新型二氧化硅纳米毛细管开管柱的制备及其电色谱性能的研究

Preparation of a Novel SiO2 Nanoparticles Based Open Tubular Capillary Column and Its Electrochromatographic Study

本文通过原位聚合反应合成了一种基于纤维状二氧化硅纳米(fSiO2)和聚合物(DMAEMA polymer)的材料(P-fSiO2),将该材料采用物理吸附的方式涂覆到毛细管内壁,制备了新型的毛细管电色谱开管柱(P-fSiO2开管柱),并将其应用于磺胺类物质的开管毛细管电色谱(OT-CEC)分离分析。P-fSiO2开管柱的制备方法简便快捷、涂层稳定、重复性好,其中日内相对标准偏差(RSD)值小于4.3%(n=6),日间RSD小于4.9%(n=6),柱间RSD为2.2%(n=5)。通过对缓冲溶液浓度、pH值以及分离电压等因素的考察,可以实现对8种磺胺类化合物的良好分离,其中磺胺喹恶啉(SQX)的柱效高达228542 N/m。

In this work,we synthesized silica nanoparticles(P-fSiO2)stationary phase based on fibrous silica nanoparticles(fSiO2)and polymer(DMAEMA,P)by in-situ polymerization.Then,a novel P-fSiO2 open-tubular column was fabricated by physical adsorption and applied for capillary electrochromatographic separation of sulfonamides.The preparation approach of P-fSiO2 column is simple,rapid,stable and repeatable,with relative standard deviations(RSDs)for run-to-run,day-to-day and column-to-column less than 4.3%,4.9%and 2.2%,respectively.The effect of ion concentration,pH value and the high voltage on the separation was also investigated,the column showed good separation efficiency in the OT-CEC separation mode,with theoretical plate numbers up to 228,542 per meter for sulfaquinoxaline.