色谱

色谱 ›› 2014, Vol. 32 ›› Issue (5): 506-512.DOI: 10.3724/SP.J.1123.2013.12035

• 研究论文 • 上一篇    下一篇

超临界流体色谱对吴茱萸中吲哚类生物碱的快速分析

李振宇, 傅青, 李奎永, 梁图, 金郁   

  1. 华东理工大学药学院, 上海 200237
  • 收稿日期:2013-12-30 修回日期:2014-02-27 出版日期:2014-05-08 发布日期:2014-04-26
  • 通讯作者: 金郁
  • 基金资助:

    国家自然科学基金项目（21005028）；华东理工大学基本科研业务费探索研究基金（WY1214070）.

Fast analysis of indole alkaloids from Evodiae fructus by supercritical fluid chromatography

LI Zhenyu, FU Qing, LI Kuiyong, LIANG Tu, JIN Yu   

  1. School of Pharmacy, East China University of Science and Technology, Shanghai 200237, China
  • Received:2013-12-30 Revised:2014-02-27 Online:2014-05-08 Published:2014-04-26

PDF

303

被引次数

31

摘要：

建立了超临界流体色谱快速分析吴茱萸中吲哚类生物碱的方法。以标准品混合物和复杂样品为对象比较4种色谱柱的分离效果，进行色谱柱的筛选；考察了进样体积、改性剂、添加剂、温度和背压对保留行为的影响。结果表明，进样体积对峰形影响显著；添加剂对保留时间和色谱峰形影响有限；改变改性剂能使保留时间显著改变；降低温度，升高背压，保留时间减小。经过优化，确定采用Waters ACQUITY UPC2 BEH色谱柱，以甲醇为改性剂，在35 ℃柱温和2.07×107 Pa背压条件下，15 min内完成复杂样品的分析。同时采用超高效液相色谱完成复杂样品的快速分析。结果表明，超临界流体色谱可用于天然产物的高效快速分析，同时该方法与超高效液相色谱在分离选择上的差异有助于天然产物分析方法的拓展。

关键词: 超高效液相色谱, 超临界流体色谱, 快速分析, 吴茱萸, 吲哚类生物碱

Abstract:

A fast chromatographic separation of indole alkaloids from Evodiae fructus was developed by supercritical fluid chromatography (SFC). The initial screening of four stationary phases was investigated with a standard mixture of evodiamine and rutaecarpine, and a complex sample of indole alkaloids prepared from Evodiae fructus as probes. Later, the effects of chromatographic parameters on separation were studied including injection volume, organic modifier, additive, temperature and back pressure. The injection volume had significant impact on the peak shape. With the additives in the mobile phase, slight changes in peak shape and retention time were observed in separation. Variation in organic modifier led to dramatic change in chromatographic behavior. Both decreased temperature and increased back pressure shortened the retention time. Finally, a fast analytical method using SFC, on a Waters ACQUITY UPC2 BEH column, methanol as modifier, under 35 ℃ and 2.07×107 Pa, was developed to separate a complex sample of indole alkaloids in less than 15 min. Another rapid approach for the separation of a complex sample of indole alkaloids was developed by using ultra-high performance liquid chromatography (UHPLC). As a result, SFC can be used in the separation of natural products, giving high performance, good resolution and fast analysis speed. The difference in selectivity with UHPLC can be used to the development of natural product separation.

Key words: Evodiae fructus, fast analysis, indole alkaloids, supercritical fluid chromatography (SFC), ultra-high performance liquid chromatography (UHPLC)

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