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目的:建立快速、灵敏的液相色谱-电喷雾离子阱质谱法测定人血浆中曲马多和对乙酰氨基酚的浓度。方法:血浆样品经乙腈直接沉淀蛋白后,以乙腈-10 mmoL·L-1甲酸胺-0.1%甲酸(65:15:20)为流动相,采用Hypurity C18柱(150mm× 2·1 mm,5μm)分离,流速为0.2 mL·min-1,通过电喷雾离子化离子阱质谱,以二级质谱选择离子反应监测(SRM)方式进行检测。结果:曲马多和乙酰氨基酚的线性范围分别为5～1000及20-12800 ng·mL-1,最低检测浓度分别为1和10 ng· mL-1,平均相对回收率均为103.7%,日内和日间变异均<20%,每个样品测试时间仅为7.0 min。结论:本法简单、快速、灵敏、重现性好,是一种有效的检测人血浆中曲马多和对乙酰氨基酚浓度的方法。
OBJECTIVE: To establish a rapid and sensitive liquid chromatography-electrospray ion trap mass spectrometry for the determination of tramadol and acetaminophen in human plasma. METHODS: The plasma samples were directly precipitated with acetonitrile and eluted with acetonitrile-10 mmoL·L-1 formamide-0.1% formic acid (65:15:20) as mobile phase and Hypurity C18 column (150 mm × 2 · 1 mm, ) At a flow rate of 0.2 mL · min-1. Electrospray ionization mass spectrometry (ESI-MS / MS) was used to detect the samples by secondary ion-exchange mass spectrometry (SRM). RESULTS: The linear range of tramadol and acetaminophen was 5-1000 and 20-12800 ng · mL-1, respectively. The minimum detectable concentrations were 1 and 10 ng · mL-1, respectively, and the average relative recoveries were 103.7% Intra- and inter-day variation was <20%, with a test time of only 7.0 min for each sample. Conclusion: The method is simple, rapid, sensitive and reproducible. It is an effective method to detect the concentration of tramadol and paracetamol in human plasma.