月桂酰基苹果酸酯胶束电动色谱-质谱法同时测定牛黄上清片中5种生物碱  

Simultaneous determination of five alkaloids in Niuhuang Shangqing Tablets by micellar electrokinetic chromatography-mass spectrometry using laurel acyl malic acid ester

作　　者：胡梦迪[1,2] 苏迪[1,2] 范晓苏[1,2] 于建华[2] 徐远金[1,2] 

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,广西南宁530004 [2]广西大学化学化工学院,广西南宁530004

出　　处：《色谱》2012年第12期1276-1281,共6页Chinese Journal of Chromatography

基　　金：国家自然科学基金项目(20865001);广西自然科学基金项目(桂科自0832034)

摘　　要：建立了基于月桂酰基苹果酸酯的胶束电动色谱-质谱法同时分离测定牛黄上清片中黄连碱、小檗碱、药根碱、黄柏碱以及川芎嗪5种有效成分含量的新方法。以7.5 mmol/L月桂酰基苹果酸酯-15 mmol/L氨水-50 mmol/L醋酸铵(含12.5%的乙腈,pH=7.0)为电泳介质,未涂层弹性石英毛细管(88 cm×50μm)为分离通道,50%异丙醇水溶液(含3 mmol/L乙酸)为鞘液,在25 kV的运行电压下,各组分可以在18 min内得到基线分离。各组分的浓度与其峰面积呈现良好的线性关系,迁移时间和峰面积的相对标准偏差均小于5%,样品中5种生物碱成分的样品加标回收率在96.0%～105%之间。该法简便、快速、准确、重现性好,可用于牛黄上清片中这5种有效成分含量的同时测定。A micellar electrokinetic chromatography-mass spectrometric method based on laurel acyl malic acid ester（LMAE） for the separation and determination of coptisine,berberine,jatrorrhizine,phellodendrine and ligustrazine in Niuhuang Shangqing Tablets was established.The baseline separation of the five compounds was attained within 18 min by an uncoated capillary（88 cm×50 μm） on the operating voltage of 25 kV using 7.5 mmol/L LMAE-15 mmol/L ammonia-50 mmol/L ammonium acetate mixture（pH=7.0） containing 12.5%（v/v） acetonitrile as the electrophoretic medium and 50% 2-propanol aqueous solution（containing 3 mmol/L acetic acid） as the sheath liquid.The peak area of each component to its concentration showed a good linear relationship.The relative standard deviations of migration times and peak areas of the five components were less than 5% and the recoveries were between 96.0% and 105%.The developed method is simple,rapid,accurate and is suitable for the routine analysis of the five alkaloid components in Niuhuang Shangqing Tablets.

关 键 词：胶束电动色谱 电喷雾离子化质谱法 月桂酰基苹果酸酯 生物碱 牛黄上清片 

分 类 号：O658[理学—分析化学]