【摘要】 目的:建立测定人血浆中二甲双胍浓度的液相色谱-电喷雾质谱联用（LC/ESI-MS-MS）法。方法:待测血浆0.2 mL经甲醇沉淀除去蛋白,离心,取上清液5 μL在氰基柱上分离,流动相为甲醇-20 mmol·L^-1醋酸铵水溶液（30:70）,流速为1.0 mL·min^-1,LC/ESI-MS-MS 多反应离子检测,正离子模式,用于定量分析的离子分别是二甲双胍 m/z 130.1→70.7和吗啉双胍（内标）m/z 172.2→59.6。结果:血浆中无干扰测定的内源性物质,每个样品分析时间小于5 min,线性范围为10.08～1008 ng·mL^-1,定量下限为10.08 ng·mL^-1,日内、日间精密度均小于10%,提取回收率大于85%。结论:该法操作快速、简单、准确、灵敏度高,适用于临床药代动力学研究。更多还原

【Abstract】 Objective:To develop a sensitive and specific LC/electrospray ionization（ESI）-MS-MS method for determination of mefformin in human plasma.Methods:The analyte was treated by methanol precipitation to remove protein component from human plasma,then separated on a cyano-column.The mobile phase consisted of methanol-20 mmol·L^-1ammonium acetate solution（30:70）,at a flow rate of 1.0 mL·min^-1.A mass spectrome- ter equipped with electrospray ionization source was used as detector and operated in the positive ion mode.In multi- ple reaction monitoring（MRM）mode,the ion combinations of m/z 130.1→70.7 and m/z 172.2→59.6 were used to qualify mefformin and internal standard（moroxydine）,respectively.Results:Chromatograms showed no endogenous in- terfering peaks with the respective blank human plasma samples.Each analysis was completed within 5 min.The cali- bration was linear in the concentration range of 10.08-1008 ng·mL^-1,and quantitative limit was 10.08 ng·mL^-1. The intra-day and inter-day RSDs were less than 10%.The recovery of the extraction was more than 85%.Conclu- sions:The method is proved to be suitable for clinical investigation of mefformin pharmacokinetics,which offers advan- tages of specificity,quickness,and higher sensitivity over the previously reported methods.更多还原