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目的:建立测定人血浆中坎地沙坦的液相色谱-质谱联用法。方法:血浆样品经液-液萃取后,以甲醇-水-异丙醇(55∶30∶15)为流动相,采用Inertsil ODS-3柱(150mm×2.1mm,5μm),通过电喷雾离子化离子阱时间串联质谱,以选择离子反应监测(SRM)方式进行检测。用于定量分析的二级碎片离子分别为m/z423(坎地沙坦)和m/z418(内标缬沙坦)。结果:线性范围为1.024～307.2ng·mL-1,最低定量浓度为1.024ng·mL-1,每个样品测试时间仅4.8min。在坎地沙坦酯片临床药物动力学研究项目中,应用此法可在1周内测试600个血浆样品。结论:该法灵敏度高,操作简便、快速、准确,适用于临床药物动力学研究。
Objective: To establish a liquid chromatography-mass spectrometry method for the determination of candesartan in human plasma. METHODS: The plasma samples were separated by electrospray ionization (IEM) on a Inertsil ODS-3 column (150 mm × 2.1 mm, 5 μm) using liquid-liquid extraction followed by methanol- water- isopropanol (55:30:15) Ion trap time-of-flight mass spectrometry was performed using a selective ion reaction monitoring (SRM) approach. Secondary fragment ions for quantitative analysis were m / z 423 (candesartan) and m / z 418 (internal standard valsartan), respectively. Results: The linear range was 1.024 ~ 307.2ng · mL-1, the lowest concentration was 1.024ng · mL-1, and the test time of each sample was only 4.8min. In the Candesartan Ester Clinical Pharmacokinetics Study, 600 plasma samples can be tested within 1 week using this method. Conclusion: The method is sensitive, simple, rapid, accurate and suitable for clinical pharmacokinetic studies.