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目的:建立高效液相色谱-质谱联用法测定人血浆中佐米曲普坦浓度。方法:选用Zorbax Extend-C18色谱柱(5μm,150mm×4.6mm),以甲醇-水-甲酸(80∶20∶1,v/v/v)为流动相,采用等度洗脱进行分离,样品用液-液萃取法处理后进样,流速:0.8mL·min-1,柱温:室温,进样量:20μL。选用API4000型三重四极杆串联质谱仪的多重反应监测(MRM)扫描方式进行检测。结果:佐米曲普坦的线性范围为0.10～40.0ng·mL-1,定量下限为0.10ng·mL-1。准确度与精密度结果显示方法日间、日内变异均小于15%,相对偏差-2.5%～3.3%,方法提取回收率大于45%,稳定性较好。结论:本研究所建立的方法快速、灵敏,专属性强、重现性好,可用于人体血浆中佐米曲普坦浓度的测定和药动学研究。
Objective: To establish a method for the determination of zolmitriptan in human plasma by high performance liquid chromatography-mass spectrometry. METHODS: Zorbax Extend-C18 column (5μm, 150mm × 4.6mm) was used to separate the sample with isocratic elution using methanol-water-formic acid (80:20:1, v / v / v) The sample was treated with liquid-liquid extraction, the flow rate was 0.8 mL · min-1, the column temperature was room temperature, the injection volume was 20 μL. The API4000 triple quadrupole mass spectrometer was used for multiple reaction monitoring (MRM) scanning. Results: The linear range of zolmitriptan was 0.10-40.0 ng · mL-1 and the lower limit of quantification was 0.10 ng · mL-1. The accuracy and precision of the method showed that the variation of the method was less than 15% and the relative deviation was -2.5% ~ 3.3% during the day and the day. The recovery rate was more than 45% and the stability was better. Conclusion: The method established in this study is rapid, sensitive, specific and reproducible. It can be used for the determination of zolmitriptan in human plasma and pharmacokinetic study.