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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10mmo·lL-1醋酸铵溶液(含0.2%甲酸)-甲醇(25∶75),流速为1.0 mL·m in-1;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 n·gmL-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。
Objective: To establish a method for the determination of oxymatrine and matrine in human plasma by LC-MS / MS. Methods: The plasma sample to be tested was extracted with methylene chloride and detected by LC-MS / MS. Cimetidine was used as internal standard. The mobile phase consisted of 10 mmol·L-1 ammonium acetate solution (containing 0.2% formic acid) -methanol (25:75) at a flow rate of 1.0 mL · m in-1 and the mass spectrum was determined by electrospray ionization (ESI ) Mode and multi-reactive ion monitoring (MRM) mode for positive ion detection. Results: The linear range of oxymatrine was 4.99-998.0 ng · mL-1 with the lowest concentration of 4.99 ng · mL-1. The linear range of matrine was 9.71-4.885.0 n · g mL-1. The lowest concentration of oxymatrine 9.71 ng · mL-1. Accuracy, precision (day, day), extraction recovery, matrix effect and stability (room temperature, frozen) are in line with the relevant requirements. Conclusion: The method is simple, accurate, sensitive and specific. It is suitable for the determination of oxymatrine and matrine in human plasma.