超高效液相色谱-质谱联用同时测定旋覆代赭汤中15种成分含量

Simultaneous determination of fifteen components in Xuanfudaizhe decoction by UPLC-MS/MS

目的 建立同时测定旋覆代赭汤中15种成分含量的超高效液相色谱-质谱联用(UPLC-MS/MS)方法。方法 采用Shim-pack GIST C18(2.1 mm×100 mm,2.0μm)色谱柱,流动相用乙腈-0.1%甲酸,梯度洗脱,流速0.3 mL·min^(-1),柱温35℃。采用ESI源,以MRM负离子模式检测。结果 甘草苷、甘草酸、甘草素、异甘草素、异甘草苷、芹糖异甘草苷、新甘草苷、绿原酸、隐绿原酸、阿魏酸、异绿原酸A、异绿原酸C、人参皂苷Rb1、人参皂苷Re和6-姜辣素在各自浓度范围内线性关系良好(r> 0.998 6),平均回收率在97.0%~103.1%,精密度、重复性、稳定性均符合要求。结论 建立的方法简单、准确性好,可为旋覆代赭汤及其制剂的质量控制提供参考。

Objective To establish a method for simultaneous determination of fifteen components in Xuanfudaizhe decoction by UPLC-MS/MS.Methods The separation was performed on a Shim-pack GIST C18 column(2.1 mm×100 mm,2.0μm)with acetonitrile-0.1%formic acid as the mobile phase under gradient elution at a flow rate of 0.3 mL·min-1.The column temperature was 35℃.The detection was carried out via electrospray ionization(ESI).Multiple-reaction monitoring(MRM)scanning was used for quantification in a negative ion mode.Results Liquiritin,glycyrrhizic acid,liquiritigenin,isoliquiritigeni,isoliquiritin,isoliquiritin apioside,neoliquiritin,chlorogenic acid,cryptochlorogenic acid,ferulic acid,isochlorogenic acid A,isochlorogenic acid C,ginsenoside Rb1,ginsenoside Re and 6-gingerol had good linear relationships in their respective concentration ranges(r>0.9986).The average recovery ranged from 97.0%to 103.1%,and the precision,stability and repeatability of the method were good.Conclusion This method is simple and accurate,which can provide reference for Xuanfudaizhe decoction and its preparations.