聚甲基丙烯酸酯毛细管整体柱的制备及其性能考察

Preparation and performance of polymethacrylate capillary monolithic columns

以甲基丙烯酸丁酯(BMA)为单体,乙二醇二甲基丙烯酸酯(EDMA)为交联剂,以正丙醇和1,4-丁二醇为二元致孔剂,在毛细管内由热引发进行原位聚合制备聚甲基丙烯酸酯毛细管整体柱。以柱通透性为前提,柱效为优化指标,通过预实验和正交设计优化聚合反应条件,并重点考察显著因素——二元致孔剂之间的比例对柱性能的影响,结果表明,当1,4-丁二醇与正丙醇的质量比为1∶3时,柱通透性好,柱效达到最高水平。对在优化条件下制备的整体柱进行柱性能表征,柱内部结构均匀、渗透性佳,重复性和稳定性的RSD均小于8.5%,说明柱制备方法良好。将所制备的毛细管整体柱分离苯等中性小分子类化合物,表现出典型反相色谱特征,苯的理论塔板数达到22 400,分离度大于4.0,能够满足实际分离分析需求。

A porous polymethacrylate ester-based capillary monolithic column was prepared using in situ co-polymerizing butyl methacrylate（BMA） and ethylene dimethacrylate（EDMA） in binary porogenic solvent 1,4-butanediol and 1-propanol.A series of preliminary experiments and orthogonal experiments were carried out,and demonstrated that the ratio between 1,4-butanediol and 1-propanol was a significant factor.Under the optimized mass ratio of 1 ∶3,the best synthetic polymers were achieved.The column exhibited a uniform structure,good permeability,reproducibility and stability with RSD less than 8.5%,which proved that the polymerization condition was satisfactory.Alkylbenzenes were analyzed to evaluate this monolithic column with CEC method,and the separation of alkylbenzenes was mainly based on typical reversed-phase chromatographic retention mechanism.The theoretical plate number of benzene was 22 400 and the resolutions of alkylbenzenes were more than 4.0.Therefore,the synthetic monolith can be successfully applied to separate neutral small molecules.