新型聚合物多孔涂层毛细管开管柱的制备及电色谱研究

以甲基丙烯酸缩水甘油酯(GMA)和乙二醇二甲基丙烯酸酯(EDMA)为前驱体制备了新型聚合物多孔涂层毛细管开管(PLOT)柱固定相。通过优化聚合反应时间、致孔剂比例及交联剂比例获得了色谱性能良好的PLOT柱,扫描电镜结果显示毛细管柱内的多孔涂层厚度适中且均匀。在毛细管电色谱模式下,PLOT柱以反相色谱分离机理有效分离了中性、酸性和碱性小分子。人血清白蛋白(HSA)共价结合的蛋白亲和PLOT柱对5对手性对映体实现了较好的分离,且其分离度远高于HSA修饰的单层聚合物毛细管开管柱。PLOT柱分离烷基苯的日内、日间和柱间的相对标准偏差分别小于1.7%、4.8%和7.8%。

Preparation of a Novel Polymer Porous Layer Open Tubular Capillary Column and Its Electrochromatographic Study

A novel polymer porous layer stationary phase containing the copolymer of glycidyl methacrylate and ethylene glycol dimethacrylate (GMA-EDMA) was fabricated,and applied as a porous layer open tubular capillary (PLOT) column.To obtain a suitable capillary for electrochromatography,various conditions including the polymerization time,the ratio of n-propanol/1,4-butanediol and GMA/EDMA in the polymerization mixture were optimized.Scanning electron microscopy demonstrated a nearly uniform polymer porous layer on the inner wall of the open tubular capillary column.In the capillary electrochromatographic mode,the PLOT column provided the reasonable separation of neutral,acidic and basic small molecules based on a reversed phase mechanism.After immobilizing the chiral selector human serum albumin (HSA),the HSA-PLOT column performed a better chiral recognition for five pairs of enantiomers compared with the single-layer polymer coated open tubular capillary column modified with HSA.The intra-day,inter-day and column-to-column relative standard deviations for alkylbenzenes separated on the PLOT column were less than 1.7％,4.8％ and 7.8％,respectively.