色谱

色谱 ›› 2014, Vol. 32 ›› Issue (5): 447-451.DOI: 10.3724/SP.J.1123.2013.12040

• 研究论文 • 上一篇    下一篇

混合模式毛细管聚合物整体柱的制备及应用

窦阿波1, 邹存杰2, 单圆鸿1, 石先哲1, 许国旺1   

  1. 1. 中国科学院大连化学物理研究所, 中国科学院分离分析化学重点实验室, 辽宁 大连 116023;
    2. 辽宁对外经贸学院, 辽宁 大连 116052
  • 收稿日期:2013-12-31 修回日期:2014-03-27 出版日期:2014-05-08 发布日期:2014-04-26
  • 通讯作者: 石先哲
  • 基金资助:

    国家自然科学基金项目（21275141）.

Preparation and application of mixed-mode capillary polymer monolithic column

DOU Abo1, ZOU Cunjie2, SHAN Yuanhong1, SHI Xianzhe1, XU Guowang1   

  1. 1. Dalian Institute of Chemical Physics, Key Laboratory of Separation Science for Analytical Chemistry, Chinese Academy of Sciences, Dalian 116023, China;
    2. Liaoning University of International Business and Economics, Dalian 116052, China
  • Received:2013-12-31 Revised:2014-03-27 Online:2014-05-08 Published:2014-04-26

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摘要：

混合模式毛细管整体色谱柱由于保留机理多样，具有很好的应用前景。本文以[2-（甲基丙烯酰基氧基）乙基]二甲基-（3-磺酸丙基）氢氧化铵（SPE）为单体，乙二醇二甲基丙烯酸酯（EDMA）为交联剂，偶氮二异丁腈（AIBN）为引发剂，正丙醇/1，4-丁二醇/水三元体系为致孔剂，制备了聚合物基质SPE-co-EDMA毛细管液相色谱整体柱。通过系统优化致孔剂和反应物种类和配比、引发剂的用量、反应时间和反应温度等因素，提高了整体柱的柱效、机械强度、渗透性和重复性。结果表明该毛细管整体柱在10 MPa内具有良好的机械强度，渗透性为2.17×10-14 m2，而且批次内和批次间峰面积的重现性（RSD）分别为1.0%和4.6%。以极性和非极性的多种化合物评价了该毛细管整体柱的色谱性能，结果表明该柱在高有机相中具有亲水相互作用机理，在低有机相中具有反相作用机理，显示出混合模式分离特性。

关键词: 混合模式, 毛细管高效液相色谱, 毛细管整体柱, 制备

Abstract:

Based on the diversity of the retention mechanism, mixed-mode capillary monolithic columns have broad application prospect. In this work, a novel capillary polymer monolithic column was prepared with [2-(methacryloyloxy)ethyl]dimethyl-(3-sulfopropyl)ammonium hydroxide (SPE) as monomer, ethylene dimethacrylate (EDMA) as crosslinking agent, azobisisobutyronitrile (AIBN) as initiator and butylalcohol/1,4-butanediol/water as ternary porogens. Under the optimized reaction conditions including the proportion of monomer and porogens, amount of initiator, reaction temperature and polymerization time, the monolithic column showed good mechanical strength up to 10 MPa, high permeability of 2.17×10-14 m2 and good repeatability. The peak area RSDs of column-to-column and batch-to-batch reproducibility were 1.0% and 4.6%, respectively. Finally, the capillary monolithic column was evaluated with polar and non-polar test mixtures. It showed hydrophilic interaction under high organic phase while hydrophobic interaction under low organic phase, indicating it a mixed-mode monolithic column.

Key words: capillary high performance liquid chromatography, capillary monolithic column, mixed-mode, preparation

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