液相色谱-电喷雾串联质谱法测定人血浆中辛伐他汀浓度  

LC-ESI-MS/MS determination of simvastatin in human plasma

作　　者：江波[1] 袁虹[1] 许东航[1] 周权[1] 阮邹荣[1] 

机构地区：[1]浙江大学医学院附属第二医院临床药理室,杭州310009

出　　处：《药物分析杂志》2007年第6期800-804,共5页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立液相色谱-电喷雾串联质谱联用测定人血浆中辛伐他汀浓度的方法。方法:色谱条件为 Discovery ODS C_(18)(2.1 mm×100 mm,3μm)色谱柱;流动相为乙腈-0.1%甲酸溶液(65:35,v/v);柱温30℃;流速0.2 mL·min^(-1);进样量5μL。质谱条件为电喷雾电离源(ESI),选择性检测定量离子为 m/z 441.3/325.0(辛伐他汀)和 m/z 427.2/325.0(洛伐他汀,内标)带正电荷的离子峰。样品用乙酸乙酯提取。结果:血浆中辛伐他汀浓度在0.20～20.0 ng·mL^(-1)内呈良好线性关系,r=0.9996。提取回收率为90.0%～92.4%(RSD 6.0%～14.9%),方法回收率在85%～115%之内,日内和日间精密度试验的RSD 均<15%,最低检测浓度为0.2 ng·mL^(-1)。结论:该测定方法经全面考察符合血浆样品的测定要求,可以应用于辛伐他汀的人体药动学研究和生物等效性评价。Objective：To establish an LC - ESI - MS/MS method for determination of simvastatin in human plasma. Methods ： LC condition： Adopted Discovery ODS ClS column （2. 1 mm ×100 mm, 3 μm） ; mobile phase consisted of acetonitrile -0. 1% formic acid（65：35 ,v/v） ;flow rate was 0. 2 mL · min^-1 ;column temperature 30 ℃. MS condition： adopted electrospray ionization（ ESI）, and selected ion mass monitoring （m/z） 441.3/325.0 （ simvastatin）, 427.2/325.0 （lovastatin, internal standard） to quantify. The plasma samples were extracted with ethyl acetate. Results： The calibration curve was linear within the range of 0. 20 - 20.0 ng mL ^- 1 （ r = 0. 9996 ）. The absolute recoveries were 90. 0% -92. 4% （ RSD 6.0% - 14. 9% ）. The method recoveries were 85% - 115%. The intra - day and inter- day RSD were less than 15% and the detection limit was 0. 2 ng · mL^-1. Conclusion：The method is validated according to the requirements of bioanalysis and is suitable for the clinical pharmacokinetical study and bioequivalence test of simvastatin.

关 键 词：辛伐他汀 液相色谱-电喷雾串联质谱法 血药浓度 

分 类 号：R917[医药卫生—药物分析学]