【摘要】 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。更多还原

【Abstract】 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 Inertsil 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.更多还原