【作者】 白泉； 夏红军； 万广平； 王军； 刘艳娜； 杨晓辉；

【Author】 Quan Bai;Hongjun Xia;Guangping Wan;Jun Wang;Yanna Liu;Xiaohui Yang;Institute of Modern Separation Science, Key Lab of Modern Separation Science in Shaanxi Province, Northwest University;

【机构】 西北大学现代分离科学研究所陕西省现代分离科学重点实验室；

【摘要】 表面多孔核壳型色谱柱具有高柱效、高分辨的特点而成为超快HPLC分析的理想工具,已应用于复杂样品的快速分离分析中^[1]。目前,其制备方法有层层自组装法（LbL）^[2]、脲醛树脂法^[3]、沉积法^[4]及模板法^[5]。但是上述方法尚存在制备过程繁琐,粒径分布不均,易团聚、孔径的尺寸和结构不易控制等问题。针对上述问题,本文以脲醛树脂为模板,采用聚合诱导胶体聚集技术（PICA）制备核-壳型微球,改进了硅胶核的改性方法并对反应条件进行了优化和精确控制,有效地解决了在SiO₂@SiO₂核-壳微球制备过程中二次成核的问题。通过调控核/壳投料比和硅溶胶纳米粒子的粒径,实现了不同壳层厚度和孔径的SiO₂@SiO₂核-壳微球的可控制备,成功制备出了单分散性良好、粒径均一的SiO₂@SiO₂核-壳微球。将不同孔径的核-壳微球经C-18改性后,分别用于小分子和蛋白质的分离,在2 min内实现对小分子的快速分离,而在5min内完成了6种蛋白质的快速分离。表明利用PICA法制备的SiO₂@SiO₂核壳微球在液相色谱快速分离分析中具有很好的应用前景。更多还原

【Abstract】 Superficially porous core-shell silica microspheres(CSSMs) have been a great success for the fast separation of small molecules and proteins in recent years. In this paper, the CSSMs were synthesized by an improved polymerization-induced colloid aggregation(PICA) method using urea-formaldehyde polymers as the templates. The agglomeration of the functionalized silica core was avoided by the surface modification through reflux with ureidopropyltrimethoxysilane in the neutral ethanol solution at 80 °C, and the secondary nucleation of the silica nanoparticles during the preparation process could also be inhibited via the optimization of the reaction conditions,such as pH, temperature, colloidal silica sol concentration and the reaction time. The controllable shell thickness and pore size of the synthesized monodisperse CSSMs were successfully obtained by adjusting the weight ratio of silica core/colloidal silica sol and the particle size of colloidal silica sol, respectively. The C18-modified CSSMs with different pore sizes were used to separate small solutes and proteins. The higher efficient separation and relatively low back pressure of the synthesized core-shell column demonstrate that the CSSMs have a great potential application for fast HPLC.更多还原