层色谱法对黄白止痢颗粒中黄连、大黄炭、白头翁进行定性鉴别,并采用高效液相色谱法测定盐酸小檗碱含量。Agilent Eclipse XDB-C18色谱柱(4.6 mm×250 mm,5μm);流动相乙腈-0.3%磷酸水溶液(32∶68),检测波长348 nm,柱温25℃,流速1.0 mL·min-1,进样量10μL。结果:在薄层鉴别中黄连、大黄炭、白头翁有良好的鉴别特征有效成分盐酸小檗碱含量在0.008 8~0.11 g·L-1具有良好的线性关系(r=0.999 1),平均加样回收率为98.58%,RSD 1.05%。结论:使用薄层色谱法对黄连、大黄炭、白头翁进行定性鉴别,操作简便、重复性好,且阴性对照无干扰;盐酸小檗碱的含量测定方法简便、快速、准确,具有良好的重复性和回收率,可作为黄白止痢颗粒的质量控制方法。
Objective:To establish the quality standard of Huangbaizhili Granules.Method:The Coptis chinensis,Rhubarb charcoal and Pulsatilla chinensis were identified by TLC and the content of berberine hydrochloride was detected by HPLC.The separation was carried out on an Agilent Eclipse XDB-C18 column(4.6 mm × 250 mm,5 μm).The mobile phase consisted of acetonitrile-0.3% phosphoric acid(32:68).The detective wavelength was set at 348 nm.The column temperature was kept at 25 ℃.The flow rate was 1.0 mL·min-1and the injection volume was 10 μL.Result:The C.chinensis,R.charcoal and P.chinensis could be identified by TLC and the calibration curve of berberine hydrochloride showed a good linearity in the range of 0.008 8-0.11 g·L-1(r =0.999 1).The average recovery was 98.58% with RSD 1.05%.Conclusion:This method to identify three main ingredients in Huangbaizhili Granules by TLC is simple and has a great repeatability.The negative control sample has no interference.The method to determine the content of berberine hydrochlorid in Huangbaizhili Granules is rapid,accurate and the results have a good repeatability and recovery.The methods can be used for the quality of the Huangbaizhili Granules.