大鼠血浆中利培酮及9-羟基利培酮的LC-MSMS法测定.pdfVIP

· 360 · 中国医药工业杂志 Chinese Journal of Pharmaceuticals 2010, 41(5) 药品分析与质控 大鼠血浆中利培酮及 9-羟基利培酮的 LC-MS/MS 法测定 高科攀1,2，陈 钧3，陈庆华1* (1. 上海医药工业研究院，药物制剂国家工程中心，上海 200437；2. 上海医药(集团)有限公司中央研究院； 3. 复旦大学药学院，上海 201203) 摘要 ：建立了 LC-MS/MS 法测定大鼠血浆中的利培酮和 9- 羟基利培酮。用蛋白沉淀法处理血样，采用 C18 色谱柱，以 0.1％ 甲酸溶液 - 甲醇 (40 ︰ 60) 为流动相，盐酸苯海拉明为内标，使用多反应监测，检测离子对分别为 m/z 411.3→191.4( 利 培酮 )、m/z 427.2→207.1(9- 羟基利培酮 ) 和 m/z 256.2→167.3( 苯海拉明 )。利培酮和 9- 羟基利培酮在 0.5 ～ 1 000 ng/ml 范围内线性关系良好，批内、批间 RSD 均小于 5％，回收率为 90％～ 110％。 关键词：利培酮；9- 羟基利培酮；液相色谱 - 串联质谱；测定 中图分类号：R917；O657.7+2 文献标志码：A 文章编号：1001-8255(2010)05-0360-03 Determination of Risperidone and 9-Hydroxyrisperidone in Rat Plasma by LC-MS/MS GAO Kepan1,2, CHEN Jun3, CHEN Qinghua1* (1. National Pharmaceutical Engineering Research Center, Shanghai Institute of Pharmaceutical Industry, Shanghai 200437; 2. Central Research Institute of Shanghai Pharmaceutical (Group) Co.; 3. School of Pharmacy, Fudan University, Shanghai 201203) ABSTRACT: A LC-MS/MS method was established for the simultaneous determination of risperidone and 9-hydroxyrispeirdone in rat plasma. The plasma samples were treated by protein precipitation. A C18 column was used with the mobile phase of 0.1％ formic acid solution-methanol (40︰60) and diphenhydramine hydrochloride as the internal standard. A multiple reaction monitoring (MRM) mode was chosen for the detection of m/z 411.3→191.4 (risperidone), m/z 427.2→207.1 (9-hydroxyrispeirdone) and m/z 256.2→167.3 (diphenhydramine). The calibration curves of risperidone and 9-hydroxyrisperidone were linear in the concentra