LC-MS/MS法测定升麻中咖啡酸、阿魏酸、异阿魏酸含量的研究  

LC-MS/MS determination of caffeic acid, ferulic acid acid, and isoferulic acid in Rhizoma Cimicifugae

作　　者：王晓明[1] 张帆[1] 刘莹[1,2] 张娜[1,2] 

机构地区：[1]天津中医药大学,天津市现代中药重点实验室-省部共建国家重点实验室培育基地,天津300193 [2]天津国际生物医药联合研究院,天津300457

出　　处：《天津中医药》2014年第11期686-689,共4页Tianjin Journal of Traditional Chinese Medicine

基　　金：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)

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誖BEH C18（2.1 mm×100 mm,1.7μm）色谱柱,乙腈-0.1%甲酸水为流动相,梯度洗脱,流速为：0.3 m L/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/m L,10～200 ng/m L,50～1 000 ng/m L,线性关系良好,最低定量限分别为5、10和50 ng/m L,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。[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誖 BEH C18coloum（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 m L/min. [Results] Caffeic acid,ferulic acid and isoferulic acid showed good linearity in the range of 5 ～100 ng/m L, 10～200 ng/m L, 50～1 000 ng/m L. The lower limit of quantification of the 3 essential compounds was 5, 10 and 50 ng/m L 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.

关 键 词：LC-MS/MS 升麻 咖啡酸 阿魏酸 异阿魏酸 

分 类 号：R285.5[医药卫生—中药学]