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用于电色谱分离的丙烯酸酯基整体固定相的开发。

Development of acrylate-based monolithic stationary phases for electrochromatographic separations.

作者信息

Barrioulet Marie-Pierre, Delaunay-Bertoncini Nathalie, Demesmay Claire, Rocca Jean-Louis

机构信息

Laboratoire des Sciences Analytiques, Université Claude Bernard Lyon I, Villeurbanne, France.

出版信息

Electrophoresis. 2005 Nov;26(21):4104-15. doi: 10.1002/elps.200500251.

Abstract

Organic monolithic stationary phases were synthesized in fused-silica capillaries. They were prepared by in situ polymerization under UV irradiation of various alkyl acrylates, 1,3-butanediol diacrylate, and 2-acrylamido-2-methyl-1-propanesulfonic acid in a ternary porogenic solvent. The resulting stationary phases were tested in CEC. The influence of UV irradiation energy on the resulting separative performances of the monoliths was studied. It was thus demonstrated that the use of hexyl acrylate rather than butyl acrylate and lauryl methacrylate gives highly efficient monoliths (more than 300 000 plates per meter) with optimized EOF. It was also confirmed that the mobile phase ionic strength may affect significantly the separation efficiency. The influence of the nature of the mobile phase organic modifier (ACN or methanol) on EOF, retention, efficiency, and selectivity was studied and differences were observed. Finally, the performances of monolithic stationary phases developed and optimized for CEC separations were evaluated in nanoLC.

摘要

在熔融石英毛细管中合成了有机整体固定相。它们是通过在紫外光照射下,使各种丙烯酸烷基酯、1,3 - 丁二醇二丙烯酸酯和2 - 丙烯酰胺 - 2 - 甲基 - 1 - 丙磺酸在三元致孔溶剂中原位聚合制备而成。将所得的固定相用于毛细管电色谱(CEC)测试。研究了紫外光照射能量对整体柱分离性能的影响。结果表明,使用丙烯酸己酯而非丙烯酸丁酯和甲基丙烯酸月桂酯可得到具有优化电渗流(EOF)的高效整体柱(每米超过300000块理论塔板)。还证实了流动相离子强度可能会显著影响分离效率。研究了流动相有机改性剂(乙腈或甲醇)的性质对电渗流、保留、效率和选择性的影响,并观察到了差异。最后,在纳升液相色谱(nanoLC)中评估了为毛细管电色谱分离开发和优化的整体固定相的性能。

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