摘要
目的建立HPLC-MS-MS方法测定人血浆中托烷司琼浓度。方法色谱柱为Hypurity C18柱（Thermo Hypersil-Keystone，2．1mm×150mm，5μm）；流动相为乙腈-0．1％甲酸水溶液-60：40；流速为0．2mL·min^-1，柱温为40℃，自动进样瓶温10℃。采用电喷雾离子源（ESI）正离子模式，用多反应监测模式（MRM）进行定量分析。用于定量分析的托烷司琼和内标的碎片离子分别为m／z 124和m／z 201。结果托烷司琼（TST）线性范围为0．22-57．25ng·mL^-1，决定系数（相关系数r的平方）为0．998，定量下限为0．22ng·mL^-1，提取回收率〉50％，日内和日间RSD均〈15％。结论此方法简便、高效、快速、和灵敏，可用于托烷司琼药动学及生物等效性研究。
Objective To establish a liquid chromatography - electrospray ionization tandem mass spectrum （HPLC- MSMS） method for the determination of tropisetron in human plasma. Methods Chromatographic column was Hypurity C18 （150 min×2. 1 mm, 5μm） ; the mobile phase was composed of methanol： acetonitrile-0. 1% formic acid= 60 ： 40, the flow rate was 0.2 mL · min^-1, and the column temperature was 40 ℃ . Results The ionization was optimized using ESI （＋） and enhanced selectivity was achieved using tandem mass spectrometric analysis via MRM functions, 285→124 for tropisetron, and 295→201 for inertal standard. The calibration curve was linear at 0.22-57. 25 ng · mL^-1 （r^2= 0. 998） for tropisetron. The extract recovery was more than 50%0. The RSD of inter-day and intraday was less than 15%. Conclusions The method is simple, rapid, efficient, sensitive and suitable for the determination the content of tropisetron in healthy volunteers. It can be used in the pharmacokinetic and bioequivalent research of tropisetron.
出处
《中南药学》
CAS
2008年第4期423-426,共4页
Central South Pharmacy
