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作 者:陈英[1] 谭志荣[1] 陈尧[1] 郭栋[1] 韩仰[1] 陈豪[1] 肖昌琼[1] 王亦男[1] 张敏[1] 许婷[1] 周宏灏[1]
出 处:《中南药学》2008年第2期168-170,共3页Central South Pharmacy
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,r^2=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。Objective To develop a liquid chromatography tandem mass spectrometric method (LC-MS-MS) for quanti fying 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× 50mm, 5μm) 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 con centration and for pharmacokinetic study since it is economic, simple, sensitive and fast.
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