【摘要】 目的建立液-质联用法测定人血浆中奥美沙坦的浓度。方法用替米沙坦作内标,采用乙腈直接沉淀血浆样品,LC-MS-MS进行分析。色谱柱为Waters Xterra MS C18(2.1mm×50mm,5μm),柱温为40℃,流动相为乙腈-0.1%甲酸(50∶50,v/v),流速为0.3mL.min-1,进样量为10μL。ESI正离子方式进行扫描,MRM方式检测,用于定量分析的检测离子为m/z:448.27→429.7(奥美沙坦)和m/z:516.43→497.8,276.5(替米沙坦)。结果本方法线性范围是1.16~2280ng.mL-1,权重为1/w,r2=0.999,最小检出浓度(LLOQ)为1.16ng.mL-1。绝对回收率均在80%以上,相对回收率为85%~115%,日内、日间RSD均<15%。结论本方法经济、简单、灵敏、快速,可用于奥美沙坦血药浓度检测和药物动力学研究。更多还原

【Abstract】 Objective To develop a liquid chromatography-tandem mass spectrometric method(LC-MS-MS)for quantifying the concentration of olmesartan in the human plasma.Methods Telmisartan was added as the internal standard.The plasma sample was extracted using acetonitrile and then separated on a Waters Xterra MS C18(2.1 mm×50 mm,5 μm)column and the column temperature was 40 ℃.The mobile phase consisted of acetonitrile-0.1% formic acid water solution(50∶50,v/v),and the flow rate was 0.3 mL·min-1.The ionization was optimized using ESI+,and enhanced selectivity was achieved using tandem mass spectrometric analysis via MRM functions.The ion of m/z:448.3→429.7 and m/z:516.4→497.8,276.5 was used to qualify olmesartan and telmisartan,respectively.Results The concentration range of olmesartan was 1.16~2 280 ng·mL-1,with a good linearity.The LLOQ of olmesartan in the plasma was 1.16 ng·mL-1.The extracted recovery was >80%,and the relative recovery was 85%~115 %.The intra-and inter-day RSD was <15%.Conclusion It can be used for the determination of olmesartan plasma concentration and for pharmacokinetic study since it is economic,simple,sensitive and fast.更多还原