UPLC法同时测定清金益气颗粒中橙皮苷、黄芩苷、甘草酸含量OACSTPCD
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,1.6 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.
[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.
张智贤;张碧茜;王勇
天津中医药大学,天津 301617||华润三九医药股份有限公司,深圳 518110天津现代创新中药科技有限公司,天津 300384华润三九医药股份有限公司,深圳 518110
中医学
清金益气颗粒橙皮苷黄芩苷甘草酸UPLC含量测定
Qingjin Yiqi Granuleshesperidinbaicalinglycyrrhizic acidUPLCcontent determination
《天津中医药大学学报》 2024 (006)
518-522 / 5
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