HPLC-MS/MS法测定人血浆中美普他酚的浓度

摘要

目的:建立人血浆中美普他酚浓度的HPLC-MS/MS测定法.方法:血浆样品500 μL经液-液萃取后,以10 mmol·L-1醋酸铵(含0.5％甲酸水溶液)-乙腈(70:30)为流动相,采用Inertsil(R) CN( 150 mm×4.6mm,3.5 μm)柱分离,采用电喷雾电离化(ESI)方式和多反应离子监测(MRM)模式进行正离子检测.用于定量分析的离子反应分别为m/z 234.2→107.0(美普他酚)和m/z 152.0→110.0(对乙酰氨基酚).结果:美普他酚血药浓度线性范围为0.20～508.00 μg·L-1,定量下限为0.20 μg·L-1.低、中、高3个浓度提取回收率分别为68.1％,67.0％,65.6％.结论:该法操作简便、快速、灵敏,适用于美普他酚的药代动力学研究及制剂的生物等效性评价.%Objective: To develop a high-performance liquid chromatography coupled to tandem mass spec-trometry (HPLC-MS/MS) method for quantification of meptazinol in human plasma. Methods: After a simple liquid-liquid extraction, meptazinol and the internal standard paracetamol were separated on a Inertsil CN (150 mm ×4.6 mm, 3.5 μm) column and detected by tandem mass spectrometry. The mobile phase consisted of l0mmol·L-1 ammonium acetate (including 0. 5% formic acid water)-acetonitrile (70:30). A mass spectrometer equipped with electrospray ionization source was used as detector operated in the positive ion mode. Multiple reaction monitoring ( MRM) mode was used with the trasitions of m/z 234. 2→107. 0 for meptazinol and m/z 152. 0→ 110.0 for the internal standard, respectively. Results: The linear calibration curve was obtained in the concentration range of 0. 20 - 508. 00 μg ·L-1 . The limit of quantification was 0. 20 μg · L-1 . The extraction recoveries of the three concentrations were 68. 1% , 67. 0% and 65. 6% , respectively. Conclusion: This method is proved to be suitable for the clinical investigation of meptazinol pharmacokinetics, which offers the advantages of specificity, speed and greater sensitivity compared with the reported methods.