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基于聚甲基丙烯酸酯的弱阳离子交换功能整体毛细管柱用于毛细管电色谱。

Polymethacrylate-based monolithic capillary column with weak cation exchange functionalities for capillary electrochromatography.

机构信息

Department of Chemistry, Biochemistry Division, Hacettepe University, Ankara, Turkey.

出版信息

J Sep Sci. 2012 Apr;35(8):1010-6. doi: 10.1002/jssc.201100927.

DOI:10.1002/jssc.201100927
PMID:22589162
Abstract

Polymethacrylate-based monolith with weak cation exchange functionalities was prepared in capillary column (i.d. 100 μm, o.d. 375 μm) by in situ polymerization of butyl methacrylate, ethylene dimethacrylate and N-methacryloyl-L-glutamic acid in presence of porogens. The porogen mixture included N,N-dimethyl formamide and phosphate buffer. The preparation procedure of stationary phase contained the synthesis of monomer, silanization of capillary inner wall and in situ polymerization. The use of amino acid based monomer for the monolith synthesis is one of the originalities of this novel approach. N-methacryloyl-L-glutamic acid has two carboxyl functionalities. The separation of the solutes were performed at different acetonitrile/phosphate buffer and acetonitrile/sodium hydroxide contents. The applied voltage for the alkyl benzenes was changed between +5 and +30 kV. CEC separations of alkyl benzenes, acidic, basic, phenolic and some polycylic aromatic compounds were succesfully performed under capillary-electrochromatography mode with cathodic electroosmotic flow.

摘要

采用原位聚合法在毛细管柱(内径 100μm,外径 375μm)中制备了具有弱阳离子交换功能的聚甲基丙烯酸酯整体柱。在致孔剂存在下,由甲基丙烯酸丁酯、二乙烯基苯和 N-丙烯酰-L-谷氨酸共聚而成。致孔剂混合物包括 N,N-二甲基甲酰胺和磷酸盐缓冲液。固定相的制备过程包括单体的合成、毛细管内壁的硅烷化和原位聚合。在整体柱合成中使用氨基酸单体是这种新方法的创新之一。N-丙烯酰-L-谷氨酸具有两个羧基官能团。在不同的乙腈/磷酸盐缓冲液和乙腈/氢氧化钠含量下进行了溶质的分离。烷基苯的应用电压在+5 和+30 kV 之间变化。在阴极电渗流作用下,成功地以毛细管电色谱模式分离了烷基苯、酸性、碱性、酚类和一些多环芳烃化合物。

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