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Neutral Charged and Stratified Polar Monoliths for Hydrophilic Interaction Capillary Electrochromatography

机译:亲水相互作用毛细管电色谱的中性带电和分层极性整料

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摘要

Novel polar monoliths were introduced for hydrophilic interaction capillary electrochromatography (HI-CEC). In one case, a neutral polar monolith resulted from the in situ polymerization of glyceryl methacrylate (GMM) and pentaerythritol triacrylate (PETA) in a ternary porogenic solvent. GMM and PETA possess hydroxyl functional groups, which impart the monolith with hydrophilic interaction sites. This monolith is designated as hydroxy monolith. Although the hydroxy monolith is neutral and void of fixed charges on the surface, a relatively strong cathodal EOF was observed due to the electric double layer formed by the adsorption of ions from the mobile phase, producing a bulk mobile phase flow. The second monolith is charged and referred to as AP-monolith that possesses amine/amide functionalities on its surface, and was prepared by the in situ polymerization of N-(3-aminopropyl) methacrylamide hydrochloride (NAPM) and ethylene dimethacrylate (EDMA) in the presence of cyclohexanol, dodecanol and methanol as porogens. Over the pH range studied a strong anodal EOF was observed. The AP-monolith was further exploited in HI-CEC by modifying its surface with neutral mono- and oligosaccharides to produce a series of the so called sugar modified AP-monoliths (SMAP-monolith), which are considered as stratified hydrophilic monoliths possessing a sub-layer of polar amine/amide groups and a top layer of sugar (a polyhydroxy top layer).The SMAP-monoliths can be viewed as a blend of both the hydroxy monolith and the AP-monolith. The polarity of the various monoliths seems to follow the order: hydroxy monolith < AP-monolith < SMAP-monolith. The novel monoliths were characterized over a wide range of elution conditions with a variety of polar solutes including phenols, substituted phenols, nucleic acid bases, nucleosides and nucleotides
机译:新型极性单块被引入用于亲水相互作用毛细管电色谱(HI-CEC)。在一种情况下,中性极性整料是由三元致孔剂溶剂中的甲基丙烯酸甘油酯(GMM)和季戊四醇三丙烯酸酯(PETA)原位聚合产生的。 GMM和PETA具有羟基官能团,这些官能团使整体结构具有亲水相互作用位点。该整料被称为羟基整料。尽管羟基整料是中性的,并且在表面上没有固定电荷,但是由于通过吸附来自流动相的离子而形成的双电层,形成了较大的流动相流,因此观察到了相对较强的阴极EOF。将第二块料装入并称为AP-块,在其表面上具有胺/酰胺官能团,并通过将N-(3-氨基丙基)甲基丙烯酰胺盐酸盐(NAPM)和二甲基丙烯酸乙二酯(EDMA)原位聚合而制得。存在环己醇,十二烷醇和甲醇作为致孔剂。在所研究的pH范围内,观察到了较强的阳极EOF。通过用中性单糖和寡糖修饰其表面,在HI-CEC中进一步开发了AP-整料,以生产一系列所谓的糖修饰的AP-整料(SMAP-整料),它们被认为是具有亚结构的分层亲水性整料极性胺/酰胺基团层和糖的顶层(多羟基顶层)。SMAP整体料可以看作是羟基整体料和AP整体料的混合物。各种整体结构的极性似乎遵循以下顺序:羟基整体结构

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