天然产物研究与开发 ›› 2016, Vol. 28 ›› Issue (9): 1397-1401.doi: 10.16333/j.1001-6880.2016.9.010

• 研究简报 • 上一篇    下一篇

超高效液相色谱-三重四级杆质谱同时测定灯盏细辛中10种指标成分的含量

侯佳1，邹欢1，李勇军2,3，巩仔鹏1,3，王爱民2,3*   

  1. 1 贵州医科大学 贵州省药物制剂重点实验室；2 贵州医科大学 民族药与中药开发应用教育部工程研究中心；3 贵州医科大学药学院，贵阳 550004
  • 出版日期:2016-09-30 发布日期:2017-03-24

Simultaneous Determination of Ten Index Compounds in Erigeron breviscapus Using UPLC-MRM-MS

HOU Jia1,ZOU Huan1,LI Yong-jun2,3,GONG Zi-peng1,3,WANG Ai-min2,3*   

  1. 1 Guizhou Provincial Key Laboratory of Pharmaceutics,Guizhou Medical University; 2 Engineering Research Center for the Development and Application of Ethnic Medicine and TCM (Ministry of Education), Guizhou Medical University; 3 School of Pharmacy,Guizhou Medical University,Guiyang 550004,China
  • Online:2016-09-30 Published:2017-03-24

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摘要： 建立超高液相色谱-三重四级杆质谱同时测定灯盏细辛药材中的绿原酸、新绿原酸、隐绿原酸、野黄芩苷、灯盏甲素、芹菜素、咖啡酸、3,4-二咖啡酰基奎宁酸、3,5-二咖啡酰基奎宁酸、4,5-二咖啡酰基奎宁酸含量的分析方法。采用Waters BEH C18柱（2.1 mm × 50 mm，1.7 μm）；流动相为0.1%甲酸乙腈溶液（A）-0.1%甲酸水溶液（B），梯度洗脱，质谱采用电喷雾离子源（ESI），多反应离子监测（MRM）模式。绿原酸、新绿原酸等10个成分在选定的浓度范围内线性关系良好（r≥0.9993）。加样回收率在97.65%~105.4%，RSD为0.66%~5.9%，重复性、稳定性、精密度良好。含量测定结果显示，灯盏细辛药材中野黄芩苷含量均高于《中国药典》2015版所规定的含量限度（≥0.30%）。本方法简便、快速、灵敏度高、准确，可用于灯盏细辛药材中多指标成分的含量测定，并控制灯盏细辛药材质量。

关键词: 超高效液相色谱-三重四级杆质谱, 灯盏细辛, 指标成分, 含量测定

Abstract: An ultra-high performance liquid chromatography-multiple reactions monitoring-mass spectrometry (UPLC-MRM-MS) method was established for the simultaneous determination of ten components namely chlorogenic acid,neochlorogenic acid,cryptochlorogenic acid,scutellarin,apigenin-7-O-glucronide, apigenin, caffeic acid, 3,4-dicaffeoylquinic acid,3,5-dicaffeoylquinic acid and 4,5-dicaffeoylquinic acid in Erigeron breviscapus. A waters BEH C18 column (2.1 mm×50 mm,1.7 μm) was used for the chromatographic separation with a gradient solvent system of 0.1% formic acid in acetonitrile (A)-0.1% formic acid in water (B) as mobile phases.MRM mode was used as detection mode with electro-spray ionization (ESI) source.In certain range of concentrations,good linear relationships were established for the ten analytes.The average recoveries were 97.65%~105.4%,RSD were 0.66%~5.9%.The precision,repeatability and stability were good.The results showed that the contents of scutellarin components in E.breviscapus were all beyond the standard in Pharmacopoeia of the People’s Republic of China.The developed UPLC-MRM-MS method was simple,rapid and effective for the determination of the components in E.breviscapus. It provided a reliable way to control the quality of E.breviscapus.

Key words: UPLC-MRM-MS, Erigeron breviscapus, index compounds, content determination

中图分类号: 

R969.1

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