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目的建立液相色谱-串联质谱(LC-MS/MS)法测定人血浆样本中莫沙必利的浓度。方法血浆样本经固相小柱萃取处理后,以甲醇-0.5%甲酸溶液(70:30)为流动相,采用Agilent TC-C18(4.6 mm×150mm,5μm)色谱柱进行分离,流速为0.5 m L·min-1,柱温25℃;采用ESI正离子模式检测,离子监测方式为MRM,用于定量分析的离子反应分别为m/z 422.1→m/z 198(莫沙必利)和m/z 466.1→m/z 184(西沙必利)。结果莫沙必利在0.512~125μg·L-1与峰面积线性关系良好(r2=0.999 3),定量下限为0.512μg·L-1,日内及日间RSD均<10%,莫沙必利的提取回收率和基质效应分别在95.8%~101.6%和101.6%~113.0%。结论本方法特异性强,灵敏度高,测定结果可靠,样本检测时间为3 min,适用于血浆样本中莫沙必利的浓度测定及其药物代谢动力学研究。
Objective To establish a liquid chromatography-tandem mass spectrometry (LC-MS / MS) method for the determination of mosapride in human plasma samples. Methods The plasma samples were separated on a solid phase cartridge and separated on a TC-C18 (4.6 mm × 150 mm, 5 μm) column using methanol-0.5% formic acid (70:30) as the mobile phase at a flow rate of 0.5 m L · min-1 and column temperature of 25 ℃. The ion detection mode was MRM with ESI positive ion mode. The ion reactions for quantitative analysis were m / z 422.1 → m / z 198 (mosapride) and m / z 466.1 → m / z 184 (cisapride). Results Mosapride had a good linear relationship (r2 = 0.999 3) with a peak area of 0.512-125 μg · L-1 and a lower limit of quantitation of 0.512 μg · L-1 with RSD <10% The recoveries and matrix effects were 95.8% ~ 101.6% and 101.6% ~ 113.0%, respectively. Conclusion The method is specific, sensitive and reliable. The detection time is 3 min, which is suitable for the determination of mosapride and its pharmacokinetics in plasma samples.