【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。更多还原

【Abstract】 A zwitterionic sulfobetaine functional monomer N,N-dimethyl-N-acryloyloxyethyl-Nammonium 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 by1H-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.更多还原