| 摘要: |
| [目的] 建立LC-MS/MS测定升麻药材中3种苯丙酸类成分含量的方法。[方法]采用ACQUITY UPLC® BEH C18(2.1 ｍｍ×100 ｍｍ,1.7 μｍ)色谱柱,乙腈-0.1%甲酸水为流动相,梯度洗脱,流速为:0.3 mL/min;质谱检测器:采用ESI电离源,负离子检测,MRM监测模式,对升麻药材中苯丙酸类成分咖啡酸、阿魏酸、异阿魏酸进行含量测定。[结果] 咖啡酸、阿魏酸、异阿魏酸的线性范围分别为5~100 ng/mL,10~200 ng/mL,50~1 000 ng/mL,线性关系良好,最低定量限分别为5、10和50 ng/mL,加样回收率97.83%~98.40%。[结论] 该方法简便,快速,精密度高,重复性好,可用于同时测定升麻中咖啡酸、阿魏酸、异阿魏酸的含量。 |
| 关键词: LC-MS/MS 升麻 咖啡酸 阿魏酸 异阿魏酸 |
| DOI：10.11656/j.issn.1672-1519.2014.11.13 |
| 分类号: |
| 基金项目:国家自然科学基金项目(81001633,81173523, 81303182),国家重大新药创制项目(2012ZX09101202),国家973计划项目(2012CB723504) |
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| LC-MS/MS determination of caffeic acid, ferulic acid acid, and isoferulic acid in Rhizoma Cimicifugae |
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WANG Xiao-ming1, ZHANG Fan1, LIU Ying1,2, ZHANG Na1,2
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1.Tianjin University of Traditional Chinese Medicine, Modern Chinese Medicine-Province and Ministry Coestablished State Key Laboratory Cultivation Base, Tianjin Key Laboratory Tianjin 300193, China;2.Tianjin International Joint Academy of Biotechnology and Medicine, Tianjin, 300457
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| Abstract: |
| [Objective] To develop a LC-MS/MS method for simultaneous determination of caffeic acid, ferulic acid and isoferulic acid in the Rhizoma Cimicifugae. [Methods] Chromatographic separation was achieved with gradient elution by a ACQUITY UPLC® BEH C18 coloum (2.1 mm×100 mm,1.7 μm) hyphenated to a mass spectrometer system was operated under the MRM mode with electrospray negative ionization. The mobile phase was acetonitrile-0.1% formic acid aqueous and the flow rate was 0.3 mL/min. [Results] Caffeic acid, ferulic acid and isoferulic acid showed good linearity in the range of 5~100 ng/mL, 10~200 ng/mL, 50~1 000 ng/mL. The lower limit of quantification of the 3 essential compounds was 5, 10 and 50 ng/mL respectively. The average recoveries of the method were in the range of 97.83%~98.40%. [Conclusion] The method is fast, sensitive and reproducible. It can be used for the simultaneous determination of caffeic acid, ferulic acid and isoferulic acid in the Rhizoma Cimicifuga. |
| Key words: LC-MS/MS Rhizoma Cimicifugae caffeic acid ferulic acid isoferulic acid |
