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目的建立LC-MS/MS法测定人血浆中氯沙坦及其代谢物E-3174血药浓度的方法。方法血浆酸化后用乙醚提取,采用同位素内标(氘3-E-3174)进行测定。色谱柱:CAPCELL PACK C_(18)Ⅲ(100mm×2.0mm,5μm),流动相:0.02%甲酸乙腈-水溶液(53:47,V/V);等度洗脱;流速0.3mL·min~(-1);进样体积5μL;电喷雾离子化,正离子MRM扫描。结果氯沙坦和E-3174线性范围均为5~500μg·L~(-1)(r>0.999),最低定量限均为5μg·L~(-1),平均提取回收率均>50%,批内、批间精密度RSD均<8%。结论本方法灵敏度高、专一性好、操作简单,适用于氯沙坦的药动学研究。
Objective To establish a method for the determination of losartan and its metabolite E-3174 in human plasma by LC-MS / MS. Methods The plasma was acidified and extracted with ether. The isotope internal standard (deuterium 3-E-3174) was used for the determination. The mobile phase consisted of 0.02% formic acid in acetonitrile-water (53:47, V / V); isocratic elution; flow rate was 0.3 mL · min ~ (-1) -1); injection volume 5μL; electrospray ionization, positive ion MRM scan. Results The linear ranges of losartan and E-3174 ranged from 5 to 500 μg · L -1 (r> 0.999), with the lowest limits of quantitation (5 μg · L -1) and the average recovery of> 50% , Intra-batch and inter-batch precision RSD <8%. Conclusion The method is sensitive, specific and easy to operate and is suitable for the pharmacokinetic studies of losartan.