摘要
目的:建立同时检测Beagle犬血浆中四氢巴马汀、脱氢紫堇碱、小檗碱和巴马汀的分析方法,并应用有机溶剂沉淀法提取含药血浆中的成分。方法:采用C18反相柱,流动相为乙腈-0.1%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:366.2/350.2(四氢巴马汀)、356.2/191.2(脱氢紫堇碱)、336.2/320.2(小檗碱)和352.2/336.2(巴马汀)。测定血浆中四氢巴马汀、脱氢紫堇碱和小檗碱的线性范围均为0.0488～50μg.L-1,巴马汀为0.0488～100μg.L-1,这4种成分的定量下限均为0.0488μg.L-1,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,可用于血浆中这4种生物碱的药代动力学研究。
A sensitive liquid chromatography-tandem mass spectrometry（LC-MS/MS） was developed and validated for the simultaneous quantification of tetrahydropalmatine（THP）,dehydrocorydaline（DHC）,berberine（Ber） and palmatine（Pal） in dog plasma.The compounds were pretreated by protein precipitation using organic solvent.Chromatographic separation was achieved on a reversed-phase C18 column with the mobile phase of acetonitrile-water（0.1% acetic acid） and step gradient elution resulted at a flow rate of 0.60 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 366.2/350.2（THP）,356.2/191.2（DHC）,336.2/320.2（Ber） and 352.2/336.2（Pal）.The method showed excellent linearity over the concentration range of 0.0488-50 μg·L-1 for DHC,THP,Ber and 0.0488-100 μg·L-1 for Pal.The low limits of quantification were at 0.0488 μg·L-1.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 four alkaloids.
出处
《世界科学技术-中医药现代化》
北大核心
2012年第3期1578-1582,共5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
关键词
元胡
药代动力学
液质联用
Rhizoma Corydalis
pharmacokinetics
LC-MS/MS
