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混合模式硅胶基质毛细管电色谱整体柱的制备及其电色谱性能研究

Preparation and Evaluation of Mixed-Mode Silica Monolithic Column for Capillary Electrochromatography

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【作者】 丁国生笪振良袁瑞娟包建民

【Author】 Ding Guosheng, Da Zhenliang, Yuan Ruijuan, Bao Jianmin (School of Pharmaceutical Science and Technologies, Tianjin University, Tianjin 300072)

【机构】 天津大学药物科学与技术学院天津大学药物科学与技术学院 天津300072天津300072

【摘要】 采用温和条件下的溶胶-凝胶技术,成功制备了阴离子交换-反相混合模式硅胶基质毛细管电色谱整体柱。通过调整反应液中不同前体的比例,优化了整体柱的制备条件。通过扫瞄电镜,对柱床进行了表征和分析。实验发现,所制备的整体柱电渗流的方向和大小可随流动相pH值的改变而改变,在酸性和中性条件下,具有从阴极流向阳极的电渗流;当流动相pH值升至约7·5时,电渗流方向发生了反转(由阳极流向阴极)。在优化的实验条件下,用所制备的整体柱对所考察的酸性(中性)化合物实现了快速分离,并获得了高达160,000N/m的柱效。

【Abstract】 A mixed-mode silica monolithic column was successfully prepared by sol-gel technique at mild temperature, and the synthesizing procedure was optimized by changing the ratios of monomers in the mixture. The morphology of monolithic columns was characterized and analyzed by scanning electron microscopy. It was found experimentally that both direction and magnitude of the electroosmotic flow(EOF) changed with the pH values of mobile phase. A reversed anionic EOF was observed in acidic and neutral conditions. When pH increased to 7.5, the direction of the EOF was from anode to cathode. Acidic and neutral compounds were quickly separated on the column under optimized conditions, column efficiency of 160,000 N/m was achieved for o-hydroxybenzoic acid under experimental conditions.

【基金】 天津市科技发展计划资助项目(No.05YFGPGX07900);教育部科学技术研究资助项目(No.704013)
  • 【文献出处】 分析化学 ,Chinese Journal of Analytical Chemistry , 编辑部邮箱 ,2006年S1期
  • 【分类号】O657.8
  • 【被引频次】9
  • 【下载频次】315
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