Shanghai Key Laboratory of Functional Materials Chemistry, East China University of Science and Technology, Shanghai 200237, China.
J Chromatogr A. 2012 May 25;1239:64-71. doi: 10.1016/j.chroma.2012.03.065. Epub 2012 Mar 28.
The core-shell silica nanoparticles Fe(3)O(4)@SiO(2)/NH(2), wormlike and hexagonal SBA-15 silica were incorporated into polymethacrylate monolithic columns containing butyl methacrylate (BMA) and ethylene dimethacrylate (EDMA), respectively to develop novel stationary phases with mixing mechanism of reverse phase and ion exchange. Experimental conditions including types of nanoparticles, dispersion pattern, nanoparticles concentration, column placement mode, and reaction temperature were optimized for simple and stable column preparation. The poly(BMA-EDMA-Fe(3)O(4)@SiO(2)/NH(2)) and poly(BMA-EDMA-SBA-15/NH(2)) (both wormlike and hexagonal shape nanoparticles) monolithic columns were evaluated with mixture of organic acids as sample in capillary electrochromatography (CEC) mode and the relative column efficiency reaches 290,000plates/m. The results indicate that the incorporation of nanoparticles with various shapes enhances both selectivity and column efficiency due to high specific surface area of nanoparticles and mixing separation mechanism. In addition, poly(BMA-EDMA-Fe(3)O(4)@SiO(2)/NH(2)) monolith capillary column was applied to separation of aqueous extract of rhizoma gastrodiae and showed great potential in the method development of complex samples.
核壳结构的 Fe(3)O(4)@SiO(2)/NH(2) 纳米硅球、蠕虫状和六方介孔硅 SBA-15 被分别引入到含有甲基丙烯酸丁酯（BMA）和二甲基丙烯酸乙二醇酯（EDMA）的聚甲基丙烯酸甲酯整体柱中，以开发具有反相和离子交换混合作用的新型固定相。实验条件包括纳米粒子的类型、分散方式、纳米粒子浓度、柱子放置模式和反应温度，以优化简单且稳定的柱子制备方法。聚（BMA-EDMA-Fe(3)O(4)@SiO(2)/NH(2)）和聚（BMA-EDMA-SBA-15/NH(2)）（均为蠕虫状和六方状纳米粒子）整体柱在毛细管电色谱（CEC）模式下以有机酸混合物作为样品进行了评估，相对柱效率达到 290000 板/米。结果表明，由于纳米粒子的高比表面积和混合分离机制，不同形状的纳米粒子的加入增强了选择性和柱效率。此外，聚（BMA-EDMA-Fe(3)O(4)@SiO(2)/NH(2)）整体柱毛细管柱被应用于天麻根茎提取物的分离，在复杂样品的方法开发中显示出巨大的潜力。
