散堆聚乙二醇开管毛细管液相色谱柱的原位制备与评价  

Situ Preparation and Performance Evaluation of Open Tubular Columns Fabricated by Bulk Polyethylene Glycol for Capillary Liquid Chromatography

作　　者：张维冰[1] 彭丽[1] 张凌怡[1] 高羽[1] 陈雅静[1] 刘海燕[1] 

机构地区：[1]华东理工大学化学与分子工程学院,上海200237

出　　处：《华东理工大学学报（自然科学版）》2016年第3期357-362,共6页Journal of East China University of Science and Technology

基　　金：国家自然科学基金项目(21475044);国家重大科学仪器设备开发专项(2012YQ120044)

摘　　要：采用表面引发原子转移自由基聚合反应,原位制备了聚乙二醇开管毛细管液相色谱柱,色谱固定相床超长的聚乙二醇分子在毛细管内壁形成散堆结构,极大地提高相比及样品容量,扫描电镜可观察到毛细管内壁形成的床层表面粗糙。在毛细管液相色谱模式下,4-羟基苯甲酸、苯甲酸、2,4-二羟基苯甲酸和苯的混合样品被用于评价其分离性能,结果表明,所制备的新型开管柱不仅保留了开管柱分析速度快的特征,也因其散堆结构较通常的开管柱提供更多的作用位点,还能有效改善分离性能。连续5次进样,4种小分子的混合物保留时间的相对标准偏差均小于2.5%,说明该柱的重复性较好。进一步将色谱柱用于混合蛋白质的分离,也取得了良好的效果。An open tubular capillary liquid chromatography column （OTCLC） coated by poly[-glycidyl methacrylate-co-poly（ethylene glycol） diacrylate] （GMA-co-PEGDA） was prepared by surface initiated atom transfer radical polymerization （SI-ATRP）. The polyethylene glycol grafting resulted in the formation of bulk structure, obviously increasing the phase ratio and column capacity. Characterized by scanning electron microscopy （SEM）, the monolithic layer was observed to be rough. Four small molecules including 4-hydroxy benzoic acid, benzoic acid, 2, 4-dihydroxy benzoic acid and benzene were used to evaluate the separation performance of the open-tubular capillary liquid chromatography column. The results showed that bulk structure of the poly （GMA-co-PEGDA） OTCC not only remained the characteristic of fast separation but also provided more active sites. The run-to-run （n=5） relative standard deviations （RSDs） for retention time for 5 consecutive injections of 4 molecules were less than 2.5%, indicating good repeatability. Finally,the OTCC was applied to the separation of protein mixtures, and also obtained good separation ability.

关 键 词：开管毛细管柱 表面引发原子转移自由基聚合反应 毛细管液相色谱 

分 类 号：O658[理学—分析化学]