Abstract

In this proof-of-concept study, new monolithic columns were prepared by incorporating fumed silica nanoparticles (FNSPs) that are surface functionalized by covalent attachment of 1-[3-(trimethoxysilyl)propyl]urea moieties (i.e., carbamide-FSNPs). The prepared monolithic columns were successfully utilized in hydrophilic interaction liquid chromatography (HILIC) of small, relatively polar solutes. The organic polymer monolithic matrix was based on the in situ polymerization of glyceryl monomethacrylate (GMM) and ethylene glycol dimethacrylate (EDMA) yielding the poly(GMM-co-EDMA) monolith for the incorporation of carbamide-FSNPs. The poly(GMM-co-EDMA) monolithic column with incorporated carbamide-FSNPs which is referred to as carbamide-FSNPs-poly(GMM-co-EDMA) was investigated over a wide range of mobile phase compositions with polar acidic, weakly basic and neutral analytes including organic acids, food additives, vitamins, biological amines, nucleosides, nucleobases, dimethylformamide, formamide and thiourea. Improved peak shapes and better separations were achieved when anisocratic (i.e., gradient) elution conditions were used for the separation of nucleobases, nucleosides and vitamins. The run-to-run, day-to-day and column-to-column reproducibilities were satisfactory.

摘要

在此概念验证研究中，通过结合气相二氧化硅纳米颗粒（FNSP）制备新的整体式色谱柱，该颗粒通过1- [3-（三甲氧基甲硅烷基）丙基]脲部分（即尿素-FSNP）的共价连接进行了表面官能化处理。制备的整体式色谱柱已成功用于小的相对极性溶质的亲水作用液相色谱（HILIC）中。有机聚合物整体基质基于原位聚合单甲基丙烯酸甘油酯（GMM）和乙二醇二甲基丙烯酸酯（EDMA），得到用于掺入氨基甲酰胺-FSNP的聚（GMM-co-EDMA）整体料。在广泛的极性，弱碱性和极性酸性流动相组成范围内，研究了掺入氨基甲酰胺-FSNPs的聚（GMM-co-EDMA）整体柱，即氨基甲酰胺-FSNPs-聚（GMM-co-EDMA）。中性分析物，包括有机酸，食品添加剂，维生素，生物胺，核苷，核碱，二甲基甲酰胺，甲酰胺和硫脲。当使用各向异性（即梯度）洗脱条件分离核苷碱基，核苷和维生素时，可实现改善的峰形和更好的分离效果。每次运行，每天和色谱柱到色谱柱的重现性均令人满意。