Carrasco-Correa Enrique Javier, Ramis-Ramos Guillermo, Herrero-Martínez José Manuel
Department of Analytical Chemistry, University of Valencia, Dr. Moliner 50, 46100 Burjassot, Valencia, Spain.
Department of Analytical Chemistry, University of Valencia, Dr. Moliner 50, 46100 Burjassot, Valencia, Spain.
J Chromatogr A. 2015 Mar 13;1385:77-84. doi: 10.1016/j.chroma.2015.01.044. Epub 2015 Jan 31.
Vinylized iron oxide magnetic nanoparticles (VMNPs) were incorporated into polymethacrylate monolithic columns to develop novel stationary phases with enhanced separation performance. The VMNPs were dispersed in a polymerization mixture containing gycidyl methacrylate and ethylene glycol dimethacrylate as monomers, cyclohexanol and 1-dodecanol as porogens and azobisisobutyronitrile as initiator. The stability of the VMNPs in the polymerization mixture was investigated at several VMNP contents. Using short UV-polymerization times, polymeric beds with homogenously dispersed VMNPs were obtained. The novel stationary phases were characterized by scanning electron microscopy. The chromatographic performance of these hybrid monoliths was evaluated using alkyl benzenes and organophosphorous pesticides as test solutes. Using capillary electrochromatography, efficiencies up to 130,000 plates/m were achieved. The increase of the specific surface area of hybrid monoliths led to an increase in the retention of all the test analytes, and an enhancement of efficiency. The resulting hybrid monolithic columns exhibited satisfactory column to-column and batch-to-batch reproducibilities with RSDs values below 6%.
将乙烯基化氧化铁磁性纳米颗粒(VMNPs)掺入聚甲基丙烯酸酯整体柱中,以开发具有增强分离性能的新型固定相。VMNPs分散在一种聚合混合物中,该混合物包含甲基丙烯酸缩水甘油酯和乙二醇二甲基丙烯酸酯作为单体、环己醇和1-十二烷醇作为致孔剂以及偶氮二异丁腈作为引发剂。在几种VMNP含量下研究了VMNPs在聚合混合物中的稳定性。使用较短的紫外光聚合时间,获得了VMNPs均匀分散的聚合物床。通过扫描电子显微镜对新型固定相进行了表征。使用烷基苯和有机磷农药作为测试溶质评估了这些混合整体柱的色谱性能。采用毛细管电色谱法,实现了高达130,000理论塔板数/米的柱效。混合整体柱比表面积的增加导致所有测试分析物的保留增加,并且柱效提高。所得的混合整体柱在柱与柱之间以及批次与批次之间表现出令人满意的重现性,相对标准偏差(RSD)值低于6%。