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

关键词:  清金益气颗粒  橙皮苷  黄芩苷  甘草酸  UPLC  含量测定

Key words:  Qingjin Yiqi Granules  hesperidin  baicalin  glycyrrhizic acid  UPLC  content determination

摘要:

[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，1.6 μm），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 2 μL，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（r²≥0.999 8），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。

Abstract:

[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，1.6 μm） 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（r²≥0.999 8），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.