摘 要: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228 542 N/m。
关键词:开管毛细管电色谱;固定相;二氧化硅纳米;磺胺类化合物
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Preparation of a Novel SiO2 Nanoparticles Based
Open Tubular Capillary Column and
Its Electrochromatographic Study
Abstract: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.
Keywords:Open tubular capillary electrochromatography;Stationary phase;SiO2 nanoparticles;Sulfonamides
分析科学