LC-MS/MS法同时测定犬血浆中7种人参皂苷类成分及其在人参提取物药代动力学研究中的应用  

Simultaneous Determination of Seven Ginsenoside Derivatives in Dog Plasma by LC-MS/MS: Application to Pharmacokinetic Study of Ginseng Extraction

作　　者：林力[1] 刘建勋[1] 张颖[1] 李欣志[1] 段昌令[1] 林成仁[1] 李磊[1] 

机构地区：[1]中国中医科学院西苑医院,北京100091

出　　处：《世界科学技术-中医药现代化》2012年第3期1572-1577,共6页Modernization of Traditional Chinese Medicine and Materia Medica-World Science and Technology

基　　金：国家自然基金项目(81102795):中药复方指征药代动力学的深入研究;负责人:林力;国家自然基金重点项目(30830118):有效中药复方功效的指征性物质基础研究;负责人:刘建勋;科学技术部国家科技重大新药创制专项(2009ZX09031-005-007):中药药效评价研究平台;负责人:刘建勋

摘　　要：目的:建立同时检测Beagle犬血浆中人参皂苷Rg1、Re、Rb1、Rd、Rc、Rb2/3和Rf的分析方法,并应用混合有机溶剂萃取法提取含药血浆中的成分。方法:采用C18反相柱,流动相为甲醇乙腈等比混合液-0.01%甲酸水溶液梯度洗脱,质谱采用多反应监测(MRM)方式进行正离子检测。结果:定量分析的离子对(m/z)为:1131.8/789.5(G-Rb1)、1101.7/789.7(G-Rb2/3)、1101.7/789.7(G-Rc)、823.6/789.5(G-Rd)、969.7/789.7(G-Re)、823.6/643.6(G-Rg1)和823.6/365.3(G-Rf)。7种皂苷类成分定量分析可以在14.5 min内完成,且没有离子抑制现象,各成分的最低定量限分别为0.03125μg.L-(1G-Re和G-Rg1)、0.0625μg.L-(1G-Rf和G-Rd)和0.125μg.L-(1G-Rb1、G-Rc和G-Rb2/3),该方法的精密度、准确度和稳定性均符合要求。结论:该法选择性强、灵敏度高、操作简便,可用于血浆中7种人参皂苷了成分的药代动力学研究。A sensitive liquid chromatography-tandem mass spectrometry（LC-MS/MS） was developed and validated for the simultaneous quantification of Ginsenoside Rg 1,Re,Rb 1,Rd,Rc,Rb 2/3 and Rf in dog plasma.The compounds were extracted by organic solvent using mixed organic solvent.Chromatographic separation was achieved on a reversed-phase C 18 column with the mobile phase of acetonitrile/menthol-water（0.01% acetic acid） and step gradient elution resulted at a flow rate of 0.23 mL.min-1.A tandem mass spectrometer equipped with electrospray ionization source was used as detector and operated in the positive ion mode.Quantification was performed using multiple reaction monitoring（MRM） of the transitions m/z 1131.8/789.5（G-Rb 1）,1101.7/789.7（G-Rb 2/3）,1101.7/789.7（G-Rc）,823.6/789.5（G-Rd）,969.7/789.7（G-Re）,823.6/643.6（G-Rg 1） and 823.6/ 365.3（G-Rf）.Seven ginsenosides were eluted within 14.5 min and can avoid matrix effect.The quantification limits of the newly developed method were 0.03125 μg.L-1 for G-Re and G-Rg 1,0.0625 μg.L-1 for G-Rf and G-Rd,0.125 μg.L-1 for G-Rb 1,G-Rc and G-Rb 2/3.The precision,accuracy and stability of the analytes meet the requirements.The method was sensitive,accurate and rapid.It can be applied in the determination of plasma concentration of seven ginsenosides.

关 键 词：人参皂苷 药代动力学 液质联用 

分 类 号：R282.71[医药卫生—中药学]