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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青蒿素和磷酸萘酚喹的浓度。方法:选用Zorbax extend-C18色谱柱,以甲醇-10mmol·L-1乙酸铵为流动相,样品用液-液萃取法处理后进样,选用Q-TrapTM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:青蒿素和磷酸萘酚喹的线性范围分别为4.00~1000ng·mL-1和0.500~500ng·mL-1,最低定量限分别为4.00ng·mL-1和0.500ng·mL-1,精密度在92.3%~106.5%之间,日间和日内相对标准差均低于10.6%,相对偏差-4.6%~8.7%,方法提取回收率均大于75%,稳定性较好。结论:本研究所建立的方法快速、灵敏、专属性强、重现性高,可用于复方磷酸萘酚喹片药动学研究。
Objective: To establish a method for the determination of artemisinin and naphthoquine phosphate in human plasma by high performance liquid chromatography-mass spectrometry. Methods: Zorbax extend-C18 column was used with methanol-10 mmol·L-1 ammonium acetate as the mobile phase. The sample was injected by liquid-liquid extraction method and then selected by Q-TrapTM triple quadrupole tandem mass spectrometer Response monitoring (MRM) scan detection. RESULTS: The linear ranges of artemisinin and naphthoquine were 4.00-1000 ng · mL-1 and 0.500-500 ng · mL-1, respectively. The minimum limit of quantification was 4.00 ng · mL-1 and 0.500 ng · mL-1, respectively. The precision was between 92.3% and 106.5%. The relative standard deviations were lower than 10.6% and the relative deviation was between 4.6% and 8.7% during the day and the day. The recoveries were all above 75% with good stability. Conclusion: The method established in this study is rapid, sensitive, specific and reproducible. It can be used to study the pharmacokinetics of compound naphthoflurane.