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  

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

作　　者：李文婧[1] 赵丽娟[1] 魏缠玲 戴小军[1] 龚波林[1,2] 

机构地区：[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

出　　处：《色谱》2017年第4期382-387,共6页Chinese Journal of Chromatography

基　　金：国家自然科学基金(31360077;31271868);宁夏自然科学基金(NZ13045)~~

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。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 func-tional 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-bipyr- idyl （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 zwitte-rionic stationary phase （Sil-DMAEAPS） was obtained. The Sil-DMAEAPS stationary phase was characterized by element analysis. Chromatographic evaluation in hydrophilic interaction chro-matography （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.

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

分 类 号：O658[理学—分析化学]