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

作　　者：刘元元[1] 李静 王彦[1] 闫超[1,2] LIU Yuanyuan;LI Jing;WANG Yan;YAN Chao(School of Pharmacy,Shanghai Jiaotong University,Shanghai 200240;Unimicro(Shanghai)Technologies Co.,Ltd.,Shanghai 201203)

机构地区：[1]上海交通大学药学院,上海200240 [2]上海通微分析技术有限公司,上海201203

出　　处：《分析科学学报》2020年第2期159-165,共7页Journal of Analytical Science

基　　金：上海市科委科技创新行动计划(No.1614220300,17142201000,17DZ2201500)。

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.

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 

分 类 号：O657.8[理学—分析化学]