LC-MS/MS方法检测人血浆中普伐他汀的浓度

LC-MS/MS determination of pravastatin in human plasma

目的:建立液质联用法测定人血浆中普伐他汀的浓度。方法:空白血浆加普伐他汀和内标,液液萃取后采用LC-MS/MS进行分析。采用日本Inertsil ODS-3柱(2.1mm×50mm,5μm),流动相为乙腈-1mmol.L-1甲酸铵水溶液(含0.1%甲酸)(60:40,v/v),流速为0.2mL.min-1,柱温40℃,进样量为10μL,采用ESI正离子方式进行检测,用于定量分析的监测离子为m/z448→327.7(普伐他汀)和m/z483.2→258.6(罗素他汀)。结果:本方法线性范围为0.957～510ng.mL-1(r=0.9991),最小检出浓度为0.957ng.mL-1,绝对回收率均在75%以上,相对回收率在80%～120%之间,日内、日间RSD均小于15%。结论:本方法经济、简便、灵敏,适用于普伐他汀血药浓度检测和药代动力学研究。

Objective：To establish an LC - MS/MS method for determination of pravastatin in human plasma. Methods： After addition of rosuvastatin （ internal standard） with liquid - liquid extraction, the analysis involved a Incrtsil ODS - 3 （2. 1 mm × 50 mm ,5 μm） column. The mobile phase consisted of acetonitrile - 1 mmol · L^- 1 ammonium formate water solution （ include 0. 1% formic acid） （60： 40, v/v） at a flow rate of 0. 2 mL · min^ -1, the column temperature was set at 40 ℃. ESI^＋ was performed in the MRM mode using target ions at m/z 448→327.7 （ pravastatin） and m/z 483.2→258.6 （rosuvastatin）. Results ：The peak area of pravastatin in plasma showed good linearity in the range of 0. 957 -510 ng · mL^-1 （r =0. 9991 ） ,and the LLOQ of pravastatin in plasma was 0. 957 ng · mL^-1. The extracted recovery was 〉 75% , and the relative recovery was 80% -120% , the intra -and inter- day RSDs were 〈 15 %. Conclusion：This method is sensitive, simple and accurate. And it can be used for determination of pravastatin sodium tablets plasma concentration and it＇ s pharmacokinetic study.