UPLC法同时测定清金益气颗粒中橙皮苷、黄芩苷、甘草酸含量

Simultaneous determination of hesperidin,baicalin and glycyrrhizic acid in Qingjin Yiqi Granules by UPLC method

[目的]建立1种能够同时测定清金益气颗粒中橙皮苷、黄芩苷、甘草酸含量的超高效液相色谱(UPLC)。[方法]色谱柱为Waters CORTECS UPLC T3(2.1 mm×100 mm,1.6μm),以0.1%磷酸水溶液(A)-乙腈(B)为流动相,梯度洗脱(0~13 min,11%B;13~18 min,11%~15%B;18~35 min,15%B;35~45 min,15%~26%B;45~55 min,26%~40%B;55~60 min,40%B),流速为0.3 mL/min,柱温为30℃,进样体积为2μL,检测波长为237 nm、280 nm。[结果]3种成分在所设浓度范围内线性关系良好(r^(2)≥0.9998),精密度、重复性RSD均小于2%,平均加样回收率为90%~99%,RSD均小于5%,常温放置24 h内稳定性良好。[结论]此方法稳定准确、重复性好,可为清金益气颗粒的质量评价提供一定的参考依据。

[Objective]To establish an ultra-performance liquid chromatography(UPLC)method for simultaneous determination of hesperidin,baicalin and glycyrrhizic acid in Qingjin Yiqi Granules.[Methods]The chromatography was performed on Waters CORTECS UPLC T3 column(2.1 mm×100 mm,1.6μm)and the mobile phase was 0.1%phosphoric acid aqueous solution(A)-acetonitrile(B),which was processed as follows:11%B at 0~13 min,11%~15%B at 13~18 min,15%B at 18~35 min,15%~26%B at 35~45 min,26%~40%B at 45~55 min,40%B at 55~60 min.The flow rate was 0.3 mL/min,the column temperature was set at 30℃,the injection volume was 2μL,and the detection wavelength was 237 nm and 280 nm.[Results]The linearity of the three components in the set concentration range was good(r^(2)≥0.9998),the relative standard deviation(RSD)of the precision and repeatability were less than 2%,the average recoveries were 90%~99%with RSD were less than 5%,and the stability was good at room temperature for 24 h.[Conclusion]The method was stable,accurate and reproducible,which could provide a certain reference for the quality evaluation of Qingjin Yiqi Granules.