UPLC-MS/MS法同时测定归脾丸中14种成分

Simultaneous determination of fourteen constituents in Guipi Pills by UPLC-ESI-MS/MS

目的建立UPLC-ESI-MS/MS法同时测定归脾丸中斯皮诺素、远志口山酮Ⅲ、党参炔苷、甘草苷、甘草素、黄芪甲苷、细叶远志皂苷、异甘草素、木香烃内酯、去氢木香内酯、藁本内酯、白术内酯Ⅰ、甘草次酸、茯苓酸的含量。方法该药物甲醇提取液的分析采用ACQUITY UPLC BEH C_(18)色谱柱(2.1 mm×100 mm,1.7μm);流动相乙腈-0.1%甲酸,梯度洗脱;体积流量0.25 mL/min;柱温40℃;电喷雾离子源;正负离子扫描;多反应监测模式。再进行系统聚类分析、主成分分析、偏最小二乘判别分析。结果14种成分在各自范围内线性关系良好(r>0.9995),平均加样回收率93.0%~103.9%,RSD 0.51%~1.9%。19批样品聚为3类,藁本内酯、去氢木香内酯、木香烃内酯、细叶远志皂苷为差异性成分。结论该方法稳定可靠,可用于归脾丸的质量控制。

AIM To establish a UPLC-ESI-MS/MS method for the simultaneous content determination of spinosin,polygalaxanthoneⅢ,lobetyolin,liquiritin,liquiritigenin,astragalosideⅣ,tenuifolin,isoliquiritigenin,costundide,dehydrocostus lactone,ligustilide,atractylenolideⅠ,glycyrrhetinic acid and pachymic acid in Guipi Pills by UPLC-ESI-MS/MS.METHODS The analysis of methanol extract of this drug was performed on a 40℃thermostatic ACQUITY UPLC BEH C_(18) column(2.1 mm×100 mm,1.7μm),with the mobile phase comprising of acetonitrile-0.1%formic acid flowing at 0.25 mL/min in a gradient elution manner,and electron spray ionization source was adopted in positive and negative ion scanning with multiple reaction monitoring mode.Then hierarchical cluster analysis,principal component analysis and partial least squares-discriminant analysis were performed.RESULTS Fourteen constituents showed good linear relationships within their own ranges(r>0.9995),whose average recoveries were 93.0%-103.9%with the RSDs of 0.51%-1.9%.Nineteen batches of samples were clustered into three categories,ligustilide,dehydrocostus lactone,costunolide and tenuifolin were taken as differential components.CONCLUSION This stable and reliable method can be used for the quality control of Guipi Pills.