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目的建立液相色谱-串联质谱(LC-MS/MS)快速灵敏分析血液中茶碱的定性定量方法。方法将0.1 mL血液加入0.9 mL乙腈沉淀蛋白后,直接取上清液5μL进样。LC-MS/MS采用ESI(+)模式,应用多反应监测(MRM)方法检测。结果本方法的液相分离良好,峰形优异,整个液相循环在3 min内完成。采用0.1 mL血液,茶碱和咖啡因在20~1 000μg.L-1时呈良好的线性关系,最低检测限(LOD)均为10μg.L-1。结论所建立的方法简便、快速、特异性强、灵敏度高,可同时分析茶碱的代谢物咖啡因,足以满足临床毒物分析和法庭毒物分析的需要。
Objective To establish a qualitative and quantitative method for rapid and sensitive analysis of theophylline in blood by liquid chromatography-tandem mass spectrometry (LC-MS / MS). Methods After adding 0.1 mL of blood to 0.9 mL of acetonitrile to precipitate protein, 5 μL of supernatant was directly injected into the sample. LC-MS / MS using ESI (+) mode, the application of multiple reaction monitoring (MRM) method. Results The method has good liquid phase separation and excellent peak shape. The entire liquid phase is completed within 3 min. With 0.1 mL of blood, theophylline and caffeine exhibited a good linear relationship at 20-1 000 μg.L-1 with the lowest detection limit (LOD) of 10 μg.L-1. Conclusion The established method is simple, rapid, specific and sensitive. Simultaneous analysis of caffeine, a metabolite of theophylline, is sufficient to meet the needs of clinical analysis and forensic analysis.