色谱

色谱 ›› 2017, Vol. 35 ›› Issue (4): 382-387.DOI: 10.3724/SP.J.1123.2016.09035

• 研究论文 • 上一篇    下一篇

磺酸甜菜碱型两性离子亲水作用色谱固定相的制备及色谱性能评价

李文婧1, 赵丽娟1, 魏缠玲1, 戴小军1, 龚波林1,2   

  1. 1. 宁夏大学化学化工学院, 宁夏 银川 750021;
    2. 北方民族大学化学与化学工程学院, 宁夏 银川 750021
  • 收稿日期:2016-09-17 出版日期:2017-04-08 发布日期:2013-07-30
  • 通讯作者: 戴小军,E-mail:xjdai@nxu.edu.cn;龚波林,E-mail:gongbl@nxu.edu.cn.
  • 基金资助:

    国家自然科学基金（31360077，31271868）；宁夏自然科学基金（NZ13045）.

Preparation and evaluation of chromatographic properties of sulfobetaine zwitterionic hydrophilic interaction chromatography stationary phase

LI Wenjing1, ZHAO Lijuan1, WEI Chanling1, DAI Xiaojun1, GONG Bolin1,2   

  1. 1. School of Chemistry & Chemical Engineering, Ningxia University, Yinchuan 750021, China;
    2. School of Chemistry & Chemical Engineering, Beifang University of Nationalities, Yinchuan 750021, China
  • Received:2016-09-17 Online:2017-04-08 Published:2013-07-30
  • Supported by:

    National Natural Science Foundation of China (Nos. 31360077, 31271868); Natural Science Foundation of Ningxia (No. NZ13045).

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摘要：

以丙烯酸二甲氨基乙酯（DMAEA）和1，3-丙磺酸内酯为原料，合成了含磺酸甜菜碱型两性离子的N，N-二甲基-N-丙烯酰氧乙基-N-丙基磺酸铵（DMAEAPS）功能单体，通过原子转移自由基聚合（ATRP）技术将其接枝到硅胶表面，制备了磺酸甜菜碱型两性离子色谱固定相（Sil-DMAEAPS）。研究了该固定相对安息香、维生素B6、芸香叶苷、对香豆酸和咖啡酸5种极性溶质的亲水作用色谱分离性能。结果表明，在典型的亲水作用色谱条件下，极性溶质的保留主要由静电作用和亲水作用控制；而在典型的反相色谱条件下，极性溶质则表现出反相柱的分离特征。与ZIC®-HILIC商品柱进行对比，自制色谱柱对5种极性溶质表现出不同的分离选择性。将自制色谱柱用于芦丁片中芸香叶苷含量的测定，操作方法简单，为极性样品的分离提供了新方法。

关键词: 磺酸甜菜碱, 两性离子固定相, 亲水作用色谱, 色谱性能, 原子转移自由基聚合

Abstract:

A zwitterionic sulfobetaine functional monomer N,N-dimethyl-N-acryloyloxyethyl-N-ammonium propane sulfonate (DMAEAPS) was synthesized. Dimethyl amino ethyl acrylate (DMAEA) and 1,3-propyl sulfonic acid ester as raw materials were used to synthesize the functional monomer. The DMAEAPS functional monomer was characterized by 1H-NMR and FT-IR. 2-Bromoisobutyryl bromide allyl silicone (Sil-Br) was used as the initiator, CuBr and 2,2-bipyridyl (Bpy) as the catalytic system, and the functional monomer DMAEAPS was grafted on the surface of Sil-Br by atom transfer radical polymerization (ATRP). Then the sulfobetaine zwitterionic stationary phase (Sil-DMAEAPS) was obtained. The Sil-DMAEAPS stationary phase was characterized by element analysis. Chromatographic evaluation in hydrophilic interaction chromatography (HILIC) mode showed that the materials were suitable for use as stationary phase, and the column showed a dual retention mechanism, HILIC mode in acetonitrile-rich mobile phases and RP mode in highly aqueous mobile phases. The separation selectivity and retention of the five polar solutes (benzoin, pyridoxine, rutin hydrate, p-coumaric acid and caffeic acid) on the Sil-DMAEAPS stationary phase were different from the commercially available ZIC®-HILIC. A method for the determination of rutin hydrate in rutin tablets was established. It is simple and accurate for the determination of polar compounds.

Key words: atom transfer radical polymerization (ATRP), chromatographic properties, hydrophilic interaction chromatography (HILIC), sulfobetaine, zwitterionic stationary phase

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