新型杂化两性离子毛细管电色谱整体柱的制备与评价  

Preparation and Evaluation of a Novel Organic-inorganic Hybrid Zwitterionic Monolithic Column for Capillary Electrochromatography

作　　者：李金祥[1] 杨悦 周雨晴 LI Jin-xiang;YANG Yue;ZHOU Yu-qing(School of Chemistry and Chemical Engineering,Liaoning Normal University,Dalian 116029,China)

机构地区：[1]辽宁师范大学化学化工学院,大连116029

出　　处：《德州学院学报》2020年第2期33-36,39,共5页Journal of Dezhou University

摘　　要：以表面预烯基化的硅胶纳米颗粒(直径10-20 nm)为交联剂,2-二甲基乙基胺甲基丙烯酸酯(DAMA)和甲基丙烯酸(MAA)为功能单体,环己醇、甲醇和水为致孔剂,偶氮二异丁腈(AIBN)作为引发剂,在毛细管(150μm)内通过原位聚合方法制备一种新型有机-无机杂化两性离子交换毛细管电色谱整体柱(以下简称杂化柱).实验考察了致孔剂的组成及比例、有机功能单体浓度、单体总浓度等主要因素对固定相形貌和孔结构的影响,依据扫描电镜图和压力对流速曲线确定了杂化柱的制备条件.该杂化柱与有机整体柱相比,其固定相的抗溶胀能力强、连续床孔隙均匀;与无机整体柱相比,制备过程简便、无需后修饰;与以往文献报道的有机-无机杂化整体柱相比,制备方法更简单.该柱带有两性电荷基团,通过改变流动相的pH值来调节固定相表面电荷的性质与电渗流的大小和方向,从而改变离子交换分离模式,对一组无机阴离子和有机胺类化合物进行了分离.A novel organic-inorganic hybrid zwitterionic ion-exchange monolithic column(shorted as hybrid column hereafter)was prepared for capillary electrochromatography by in-situ polymerization in a fused silica capillary(i.d.150μm)using pre-alkenylated silica nanoparticles(i.d.10-20 nm)as crosslinkers,2-dimethylethylamine methacrylate(DAMA)and methacrylic acid(MAA)as functional monomers,in the presence of the porogenic solvent consisting of water,cyclohexanol and methanol.The preparation conditions,including the composition of porogen,the total concentration of the three monomers and their ratios,the time and temperature of polymerization were investigated and selected based on scanning electron microscopic images and the curves of backpressure vs flow-rate.Compared with the organic monolithic column,the hybrid monolith has the merits of less swelling-shrinking,more uniform pore sizes.Compared with the traditional inorganic monolithic column,the preparation process of the hybrid column is simpler and no need for post-modification.Compared with the organicinorganic hybrid monolithic columns reported previously,the present preparation method is much simpler.The monolith surface possesses zwitterionic charge groups,therefore the flow-rate and direction of the electroosmotic flow can be controlled by adjusting the pH of the mobile phase.A group of commom inorganic anions were separated based on ion-exchange mechanism and a group of organic amines were separated base on the mixed mechanism of ion-exchange and hydrophobic interaction.

关 键 词：毛细管电色谱 两性离子交换 硅胶纳米颗粒 杂化整体柱 

分 类 号：O657.7[理学—分析化学]