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目的建立高效液相质谱联用法以测定人血浆中蒿甲醚(ARM)及其活性代谢物双氢青蒿素(DHA)的浓度。方法色谱条件:色谱柱为C18(150 mm×4.6 mm,5μm),流动相为0.2%醋酸-甲醇梯度洗脱系统,流速为1.0 mL.min-1。质谱条件:大气压化学电离方法(APCI)采集正离子,SIM方式对ARM和DHA检测m/z221,对内标(青蒿素)检测m/z283。血浆样品的预处理采用甲基叔丁基醚萃取法。结果ARM和DHA的线性范围为5~300μg.L-1,相关系数r>0.999 0,检测限均为2μg.L-1。ARM和DHA日内和日间测定的RSD<9.3%,回收率在92%~105%的范围内,提取回收率为80%~96%。结论该法简便、准确、灵敏、专属,适用于ARM和DHA的人体药动学研究。
Objective To establish a method for the determination of artemisinin (ARM) and its active metabolite dihydroartemisinin (DHA) in human plasma by high performance liquid chromatography-mass spectrometry. Methods Chromatographic conditions: a C18 column (150 mm × 4.6 mm, 5 μm) with a mobile phase of 0.2% acetic acid-methanol gradient elution system at a flow rate of 1.0 mL · min-1. Mass spectrometry conditions: positive ion chemical ionization (APCI), m / z 221 for SIM and ARM, and m / z 283 for internal standard (artemisinin). Pretreatment of plasma samples using methyl tert-butyl ether extraction method. Results The linear range of ARM and DHA was 5 ~ 300μg.L-1 with correlation coefficient r> 0.999 0 and the detection limit was 2μg.L-1. The RSD of intra-day and inter-day determination of ARM and DHA was <9.3%. The recoveries ranged from 92% to 105%. The recoveries ranged from 80% to 96%. Conclusion The method is simple, accurate, sensitive and specific and suitable for human pharmacokinetic studies of ARM and DHA.