Objective; To establish a liquid chromatography tandem mass spectrometry (LC-MS/MS) method for the determination of oxymatrine and matrine in human plasma. Methods; The analyses and an inter- nal standard (cimetidine) were extracted from plasma with dichloromethane. The compounds were separated on a ZORBAX-NH2 column by applying LC-MS/MS; 10 mmol·L-1 ammonium acetate (0. 2% formic acid)-methanol (25:75) was used as mobile phase at a flow rate of 1. 0 mL · min -1. The detection was carried out by means of electrospray ionization tandem mass spectrometry in positive ion mode and multiple reaction monitoring ( MRM) mode. Results; The assay had the calibration range from 4. 99 to 998.0 ng·mL-1 and lower limit of quantification (LOQ) was 4.99 ng·mL-1 for oxymatrine. The calibration range from 9. 71 to 4 855. 0 ng·mL-1 and LOQ was 9. 71 ng·mL-1 for matrine. The accuracy, precision (intra-day and inter-day) , extraction recovery, matrix effects and stability ( ambient temperature, freeze storage) of the method fulfilled the analytical validation criteria of the guidelines. Conclusion: The method is simple, accurate, sensitive and specific for the determination of oxymatrine and its metabolite matrine in human plasma.%目的:建立LC-MS/MS法测定人血浆中氧化苦参碱和苦参碱浓度的方法.方法:待测血浆样品经二氯甲烷萃取后,用LC-MS/MS法进行检测,以西咪替丁为内标.色谱柱为ZORBAX-NH2,流动相为10mmol· L-1醋酸铵溶液(含0.2%甲酸)-甲醇(25:75),流速为1.0 mL·min -；质谱采用电喷雾离子化(ESI)方式和多反应离子监测(MRM)模式进行正离子检测.结果:本方法氧化苦参碱的线性范围为4.99～998.0ng·mL-1,最低定量浓度4.99 ng· mL-1；苦参碱线性范围为9.71 ～4 855.0 ng·mL-1,最低定量浓度9.71ng· mL-1.准确度、精密度(日内、日间)、提取回收率、基质效应以及稳定性(室温、冻存)均符合有关要求.结论:该方法简便、准确,灵敏度高,专属性强,适用于人血浆中氧化苦参碱和苦参碱浓度的测定.
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