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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。
Objective: To develop a liquid chromatography-tandem mass spectrometry (LC / MS / MS) method for the determination of rupatadine in human plasma. METHODS: Loratadine was used as an internal standard. The plasma samples were alkalized with 0.1 mol / L sodium hydroxide and then extracted with solid-phase cartridge. The analytical column was Kromasil C18 column (150 mm × 4.6 mm, 5 μm) Was a Phenomenex Gemini C18 column (4 mm × 3.0 mm, 10 μm) with methanol-10 mmol / L ammonium formate solution (85:15) as the mobile phase. Electrospray ionization (ESI), positive ion MRM Test. Results: The analysis time of each sample was 5 min, and the plasma endogenous substance had no interference with the determination. The linear range of rupatadine was 0.011 9 ~ 15.000 0 μg / L, the regression equation Y = 2.883X + 0.009, r = 0.999, The lower limit of quantification was 0.011 9 μg / L. The intra-day and inter-day precision (RSD) were less than 10%. The average recoveries of rupatadine and internal standard were 102.0% and 104.1%, respectively. The average matrix effects were 103.7% and 106.2%, respectively, and no concentration dependence existed. Conclusion: The method is specific, sensitive and reliable. It is suitable for high-throughput analysis of plasma samples in clinical trials.