4-氨基吡啶分子印迹聚合物毛细管整体柱的制备及电色谱性能研究  

Preparation of 4-Aminopyridine Imprinted Polymer-based Monolithic Capillary Column and Evaluation of Electrochromatography

作　　者：闫伟英[1] 张智超[1] 高如瑜[1] 王琴孙[1] 

机构地区：[1]南开大学元素有机化学研究所,元素有机化学国家重点实验室,天津300071

出　　处：《高等学校化学学报》2003年第6期1026-1030,共5页Chemical Journal of Chinese Universities

基　　金：国家自然科学基金 (批准号 :2 0 175 0 10 )资助

摘　　要：以 4 -氨基吡啶 (4 -AP)为印迹分子 ,热引发原位合成了分子印迹聚合物毛细管整体柱 ,聚合物通过共价键和石英毛细管内壁相连 ,制备方法简单、快捷 .在最佳电色谱条件下 ,4 -AP和 2 -AP之间的分离度在印迹聚合物柱上高达 2 .5 ,而在不含印迹的对照柱上仅为 0 .35 .通过研究流动相条件对 4 -AP,2 -AP和硫脲迁移的影响 ,对 4 -AP印迹聚合物的电色谱识别机理进行了探讨 .印迹识别能力随缓冲溶液离子强度的减小或流动相中乙腈比例的增大而增大 .上述两种情形下 ,流动相中阳离子浓度均减少 ,使得聚合物孔穴中可与4 -AP发生静电作用的有效羧基作用位点增加 ,从而显现出孔穴对印迹分子的专一亲和作用 (形状、大小和作用力 ) .缓冲溶液的种类和 p H值对该印迹聚合物识别能力的影响较为复杂 ,在磷酸盐缓冲溶液体系中 ,p H值对识别能力的影响呈抛物线形 ,p H=5时识别能力最强 ;在醋酸盐缓冲溶液体系中 ,高 p H值有利于分离 .The 4-aminopyridine(4-AP) molecularly imprinted polymer(MIP)-based monolithic capillary column was prepared by an in situ thermal-initiated polymerization process; the preparation process is simple and quick. The MIP was covalently linked to the inner wall of fused silica capillary. The performance of the column was evaluated by capillary electrochromatography(CEC). Under the optimal CEC conditions, the resolution of 4-AP and 2-AP was 2.5 on the 4-AP MIP based monolithic column, while only 0\^35 on the reference column without any imprint of 4-AP. The recognition ability of MIP for 4-AP was influenced by a lot of factors including pH, sort of buffers, ionic strength and the content of organic modifier in the mobile phase. The recognition of the MIP was enhanced with decreasing the salt concentration of the buffer or increasing the acetonitrile content in the mobile phase. The phenomena are ascribed to the reduction in the amount of cationic ions in the mobile phase, which compete with 4-AP in combination with carboxyl in the cavity of MIP, and weaken the specific affinity of the imprint cavity for the imprinted molecule. The effect of the sort and pH of buffer on the recognition of the MIP is complicated. For phosphate buffer, the effect of pH is parabolic, giving the best recognition at pH=5, while for acetate buffer, increase in pH benefits the recognition.

关 键 词：4-氨基吡啶 分子印迹聚合物 毛细管整体柱 制备 电色谱性能 毛细管电色谱 微分离技术 

分 类 号：O658[理学—分析化学] O657.8[理学—化学]