【摘要】 目的:建立HPLC-MS法测定人血浆中的伊托必利浓度。方法:以舒必利为内标,选用液液萃取法,然后进行LC-MS/MS分析。色谱柱为Phenomenex Luna C18柱(150 mm×2.0 mm,5μm),流动相为乙腈-10 mmol.L-1甲酸胺水溶液(含0.1%甲酸)(60∶40),流速为0.2 mL.min-1,柱温40℃,进样量为10μL,质谱采用ESI正离子方式进行扫描,MRM方式检测,用于定量分析的监测离子为m/z359.9→71.9(伊托必利)和m/z343.0→112.2(舒必利)。结果:本方法线性范围是0.336~688 ng.mL-1,r=0.999 3,最低定量限为0.336 ng.mL-1。绝对回收率均在80%以上,相对回收率在85%~115%之间,日内、日间RSD均<5%。结论:本方法灵敏、快速和稳定,可用于伊托必利血药浓度检测和药动学研究。更多还原

【Abstract】 Objective:To develop a new sensitive LC-MS/MS method for the determination of itopride in human plasma.Methods:Sulpiride was selected as the internal standard,and the separation was performed on a Phenomenex Luna C18(150mm×2.0mm,5μm)column using acetonitrile-water(0.1% formic acid+10mmol ammonium formate)(60∶40) at a flow rate of 0.2mL·min-1 as the mobile phase.The column temperature was 40℃.ESI+ was performed in the MRM mode using target ions at m/z 359.9→71.9(itopride) and m/z 343.0→112.2(sulpiride).Results:The calibration curve was linear within the range of 0.336～688ng·mL-1(r2=0.9993).The lower limit of quantitation(LLOQ)of itopride in plasma was 0.336ng·mL-1.The extracted recovery of itopride from the plasma was more than 80%,the relative recovery was 85%～115%.The intra-and inter-day RSDs were all less than 5%.Conclusion:It can be used for the determination of itopride serum concentration and pharmacokinetic study as a sensitive,simple and accurate method.更多还原