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目的:建立液质联用法测定人血浆匹伐他汀浓度。方法:空白血浆加匹伐他汀,用乙酸乙酯作为萃取剂,然后用LC-MS/MS进行分析。采用Venusil XBP-C18柱(150 mm×2.1 mm,5μm),流动相为乙腈-0.1%甲酸水溶液(60∶40),流速为0.2 mL.min-1,柱温40℃,进样量为2μL。采用ESI正离子方式进行检测,用于定量分析的检测离子为m/z422→261.4,96.9。结果:本方法线性范围是0.23~117.6 ng.mL-1,r2=0.994 1,权重为1/x,最小检出浓度(LLOQ)为0.23 ng.mL-1,绝对回收率均在70%以上,相对回收率在98%~102%之间,日内、日间RSD均小于15%。结论:本方法简便、灵敏、准确,可用于血浆匹伐他汀浓度检测和生物等效性及药动学研究。
Objective: To establish a HPLC method for the determination of pitavastatin in human plasma. Methods: Blank plasma plus pitavastatin, with ethyl acetate as extractant, was then analyzed by LC-MS / MS. Venusil XBP-C18 column (150 mm × 2.1 mm, 5 μm) was used. The mobile phase was acetonitrile-0.1% formic acid solution (60:40) at a flow rate of 0.2 mL.min-1. . The ESI positive ion mode was used for detection. The detection ions for quantitative analysis were m / z 422 → 261.4, 96.9. Results: The linear range was 0.23 ~ 117.6 ng.mL-1, r2 = 0.994 1, weight was 1 / x, the minimum detectable concentration (LLOQ) was 0.23 ng.mL-1, and the absolute recoveries were above 70% , The relative recovery rate was between 98% ~ 102%, day and day RSD were less than 15%. Conclusion: The method is simple, sensitive and accurate and can be used for the determination of plasma pitavastatin concentration, bioequivalence and pharmacokinetics.