反相毛细管电色谱硅胶整体柱的制备及其应用
首发时间:2006-07-11
摘要:采用改进的溶胶-凝胶技术制备了具有高机械强度和化学稳定性的毛细管硅胶整体柱。详细考察了反应物配比对所制备整体柱结构和性能的影响,并在此基础上对制备条件进行了优化。将所制备整体柱用正辛基硅烷修饰后得到反相整体柱,详细考察了流动相pH值、有机改性剂含量对电渗流的影响。采用短端进样方式在优化实验条件下实现了中性化合物的快速分离,对硫脲获得了高达180,000 N/m的柱效。使用所制备整体柱,在电色谱模式下对穿心莲片中的有效成份脱水穿心莲内酯进行了分离,并获得了高达80,000 N/m的柱效。
关键词: 硅胶整体柱 反相毛细管电色谱 制备 脱水穿心莲内酯
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Preparation and Applications of Reversed-phase Silica Monolithic Column for Capillary Electrochromatography
Abstract: A silica monolithic column was successfully prepared by sol-gel technique,and the synthesizing procedure was optimized by changing the ratios of monomers in the mixture and the aftertreatment of dryness and conditioning. Further, octyl group was chemically bonded to the monolithic matrix to afford separation media of reversed-phase. The influence of pH value, organic modifier content on electroosmotic flow (EOF) was studied in detail. Adapting short-end injection method, neutral compounds were quickly separated on the column under optimized conditions, and the column efficiency of 180,000 N/m was achieved for thiourea. Using the monolithic column prepared, dehydroandrographolide in Chuanxinlian was effectively separated in CEC mode for the first time with a theoretical plate number of 80,000 N/m.
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No.7562729651152591****
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