液相色谱-串联质谱法测定人血浆中多潘立酮的浓度

Determination of domperidone in human plasma lithium by HPLC-MS/MS

目的建立一种血浆中多潘立酮测定的液相色谱-串联质谱法。方法用蛋白沉淀法处理样品,色谱柱:Venusil XBP C_(18)(2.1 mm×50.0 mm,3μm),流动相:100%水含2 mmol·L^(-1)NH_4Ac和0.1%甲酸(A)-100%甲醇(B),流速:0.40 mL·min^(-1),柱温:40℃,梯度洗脱,进样量:20.0μL。采用电喷雾离子源,正离子模式,多反应监测。考察该方法的专属性、标准曲线和定量下限、精密度与回收率、基质效应及稳定性。结果多潘立酮在0.10~50.00ng·mL^(-1)内,线性关系良好,标准曲线为y=3.39×10^(-3)x+4.86×10^(-4)(r=0.999 1),定量下限为0.10 ng·mL^(-1),日内RSD均小于10.3%,日间RSD均小于9.7%,提取回收率可达90.1%以上。结论本方法简便快速,准确度高,灵敏度好,适用于人血浆中多潘立酮的浓度测定。

Objective To establish a HPLC-MS/MS method to determinate the concentration of domperidone in plasma.Methods The samples were treated by protein precipitation method.The chromatographic column was Venusil XBP C（18）（2.1 mm×50.0 mm,3μm）,mobile phase was 100%water containing 2 mmol·L^-1NH4Ac and 0.1% formic acid（A）-100%methanol（B）,flow rate was 0.40 mL·min^-1,column temperature was 40℃,gradient elution,injection volume was 20.0μL.The sample was measured with electrospray ion source,positive ion mode,multi-reaction monitoring.The specificity,standard curve and lower limit of quantitation,precision and recovery,matrix effect and stability were investigated.ResultsThe standard curve of domperidone was y=3.39×10^（-3）x＋4.86×10^（-4）（r=0.999 1）,and domperidone had good linear relationship in 0.10-50.00 ng·m L^-1.The limit of quantification was 0.10 ng·m L^-1.The intra-day RSD and inter-day RSD were less than 10.3% and 9.7%,respectively.The recovery rate of extraction was over 90.1%.ConclusionThe method is simple,rapid,accurate and sensitive,which is suitable for the determination of domperidone in human plasma.