人血浆中马钱子碱的LC-MS/MS法测定  

Determination of Brucine in Human Plasma by LC-MS/MS

作　　者：林滨[1] 王贤亲[1] 林丹[1] 李艳霞[1] 

机构地区：[1]温州医学院分析测试中心,浙江温州325035

出　　处：《中国医药工业杂志》2008年第3期206-208,共3页Chinese Journal of Pharmaceuticals

摘　　要：建立了LC-MS/MS法测定人血浆中马钱子碱浓度。采用C18柱,流动相为乙腈-0.2%甲酸溶液(60:40),乌头碱为内标。电喷雾离子源(ESI),正离子检测,采用多反应监测方式进行定量分析,检测离子分别为m/z395→324、263(马钱子碱),m/z646→586、526(内标)。血浆中马钱子碱浓度在4～400ng/ml范围内线性关系良好,最低定量限为4ng/ml。马钱子碱的萃取回收率为86.0%～91.0%,日内及日间RSD分别低于6%和7%。A LC-MS/MS method was established for the determination of brucine in human plasma. A C18 column was used, with mobile phase of acetonitrile-0.2 % formic acid（60：40）. Aconitine was used as the internal standard. Electrospray ionization （ESI） source was applied and operated in positive ion mode. Multiple reaction monitoring （MRM） mode was used. The detected ions were m/z 395→324, 263 （brucine）, m/z 646→586, 526 （aconitine）. The calibration curve of brucine was linear in the concentration range of 4 - 400ng/ml. The LLOQ was 4ng/ml. The average extraction recovery was 86.0 % - 91.0 %. The RSDs of inter- and intra-day were less than 6 % and 7 %.

关 键 词：马钱子碱 乌头碱 液相色谱-串联质谱 测定 

分 类 号：TQ460.72[医药卫生—药物分析学] O657.63[化学工程—制药化工]