超高液相色谱-质谱法检测人血浆中格列美脲和氟西汀及其代谢产物

发布时间：2018-08-07 15:30

【摘要】：目的建立一种同时检测人血浆中格列美脲、氟西汀及其代谢物羟基格列美脲、去甲氟西汀浓度的超高液相色谱-质谱的方法。方法以咪达唑仑为内标,血浆样品用乙腈沉淀后检测。用Acquity UPLC BEH C18柱为分离柱,流动相:乙腈-0.1%甲酸,梯度洗脱,流速:0.45 m L·min-1,柱温:40℃;用Acquity Xevo TQD三重四级杆质谱仪(电喷雾离子源)质谱检测,用多反应监测法测定样品中的药物浓度。考察该方法的专属性、标准曲线和定量下限、精密度和回收率、基质效应及稳定性。结果格列美脲、羟基格列美脲、氟西汀和羟基氟西汀的标准曲线分别为y=1.49×10-2x+4.23×10-2(r=0.999 7),y=0.97×10-2x-0.26×10-2(r=0.999 5),y=1.72×10-2x+9.48×10-2(r=0.999 3),y=8.66×10-2x-1.05×10-2(r=0.999 4),分别在5~1000,2.5~500,1~200,0.5~100 ng·m L-1线性关系良好。药物及其代谢物的回收率均大于90%,日内、日间精密度均小于15%。结论该方法简便、快速,可用于人血浆格列美脲、氟西汀及其代谢产物的检测、药代动力学研究和药物相互作用研究。
[Abstract]:Objective to establish a method for simultaneous determination of glimepiride fluoxetine and its metabolites hydroxy glimepiride and norfluoxetine in human plasma by ultrahigh liquid chromatography-mass spectrometry. Methods midazolam was used as internal standard and plasma samples were precipitated with acetonitrile. Acquity UPLC BEH C18 column was used as separation column, mobile phase: acetonitrile-0.1% formic acid, gradient elution, flow rate: 0.45m 路min ~ (-1), column temperature: 40 鈩，

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