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况,况-二甲 基丙烯酰氧乙基丙基磺酸铵( 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^(R)-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.