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.
出处
《中国实验方剂学杂志》
CAS
北大核心
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)
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
Xianning Linimentum
matrine
oxymatrine
ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS-MS)