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用于毛细管液相色谱分离极性小分子的聚(甲基丙烯酸烷基酯 - 甲基丙烯酸 - 二甲基丙烯酸乙二酯)整体柱的制备与评价

Preparation and evaluation of poly(alkyl methacrylate-co-methacrylic acid-co-ethylene dimethacrylate) monolithic columns for separating polar small molecules by capillary liquid chromatography.

作者信息

Lin Shu-Ling, Wu Yu-Ru, Lin Tzuen-Yeuan, Fuh Ming-Ren

机构信息

Department of Chemistry, Soochow University, 70 Linhsi Road, Shihlin, 11102 Taipei, Taiwan.

Department of Chemistry, Soochow University, 70 Linhsi Road, Shihlin, 11102 Taipei, Taiwan.

出版信息

Anal Chim Acta. 2015 Apr 29;871:57-65. doi: 10.1016/j.aca.2015.02.015. Epub 2015 Feb 10.

DOI:10.1016/j.aca.2015.02.015
PMID:25847162
Abstract

In this study, methacrylic acid (MAA) was incorporated with alkyl methacrylates to increase the hydrophilicity of the synthesized ethylene dimethacrylate-based (EDMA-based) monoliths for separating polar small molecules by capillary LC analysis. Different alkyl methacrylate-MAA ratios were investigated to prepare a series of 30% alkyl methacrylate-MAA-EDMA monoliths in fused-silica capillaries (250-μm i.d.). The porosity, permeability, and column efficiency of the synthesized MAA-incorporated monolithic columns were characterized. A mixture of phenol derivatives is employed to evaluate the applicability of using the prepared monolithic columns for separating small molecules. Fast separation of six phenol derivatives was achieved in 5 min with gradient elution using the selected poly(lauryl methacrylate-co-MAA-co-EDMA) monolithic column. In addition, the effect of acetonitrile content in mobile phase on retention factor and plate height as well as the plate height-flow velocity curves were also investigated to further examine the performance of the selected poly(lauryl methacrylate-co-MAA-co-EDMA) monolithic column. Moreover, the applicability of prepared polymer-based monolithic column for potential food safety applications was also demonstrated by analyzing five aflatoxins and three phenicol antibiotics using the selected poly(lauryl methacrylate-co-MAA-co-EDMA) monolithic column.

摘要

在本研究中,将甲基丙烯酸(MAA)与甲基丙烯酸烷基酯结合,以提高合成的基于二甲基丙烯酸乙烯酯(EDMA基)整体柱的亲水性,用于通过毛细管液相色谱分析分离极性小分子。研究了不同的甲基丙烯酸烷基酯-MAA比例,以在内径为250μm的熔融石英毛细管中制备一系列30%甲基丙烯酸烷基酯-MAA-EDMA整体柱。对合成的含MAA整体柱的孔隙率、渗透率和柱效进行了表征。采用苯酚衍生物混合物来评估所制备的整体柱用于分离小分子的适用性。使用选定的聚(甲基丙烯酸月桂酯-co-MAA-co-EDMA)整体柱,通过梯度洗脱在5分钟内实现了六种苯酚衍生物的快速分离。此外,还研究了流动相中乙腈含量对保留因子和板高的影响以及板高-流速曲线,以进一步考察选定的聚(甲基丙烯酸月桂酯-co-MAA-co-EDMA)整体柱的性能。此外,通过使用选定的聚(甲基丙烯酸月桂酯-co-MAA-co-EDMA)整体柱分析五种黄曲霉毒素和三种氯霉素抗生素,也证明了所制备的聚合物基整体柱在潜在食品安全应用中的适用性。

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