LC-MSMS法测定人血浆中曲司氯铵的浓度.pdfVIP

食品与药品 Food and Drug 2009 年第 11卷第 11期 29 LC-MS/MS法测定人血浆中曲司氯铵的浓度 1 2 1 仲 浩 ，刘宗平 ，姚庆强 （1. 山东省医学科学院药物研究所，山东 济南 250062 ；2 ．禹城市人民医院，山东 禹城 251200 ） 摘 要：目的 建立测定人血浆中曲司氯铵浓度的LC-MS/MS方法。方法 血浆样品经液-液提取后，以甲醇 （含0.1 % 乙 酸）: 水 （含0.1 % 乙酸+2.5 mmol/L 甲酸铵） （80 ﹕20 ）为流动相，使用Agilent 1100 VL型离子阱质谱仪，电喷雾离子源 正离子模式，采用多反应离子监测方式测定曲司氯铵 （MRM ，m/z 392→164+ 182 ）。结果 血浆中曲司氯铵线性范围为 0.1～10.0 ng/mL ，定量下限为0.1 ng/mL ，准确度85 %～115 %，日内、日间精密度(RSD) ±15 % 。结论 该方法准确，专属 性强，可用于曲司氯铵药动学研究。 关键词：曲司氯铵；LC-MS/MS；药动学 中图分类号：R983 文献标识码： A 文章编号：1672-979X(2009)11-0029-03 Determination of Trospium Chloride in Human Plasma by LC-MS/MS 1 2 1 ZHONG Hao , LIU Zong-ping , YAO Qing-qiang ( 1. Institute of Materia Medica, Shandong Academy of Medical Sciences, Jinan 250062, China; 2. The People’s Hospital of Yucheng City, Yucheng 251200, China) Abstract: Objective To establish a LC-MS/MS method to determine trospium chloride in human plasma ．Methods The plasma samples were prepared by liquid-to-liquid extraction ，then separated on a Zorbax SB-C18 column ( 150 mm × 4.6 mm)with methanol(containing 0.1 % HAc)-H O(containing 0.1 % HAc and 2.5 mmol/L ammonium 2 formate) (80:20) as the mobile phase ．An electrospray ionization source(ESI) was applied and operated in the positive ion mode ．The multiple reactions monitoring (MRM)mode was used and trospium chloride was quantified by monitoring the ion transition of m/z 392 → 164+ 182 ．Results The linear calibration curve was obtained over the concentration range of 0.1~ 10 ng/mL in plasma ．The lower limit of quantitation was 0.1ng/mL ．The accuracy was within 85 % ~ 115 % and the wit