【摘要】 目的:建立人血浆中卢帕他定浓度的液相色谱-串联质谱(LC/MS/MS)检测方法。方法:以氯雷他定为内标,血浆样本经0.1 mol/L氢氧化钠碱化后用固相小柱萃取处理;分析柱为Kromasil C18柱(150 mm×4.6 mm,5μm),保护柱为PhenomenexGemini C18柱(4 mm×3.0 mm,10μm),流动相为甲醇-10 mmol/L甲酸铵水溶液(85∶15);使用电喷雾离子源(ESI),正离子多反应监测(MRM)方式进行检测。结果:每个样本分析时间为5 min,血浆中内源性物质对测定无干扰,卢帕他定线性范围为0.011 9～15.000 0μg/L,回归方程Y=2.883X+0.009,r=0.999,定量下限为0.011 9μg/L。日内、日间精密度(RSD)均小于10%,卢帕他定与内标的平均回收率分别为102.0%和104.1%,平均基质效应为103.7%和106.2%,且均不存在浓度依赖性。结论:本方法特异性强,灵敏度高,测定结果可靠,适用于临床试验中血浆样本的高通量分析。更多还原

【Abstract】 Objective: To establish LC-MS/MS method for the determination of rupatadine in human plasma by using a solid phase extraction technique.Methods: Loratadine was used as internal standard and plasma samples were alkalified by 0.1 mol/L sodium hydroxide solution,and were extracted with solid phase extraction.The extractive was separated on a Kromasill C18 analytical column(150 mm×4.6 mm,5 μm) guarded by a Phemomenex Gemini C18 column(4 mm×3.0 mm,10 μm).The mobile phase consisted of methanol-10 mmol/L ammonium formate(85∶15,v/v).Electrospray ionization(ESI) source was applied and operated in the positive multiple reactions monitoring(MRM) mode.Results: Each analysis was completed within five minutes.Chromatogram showed no endogenous interfering peaks with blank samples.Good linearity was found within 0.0119~15.0000 μg/L and with the regression equation of Y=2.883X+0.009,r=0.999.The limit of quantification was 0.0119 μg/L.The inter-and intra-day precision(RSD) were both less than 10%.The average recovery of rupatadine and loratadine were 102.0% and 104.1%,respectively.The average matrix effects of rupatadine and loratadine were 103.7% and 106.2% respectively,in which no concentration dependences were observed.Conclusions: The method is specific,sensitive and accurate,so it is suitable for the determination of rupatadine in human plasma of clinical samples.更多还原