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目的:建立一种快速、灵敏地测定人血浆中缬沙坦浓度的高效液相色谱串联质谱法(HPLC-MS/MS)。方法:血浆样品经乙腈沉淀后,以甲醇-乙腈-10mmol.L-1醋酸胺(pH4.0,20:30:50)为流动相,采用Lichrospher C18柱(150mm×2.1mm,5μm,汉邦科技有限公司),通过电喷雾离子化离子阱时间串联质谱,以选择多重反应监测(MRM)方式进行检测。用于定量分析的二级碎片离子分别为m/z418(缬沙坦)和m/z423(内标坎地沙坦)。结果:线性范围为4～4000μg.L-1,最低定量浓度为4μg.L-1,日内RSD为1.9%～4.2%,日间RSD为5.6%～5.9%,每个样品测试时间仅3min。结论:该法灵敏度高,操作简便、快速、准确,适用于临床药动学研究。
OBJECTIVE: To establish a rapid and sensitive HPLC-MS / MS method for the determination of valsartan in human plasma. Methods: After the plasma samples were precipitated by acetonitrile, the mobile phase consisted of methanol-acetonitrile-10mmol.L-1 acetate (pH 4.0, 20:30:50) and Lichrospher C18 (150mm × 2.1mm, Technology Co., Ltd.), by electrospray ionization ion trap time-of-flight mass spectrometry, to select multiple reaction monitoring (MRM) way to detect. Secondary fragment ions for quantitative analysis were m / z 418 (valsartan) and m / z 423 (candesartan internal standard) respectively. Results: The linear range was 4 ~ 4000μg.L-1, the lowest concentration was 4μg.L-1, the intraday RSD was 1.9% -4.2%, and the intraday RSD was 5.6% -5.9%. The test time was only 3min per sample. Conclusion: The method is sensitive, simple, rapid, accurate and suitable for clinical pharmacokinetic studies.