色谱 ›› 2012, Vol. 30 ›› Issue (12): 1276-1281.DOI: 10.3724/SP.J.1123.2012.09044

• 研究论文 • 上一篇    下一篇

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

胡梦迪1,2, 苏迪1,2, 范晓苏1,2, 于建华2, 徐远金1,2*   

  1. 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
  • 收稿日期:2012-09-29 修回日期:2012-11-14 出版日期:2012-12-28 发布日期:2012-12-19
  • 通讯作者: 徐远金,博士,教授,研究方向为色谱-质谱分析. Tel: (0771)3237743, E-mail: yjxu@gxu.edu.cn.
  • 基金资助:

    国家自然科学基金项目(20865001)和广西自然科学基金项目(桂科自0832034).

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

HU Mengdi1,2, SU Di1,2, FAN Xiaosu1,2, YU Jianhua2, XU Yuanjin1,2*   

  1. 1. State Key Laboratory of Conservation and Utilization of Subtropical Agro-bioresources, Nanning 530004, China, 2. School of Chemistry and Chemical Engineering, Guangxi University, Nanning 530004, China
  • Received:2012-09-29 Revised:2012-11-14 Online:2012-12-28 Published:2012-12-19

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×50 μm)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。

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

Abstract: 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.

Key words: alkaloids, electrospray ionization-mass spectrometry (ESI-MS), laurel acyl malic acid ester, Niuhuang Shangqing Tablets, micellar electrokinetic chromatography (MEKC)