HPLC-DAD法同时测定四黄止痢颗粒中5种成分

Simultaneous determination of five ingredients in Sihuang Zhili granules by HPLC-DAD

建立同时测定四黄止痢颗粒中小檗碱、大黄素、(R,S)-告依春、黄芩苷、甘草苷5种成分的HPLC-DAD法。采用HPLC-DAD法,使用SunFire C_(18)色谱柱(6 mm×150 mm,5μm);以0.1%磷酸水溶液(A)-乙腈(B)为流动相,梯度洗脱;流速为0.8 mL/min;柱温30℃;检测波长:小檗碱为345 nm,大黄素为254 nm,(R,S)-告依春为245 nm,黄芩苷、甘草苷为276 nm;进样体积为10μL。被测定的5种成分色谱峰均有良好的分离度,各组分具有良好的线性关系(r≥0.9995),精密度、稳定性、重复性良好,RSD均小于1.10%;平均加样回收率为98.57%~102.41%,RSD均小于1.40%。结果提示,该方法快速、简便、定量结果准确、灵敏度高,且通过方法学研究验证后,可将此方法作为四黄止痢颗粒质量标准中的质量控制方法。

To establish a HPLC-DAD method for the simultaneous determination of berberine,emodin,(R,S)-epigoitrin,baicalin,and glycyrrhizin in Sihuang Zhili granules.HPLC-DAD method was adopted by using SunFire^(TM) C_(18)(4.6 mm×150 mm,5 μm);gradient elution was 0.1% phosphoric acid aqueous solution(A)-acetonitrile(B);flow rate was 0.8 mL·min^(-1) with column temperature 30℃;detection wavelength:berberine was 345 nm,emodin was 254 nm,(R,S)-epigoitrin was 245 nm,baicalin,and glycyrrhizin was 276 nm;injection volume was 10 μL.The chromatographic peaks of the five components were all well resolved,and each component had a good linear relationship(r≥0.999 5).The precision,stability and repeatability were all good.RSD was less than 1.10%.The recovery rate was 98.57% to 102.41%,and RSD was less than 1.40%.This method is rapid,simple,accurate,and high in sensitivity.After verification by methodological studies,this method can be used as a quality control for the quality standards of Sihuang Zhili granules.