LC-MS测定人血浆中匹伐他汀浓度和其应用.PDF

LC-MS 测定人血浆中匹伐他汀浓度及其应用 温金华，熊玉卿*(南昌大学医学院临床药理研究所，南昌 330006) 摘要：目的 建立 LC-MS 测定人血浆中匹伐他汀的浓度。方法 采用 Shim-pack C18 色谱柱，流动相 A 为甲醇, 流动相 B 为含 0.025% 氨水和 0.05 mmol·L1 醋酸铵的水溶液，采用梯度洗脱方式。质谱检测方式：SIM。以瑞舒伐他汀为内标, 血 浆样品用乙酸乙酯提取浓缩检测, 进行 LC-MS 分析。结果 匹伐他汀在 0.2~200.0 ng·mL1 内线性关系良好(r=0.999 9) ； 平均提取回收率均为 86.28%；日内日间 RSD 均小于 12%。结论 本方法快速、简捷、准确，适用于匹伐他汀的临床药 动学研究和血药浓度监测。 关键词：匹伐他汀；液相色谱-质谱联用；血药浓度 中图分类号：R917.101 文献标志码：B 文章编号：1007-7693(2010)01-0062-04 Determination of the Concentration of Pitavastatin in Human Plasma by LC-MS and Subsequent Application to a Clinical Study * WEN Jinhua, XIONG Yuqing (Institute of Clinical Pharmacology, Nanchang University Medical College, Nanchang 330006, China) ABSTRACT: OBJECTIVE To establish an LC-MS method for the determination of pitavastatin in the human plasma. METHODS Pitavastatin and internal standard (IS, rosuvastatin) were separated on a Shim-pack C 18 column. The mobile phase consisted of methanol/water (A/B) with 0.025% aqueous ammonia and 0.05 mmol·L1 ammonium acetate. Gradient elution mode was established. The samples were extracted with ethyl acetate and determined by LC-MS with selected ion monitoring (SIM) mode. RESULTS The linear calibration curve was obtained in the concentration range of 0.2-200.0 ng·mL1 (r=0. 999 9), the average extraction recovery was 86.28% and the RSD of inter- and intra-day were less than 12%. CONCLUSION The developed analytical method was proved accurate, rapid, convenient, and suitable for the determination of pitavastatin in the human plasma and pharmacokinetic studies of pitavastatin. KEY WORDS: pitavastatin; LC-MS; plasma drug concentration 匹伐他汀(pitavastatin)是一种新型的他汀类药 1 仪器和试药 物，能很好地改善原发性高胆固醇血症、杂合型 岛津 LC-M