LC-MS／MS测定人血浆中左西孟旦

LC-MS/MS determination of levosimendan in human plasma

目的:建立LC-MS/MS法测定左西孟旦在血浆中的浓度,研究左西孟旦在健康志愿者中的药代动力学特征。方法:待测血浆1.0 mL,经0.1 mol·L-1的盐酸0.1 mL酸化后用乙酸乙酯4 mL萃取处理,采用DiamonsilTM C18(5μm,4.6 mm×150mm)色谱柱,流动相为乙腈(0.1%甲酸)-水(85∶15),LC-MS/MS选择性正离子检测法测定血浆中左西孟旦浓度。结果:血浆中内源性物质对测定无干扰,最低检测限低于0.5 ng·mL-1,在1.0～50.0 ng·mL-1范围内左西孟旦线性关系良好(r=0.9977),日内、日间RSD均小于8%,每个样品分析时间仅需5.5 min。结论:该法特异性强、灵敏度高,操作简便快速,测定结果可靠,适于进行左西孟旦药代动力学研究。

Objective：To establish an LC - MS/MS method for determination of levosimendan in human plasma. Methods： 1.0 mL plasma was acidified with 0.1 mL·0.1 mo·L^-1 HCI and extracted with 5 mL ethyl acetate. The separation was performed on DiamonsilTM C18（5μm, 150 mm×4.6 mm）. The mobile phase consisted of acetonitrile （0. 1% formic acid） - water （50：50 ） , at the flow of 1.0 mL·min^-1. Levosimendan concentrations were deter-mined by LC - MS/MS operated in the positive ion mode. Results： Chromatograms showed no endogenous interfering peaks with blank samples. The lowest detectable limit was less than 0. 5 ng·mL^-1, and a linearity obtaining in the range of 1.0- 50. 0 ng·mL^-1 was good（r =0. 9977 ） with LC -MS/MS method. The relative standard deviations of within - day and between - day determination were less than 8%. Each analysis was completed within 5.5 min. Conclusion： The method is accuracy, sensitive and simple, proved to be suitable for the study of levosimendan phar- macokinetics.