不同产地桑叶中6种化学成分含量的液相色谱-质谱联用同时测定

Simultaneous determination of six components in Mori Folium from different districts by LC-MS/MS

目的建立液相色谱-质谱联用(LC-MS/MS)方法同时测定不同产地桑叶中原儿茶酸、芦丁、异槲皮苷、紫云英苷、槲皮素、山柰酚6种化学成分含量。方法采用Agilent Eclipse Plus C18柱(2.1 mm×150 mm,3.5μm),流动相为乙腈-0.1%甲酸水溶液,梯度洗脱,流速0.3 ml.min-1,质谱采用电喷雾负离子模式电离,多反应监测(MRM)方式对6种化合物进行定量测定。结果原儿茶酸、芦丁、异槲皮苷、紫云英苷、槲皮素、山柰酚分别在10～1 000,25～2 500,80～8 000ng.ml-1,25～2 500 ng.ml-1,1～100 ng.ml-1,3～300 ng.ml-1浓度范围内线性关系良好,最低定量限分别为10,0.5,1,1,0.5,0.5 ng.ml-1。6种成分平均加样回收率分别为106.01%,94.98%,101.83%,91.38%,101.69%,103.69%。结论该方法快速、准确、重现性好,可为桑叶药材的质量控制提供依据。

Objective To develop a LC-MS/MS method for simultaneous determination of protocatechuic acid,rutin,isoquercitrin,astragalin,quercetin and kaempferol in Mori Folium from different districts.Methods The separation was completed on an Agilent Eclipse Plus C18（2.1 mm×150 mm,3.5 μm）column using 0.1%（v/v） formic acid and actonitrile as mobile phase in gradient elution mode.The flow rate was set at 0.3 ml·min-1.The mass spectrometer was operated under the negative ion mode with the ESI source and MRM mode was used for quantification.Results Protocatechuic acid,rutin,isoquercitrin,astragalin,quercetin and kaempferol were linear over the range of 10~1 000 ng·ml-1,25~2 500 ng·ml-1,80~8 000 ng·ml-1,25~2 500 ng·ml-1,1~100 ng·ml-1,3~300 ng·ml-1 and the LOQ were 10,0.5,1,1,0.5,0.5 ng·ml-1,respectively.The average recovery were 106.01%,94.98%,101.83%,91.38%,101.69%,103.69% for the six components.Conclusion The method is rapid,sensitive,accurate and reproducible,which would be applied to study the quality control of Mori Folium.