人血浆中马钱子碱的LC-MSMS法测定.pdfVIP

• 206 • 中因民药工业杂志 Chinese Joumal of Phannaceuticals 2008 , 39 (3) 人血浆中马钱子碱的LC唰MS爪fS法测定 林漓，.l.贤亲，林升，李艳霞 (温州院学院分析测试中心，浙江温州 325035) 摘要z 建立了LC-MS/MSi去测定人血浆中马钱子碱浓度.采用C -0.2% 甲酸溶液(60:40) ，乌头碱为 柱，流动相为乙脯 I8 内标.电喷雾离子源(巴SI) ，距离子检测，来用多反应监测方式进行定量是分析，检测离子分别为m/z 395→324、 263(马 钱子碱)， m/z 646呻586、 526(内标)。血浆中马钱子碱浓度在4-400ng!ml部罔内线性关系良好，最低JE最限为4ng/ml。 马钱子碱的萃取凹收率为86.0% -91.0% ，日内及日间RSD分别低于6%和7%. 关键诩z 马钱子碱;乌头碱:液相ß谱·串联质谱:测定 中团分类号: TQ460.T2; 0657.63 Jt献标识码:A 文章编号: 1001.8255(2008)03-0206.的 Determination of Brucine in Human Plasma by LC幽MS!MS LIN Bin, WANG Xian~qin， LIN Dan, LI Yan-xia (Analytica/ and Testing Center, Wenzhou Medical Co/lege, Wenzhou 325035) ABSTRACT: A LC-MSIMS method was established for the determination ofbrucine in human plasma. A C1s column was used, with mobile phase ofacetonitrile~0.2% formic acid(60:40). Aconitine was used as the intemal standard. Electrospray ionization (ESI) source was appli巳:d and operated in positive ion mode. Multiple reaction monitoring (MRM) mode was used. The detected ions were m/z 395吨324， 263 (brucine). m/z 646呻586， 526 (aconitine) .白le calibration curve of brucine was linear in the concentration range of 4 ~ 400nglml.白le LLOQ was 4nglml. The average extraction recovery was 86.0% - 91. 0%. 白le RSDs of inter.幡 and intra-day were less than 6 % and 7 % . Key Words: brucine; aconitine; LC-MSIMS; determination L腊(德国Merck公司) ，甲酸(分析纯，上海试荆总厂) ，水 马钱子碱(brucine ， 1)一般存在于马钱属植物