人血浆中氯吡格雷及其活性代谢物的LC-MSMS法测定.pdfVIP

• 202 • 中国医药工业杂志 Chinese Journal of Pharmaceuticals 2016, 47 (2) -~，，~. 5 药品分析与质控: ‘ffc.c.CC. CC.C.C.4阜cu民c.c.c.c. c‘.. 人血浆中氯毗格雷及其活性代谢物的 LC-MS/MS 法测定 田溪，杨秀岭*，张志清，王淑梅，董维冲 (河北医科大学第二医院药学部，河北石家庄 050000) 摘要:建立了液相色谱-串联质谱法测定人血浆中的氯毗格雷 (1) 及其活性代谢物 (2) 。以 2- 澳 -3- 甲氧基苯乙嗣 (MPB) 作为衍生化试剂，以唾氯匹定 (3) 为内标，使用 Diamonsil C8 色谱柱，流动相为己腊 1 mmol!L 乙酸锁水溶液(含oρ1% 甲酸) (80 : 20) 。使用电喷雾电离源 (ESI) ，正离子模式、多反应监测 (MRM) 监测离子对mlz 322.2• m/z 212.0(1) 、 m/z 504 .4• m/z 354.1 (2) 和 m/z 264.2• m/z 154.1 (3) 。血浆中的 1 和 2 衍生物在 0.53 ~ 52.50 ng!ml 和 2 ~ 200 ng!ml 范围 内线性关系良好，最低定量限 (LLOQ) 为 0.53 和 2.00 ng/ml，日内和日间 RSD 均小于 10% 。 关键词:氯口比格雷:活性代谢产物:液相色谱·串联质谱:测定 中图分类号: R969; 0657.r2 文献标志码:A 文章编号: 1001-8255 (2016) 02-0202-05 DOI: 10.l6522/ki.cjph.2016.02.016 Determination of Clopidogrel and Its Active Metabolite in Human Plasma by LC-MS剧fS TIAN Xi , YANG Xiuling* , ZHANG Zhiqi吨， WANG Shumei, DONG Weichong (Dept. ofPharmacy, The Second Hospital ofHebei Medical University, Shijiazhuang 050000) ABSTRACT: A LC-MS/MS method was established for the determination of clopidogrel (1) and its active metabolite (2) in human plasma. 2-Bromo-l- (3-methoxyphenyl) ethanone (MPB) was used as a derivation agent. A Diamonsil C18 column was used , with the mobile phase of acentonitrile : 1mmollL ammonium acetate solution containing 0.01 % formic acid (80 : 20) , with ticlopidine (3) as the intemal standard. An ESI source was applied in the multiple reaction monitoring (MRM) and positive ion mode , with transitions of mlz 322.2• mlz 212.0 (1) , mlz 504 .4• mlz 354.1 (2 derivative) and m/z 264.2• mlz 154.1 (3) , respectively. It was linear for 1 and 2 (derivative) in the ranges ofO.53 - 52.50 ngJml and 2 - 200 ngJml. Their LLOQs were 0.53 and 2.00 ng/ml , and