Department of Chemistry, Oklahoma State University, Stillwater, OK 74078-3071, United States.
J Chromatogr A. 2013 Nov 22;1317:77-84. doi: 10.1016/j.chroma.2013.07.100. Epub 2013 Aug 1.
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.
新型的立体专一性单体被引入到亲水作用毛细管电色谱(HI-CEC)中。在一种情况下,通过在三元致孔溶剂中原位聚合甲基丙烯酰甘油(GMM)和季戊四醇三丙烯酸酯(PETA),得到中性立体专一性单体。GMM 和 PETA 具有羟基官能团,赋予单体亲水性相互作用位点。这种单体被命名为羟甲基单体。尽管羟甲基单体是中性的,表面没有固定电荷,但由于来自流动相的离子吸附形成的双电层,观察到相对较强的阴极电渗流,产生整体流动相流动。第二种单体是带电荷的,称为 AP-单体,其表面具有胺/酰胺官能团,通过在环己醇、十二醇和甲醇作为致孔剂存在的情况下,原位聚合 N-(3-氨丙基)甲基丙烯酰胺盐酸盐(NAPM)和乙二醇二甲基丙烯酸酯(EDMA)制备。在研究的 pH 范围内观察到强烈的阳极电渗流。AP-单体进一步通过用中性单糖和低聚糖修饰其表面来用于 HI-CEC,以制备一系列所谓的糖修饰 AP-单体(SMAP-单体),其被认为是具有极性胺/酰胺基团亚层和糖(多羟基顶层)的分层亲水单体。SMAP-单体可以被视为羟甲基单体和 AP-单体的混合物。各种单体的极性似乎遵循以下顺序:羟甲基单体<AP-单体<SMAP-单体。新型单体在广泛的洗脱条件下进行了表征,包括各种极性溶质,如酚类、取代酚类、核酸碱基、核苷和核苷酸。