【摘要】 建立测定人血浆中莫沙必利的高效液相色谱-质谱/质谱联用法。取血浆样品经液-液萃取后,以乙腈为有机相,0.3%甲酸水溶液为水相,采用梯度洗脱的方式,用C18柱分离,通过电喷雾离子化,以多反应监测(MRM)方式进行正离子检测。莫沙必利线性范围为0.17~68.00 ng.mL-1,定量下限为0.17 ng.mL-1,每个样品测试时间仅2.8 min,日内、日间精密度(RSD)均小于13%,准确度(RE)在±6.3%范围内。应用此法研究了20名志愿者单剂量口服枸橼酸莫沙必利片后的药代动力学特点。该方法、灵敏、准确、快速,适用于莫沙必利的药代动力学及生物等效性研究。更多还原

【Abstract】 To develop a sensitive and specific high performance liquid chromatography-tandem mass spectrometric（HPLC-MS/MS） method for the determination of mosapride in human plasma,mosapride and internal standard tamsulosin were extracted from plasma with liquid-liquid extraction,then separated on a Waters ACQUITY UPLC^TM BEH C₁₈ column（50 mm×2.1 mm,1.7 μm ID） with gradient elution at flow-rate of 0.25(mL·min^-1).The mobile phase was water（containing 0.3% formic acid） and acetonitrile under gradient conditions.Electrospray ionization（ESI） source was applied and operated in the positive ion mode.Multiple reaction monitoring（MRM） mode with the transitions of m/z 422 → m/z 198 and m/z 409 → m/z 228 were used to quantify mosapride and the internal standard,respectively.The linear calibration curve was obtained in the concentration range of 0.17-68.00 ng·mL^-1.The lower limit of quantification was 0.17 ng·mL^-1.The interand intra-day precision（RSD） was less than 13%,and the accuracy（RE） was within ±6.3% calculated from QC samples.The method was used to determine the concentration of mosapride in plasma after a single oral dose of 5 mg mosapride citrate to 20 healthy male Chinese volunteers.The method has been proved to be selective,sensitive,rapid and suitable for pharmacokinetic study of mosapride.更多还原