大鼠血浆中抗精神分裂症候选新药SIPI6360立体异构体的LC-MSMS法测定.pdfVIP

• 368 • 中国医药工业杂志 αlinese Journal of Phannaceuticals 2012, 43 (5) 飞药品分析与质控} 大鼠血浆中抗精神分裂症候选新药SIPI6360 立体异构体的 LC-MS/MS 法测定 周一萌1 ，孙杰2，石劲敏2，唐黎明2，林梅2* ，周斌1* (1.中国医药工业研究总院上海医药工业研究院，上海 20∞40: 2 上海市食品药品检验所，上海 201203) 摘要z 建立了液相色谱·串联质谱法拆分并测定大鼠血浆中 SIPI6360 的立体异构体.采用 Daicel Chiralpak IA 手性柱，以 甲醇为流动相，采用 ESI 源正离子模式、多反应监测进行定量分析，结果显示， (R) - (+) -SIPI6360 与(S) - (-) -SIPI6360 立体异构体分离良好，在0.5 - 100 ng/ml 浓度范围内线性关系良好.方法回收率为94.0%-102.8% ，批内和批间 RSD 小于5.2%和 1 1.4%. 关键词， SIPI6360; 精神分裂症s 立体异构体:液相色谱·串联质谱:测定 中图分类号， R969: 0657.T2 文献标志码， A 文章编号， 1 ∞1-8255 (2012)05-0368-04 Determination of the Stereoisomers of SIPI6360 in Rat Plasma by LC-MSIMS 1 2 2 2 2 Pjc ZHOU Yimeng , SUN Jie , SHI Jinmin , TANG Liming , LIN Mei *, ZHOU 8in (1. Shanghai lnstitute ofPharmaceutical lndus町 China State Institute ofPharmaceuticallndus帅\ Shanghai 200040; 2. Shanghai lnstitutefor F.ωd andDrug Control, Shanghai 201203) ABSTRACT: A LC-MSIMS method was established for the determination of the stereoisomers of SIPI6360 in rat plasma. A Daicel Chiralpak IA chiral column was used, with methanol as the mobile phase. A tandem mass spectrome创c detection was conducted using multiple reaction monitoring (MRM) under positive ionization mode with an elec位os严-ay ionization (ESI) interface.ηle (R)-(+)-form and (阶 -(-)-form were well separated, and the calibmtion c町ves were linear in the concen田tion range ofO.5 - 100 ng/rnl. The method recoveries were 94.0% - 102.8%, with intra- and inter- batch RSDs below 5.2% and 11.4%. Key Words: SIPI6360; schizophrenosis; stereoisomer; LC-MSIMS; determination 性强，急性毒性和不良反