UPLC-MS-MS测定廯宁搽剂中苦参碱与氧化苦参碱  

Simultaneous Determination of Matrine and Oxymatrine in Xianning Linimentum by UPLC-MS-MS

作　　者：朱平川[1] 岑卫健[1] 范晓苏[2] 莫祺红[3] 

机构地区：[1]亚热带农业生物资源保护与利用国家重点实验室,广西大学,南宁530004 [2]广西大学化学化工学院,南宁530004 [3]广西大学生命科学与技术学院,南宁530004

出　　处：《中国实验方剂学杂志》2014年第6期51-54,共4页Chinese Journal of Experimental Traditional Medical Formulae

基　　金：广西自然科学基金项目(桂科自0832034)

摘　　要：目的：建立同时测定廯宁搽剂中的苦参碱与氧化苦参碱2种有效成分含量的超高效液相色谱-串联质谱（UPLC-MS-MS）分析方法.方法：采用C18（2.1 mm × 50 mm,1.8 μm）色谱柱,以甲醇-0.1％甲酸的水溶液为流动相,流速0.30 mL·min-1.在电喷雾电离（ESI）正离子模式下,采用多重反应监测模式（MRM）进行检测.结果：苦参碱与氧化苦参碱的线性范围分别为0.000 5 ～0.6,0.000 4 ～0.5 mg·L-1;检出限分别为0.2,0.2 μg·L-1;2种成分的加样回收率为95.8％ ～ 98.6％,RSD均＜1.9％.结论：该方法简便、准确、快速、高灵敏度,已成功地用于实际的样品分析.Objective：A method for simultaneous determination of matrine and oxymatrine in Xianning Linimentum was established by ultra performance liquid chromatography with tandem mass spectrometry （UPLC-MS-MS）.Method：The UPLC separation was performed on C18 column （2.1 mm ×50 mm,1.8 μm） by using methanol and water containing 0.1％ formic acid as mobile phase with the gradient elution at a rate of 0.30 mL · min-1 The analytes were detected by tandem mass spectrometry under the positive ion mode with the ESI source and carried out in the multiple reaction monitoring （MRM） mode.Result：Under the optimum conditions,the calibration curves were linear in the range of 0.000 5-0.6 mg · L-1 for matrine,0.000 4-0.5 mg · L-1 for oxymatrine.The detection limits were 0.2,0.2 μg ·L-1 respectively.The average recoveries of the three effective components were between 95.8％ and 98.6％ with all relative standard deviations not more than 1.9％.Conculsion：The developed method is simple,rapid and accurate,and suitable for the quality control of the two components in Xianning Linimentum.

关 键 词：廯宁搽剂 苦参碱 氧化苦参碱 超高效液相色谱-串联质谱 

分 类 号：R284.1[医药卫生—中药学]