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基于氟化单体甲基丙烯酸三氟乙酯的新型整体固定相的毛细管电色谱。

CEC with new monolithic stationary phase based on a fluorinated monomer, trifluoroethyl methacrylate.

作者信息

Yurtsever Arda, Saraçoğlu Berna, Tuncel Ali

机构信息

Department of Chemical Engineering, Hacettepe University, Beytepe, Ankara, Turkey.

出版信息

Electrophoresis. 2009 Feb;30(4):589-98. doi: 10.1002/elps.200800417.

Abstract

A new, fluorinated monolithic stationary phase for CEC was first synthesized by a single-stage, thermally initiated copolymerization of a fluorinated monomer, 2,2,2-trifluoroethyl methacrylate (TFEM) and ethylene dimethacrylate (EDMA) in the presence of a porogen mixture. In this preparation, 2-acrylamido-2-methyl-1-propanesulfonic acid was used as the charge-bearing monomer. The porogen mixture was prepared by mixing isoamylalcohol and 1,4-butanediol. A clear increase in the electroosmotic mobility was observed with increasing pH. The electroosmotic mobility decreased with increasing ACN concentration. Poly(TFEM-co-EDMA) monolith prepared under optimized polymerization conditions was successfully used in the separation of alkylbenzenes and phenols by CEC. The best chromatographic separation for alkylbenzenes was performed with lower ACN concentrations (i.e. 60% v/v) with respect to the common acrylic-based CEC monoliths. The theoretical plate numbers up to 220 000 plates/m were achieved in the reversed phase separation of phenols. Poly(TFEM-co-EDMA) monolith also allowed the simultaneous separation of aniline and benzoic acid derivatives by a single run and by using a lower ACN concentration in the mobile phase with respect to the similar electrochromatographic separations. A stable retention behaviour in reversed phase separation of alkylbenzenes was obtained with the poly(TFEM-co-EDMA) monolith.

摘要

一种用于毛细管电色谱(CEC)的新型氟化整体固定相首次通过在致孔剂混合物存在下,使氟化单体甲基丙烯酸2,2,2 - 三氟乙酯(TFEM)和二甲基丙烯酸乙烯酯(EDMA)进行单阶段热引发共聚而合成。在该制备过程中,使用2 - 丙烯酰胺基 - 2 - 甲基 - 1 - 丙烷磺酸作为带电单体。致孔剂混合物通过混合异戊醇和1,4 - 丁二醇来制备。随着pH值升高,电渗迁移率明显增加。随着乙腈浓度增加,电渗迁移率降低。在优化的聚合条件下制备的聚(TFEM - co - EDMA)整体柱成功用于通过CEC分离烷基苯和酚类。相对于常见的基于丙烯酸的CEC整体柱,在较低的乙腈浓度(即60% v/v)下对烷基苯进行了最佳的色谱分离。在酚类的反相分离中实现了高达220000塔板数/米的理论塔板数。聚(TFEM - co - EDMA)整体柱还允许通过一次运行并相对于类似的电色谱分离在流动相中使用较低的乙腈浓度同时分离苯胺和苯甲酸衍生物。聚(TFEM - co - EDMA)整体柱在烷基苯的反相分离中获得了稳定的保留行为。

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