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Mixed-mode chromatographic performance using nicotinic acid-functionalized chito-oligosaccharide-bonded Ti/Si hybrid monolithic capillary columns.
Analytical Sciences ( IF 1.6 ) Pub Date : 2023-09-06 , DOI: 10.1007/s44211-023-00416-3
Mahmoud A M El-Nouby 1, 2 , Lee Wah Lim 3, 4, 5
Affiliation  

This article describes the fabrication of porous nicotinic acid-functionalized chito-oligosaccharide-bonded titania/silica hybrid monoliths (TiO2/SiO2@ChO-N) through a co-gelation sol-gel process. A capillary monolith with a well-defined and homogeneous structure was obtained by controlling the hydrolysis speed of titanium alkoxides in a sol mixture by using glycerol and acetylacetone. As a result of the functionalization with chito-oligosaccharides (ChO)-modified nicotinic acid, the obtained stationary phase provides superior physiochemical properties, such as a cationic hydrophilic surface, porosity, and mechanical strength. Scanning electron microscope and attenuated total reflectance-infrared spectroscopy were used to characterize the functionalized monolithic columns. The produced capillary columns showed high chromatographic performance with acceptable selectivity for charged analytes as well as organic polar compounds such as nucleic bases, nucleosides, carbamate pesticides, and strobilurin fungicides. The obtained results also indicated that the functionalized ChO's amino, amide, hydroxyl, and pyridinium ring moieties served as hydrophilic electrostatic traps for charged substances, in addition to stroing π-π interaction with the carbamate pesticides and strobilurin fungicides analytes via hydrogen bonding.

中文翻译:

使用烟酸功能化壳寡糖键合 Ti/Si 混合整体式毛细管柱的混合模式色谱性能。

本文介绍了通过共凝胶溶胶-凝胶工艺制备多孔烟酸功能化壳寡糖键合二氧化钛/二氧化硅杂化整体材料 (TiO2/SiO2@ChO-N)。通过使用甘油和乙酰丙酮控制溶胶混合物中钛醇盐的水解速度,获得了具有明确且均匀结构的毛细管整体件。由于用壳寡糖 (ChO) 修饰的烟酸进行官能化,所得固定相具有优异的理化性质,例如阳离子亲水表面、孔隙率和机械强度。使用扫描电子显微镜和衰减全反射红外光谱来表征功能化整体柱。所生产的毛细管柱表现出高色谱性能,对带电分析物以及有机极性化合物(如核酸碱基、核苷、氨基甲酸酯农药和嗜球果伞素杀菌剂)具有可接受的选择性。所得结果还表明,功能化 ChO 的氨基、酰胺、羟基和吡啶鎓环部分除了通过氢键与氨基甲酸酯农药和甲氧基丙烯酸酯类杀菌剂分析物产生 π-π 相互作用外,还可以作为带电物质的亲水性静电陷阱。
更新日期:2023-09-06
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