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目的:建立高效液相色谱-质谱联用法同时测定人血浆中兰索拉唑及其代谢产物浓度。方法:以奥美拉唑为内标,血浆样品经乙腈沉淀后,经HPLC-MS-MS分离-分析。采用Diamonsil C18柱(150mm×2.1mm,5μm),以甲醇-水(含0.01%甲酸)(43.3:56.7)为流动相;流速为0.3mL·min-1,采用电喷雾离子源(ESI),以多离子反应监测方式(MRM)进行负离子监测,兰索拉唑、5-羟基兰索拉唑、兰索拉唑砜和内标奥美拉唑的定量分析离子对分别为m/z368.0→163.9,384.1→178.8,384.1/115.9和326.2→280.1。结果:兰索拉唑、5-羟基兰索拉唑、兰索拉唑砜的线性范围分别为11.4～4 560,1.26～504,1.24～496μg.L-1,r>0.99。定量下限分别为11.4,1.26,1.24μg.L-1,方法回收率在85%～115%之间。日内和日间RSD小于10%。结论:本方法灵敏、准确、可靠,适用于兰索拉唑及其代谢产物的人体药动学研究。
Objective: To establish a simultaneous determination of lansoprazole and its metabolites in human plasma by high performance liquid chromatography-mass spectrometry. Methods: With omeprazole as an internal standard, plasma samples were separated by acetonitrile-acetonitrile and analyzed by HPLC-MS-MS. A Diamonsil C18 column (150 mm × 2.1 mm, 5 μm) was used with mobile phase consisting of methanol and water (containing 0.01% formic acid) (43.3: 56.7) as the mobile phase at a flow rate of 0.3 mL · min -1 using electrospray ionization (ESI) Negative ion monitoring was performed in the multi-ion reaction monitoring (MRM) mode. Quantitative ion-pair analysis of lansoprazole, 5-hydroxy-lansoprazole, lansoprazole sulfone and the internal standard omeprazole were m / z 368.0 → 163.9, 384.1 → 178.8, 384.1 / 115.9 and 326.2 → 280.1. Results: The linear ranges of lansoprazole, 5-hydroxy-lansoprazole and lansoprazole-sulfone were 11.4-4 560,1.26-504,1.24-496μg.L-1 respectively, with r> 0.99. The lower limit of quantification was 11.4, 1.26 and 1.24 μg.L-1, respectively. The recovery rate was between 85% and 115%. The RSD is less than 10% during and after the day. Conclusion: The method is sensitive, accurate and reliable and suitable for the study of human pharmacokinetics of lansoprazole and its metabolites.