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A new anion-exchange/hydrophobic monolith as stationary phase for nano liquid chromatography of small organic molecules and inorganic anions

机译:一种新型阴离子交换/疏水整体柱作为固定相,用于有机小分子和无机阴离子的纳米液相色谱

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In this study, an anion-exchange/hydrophobic polymethacrylate-based stationary phase was prepared for nano-liquid chromatography of small organic molecules and inorganic anions. The stationary phase was synthesized by in situ polymerization of 3-chloro-2-hydroxypropylmethacrylate and ethylene dimethacrylate inside silanized 100 mu m i.d. fused silica capillary. The porogen mixture consisted of toluene and dodecanol. The pore size distrubution profiles of the resulting monolith were determined by mercury intrusion porosimetry and the morphology of the prepared monolith was investigated by scanning electron microscope. Good permeability, stability and column efficiency were observed on the monolithic column with nano flow. The produced monolithic column, which contains reactive chloro groups, was then modified by reaction with N,N-dimethyl-N-dodecylamine to obtain an anion-exchange/hydrophobic monolithic stationary phase. The functionalized monolith contained ionizable amine groups and hydrophobic groups that are useful of anion-exchange/hydrophobic mixed-mode chromatography. The final monolithic column performance with respect to anion-exchange and hydrophobic interactions was assesed by the separation of alkylbenzene derivatives, phenolic compounds and inorganic anions, respectively. Theoretical plate numbers up to 23,000 plates/m were successfully achieved in the separation of inorganic anions. (C) 2015 Elsevier B.V. All rights reserved.
机译:在这项研究中,制备了阴离子交换/疏水性聚甲基丙烯酸酯基固定相,用于有机小分子和无机阴离子的纳米液相色谱分析。固定相是通过在硅烷化的100 µm i.d内原位聚合甲基丙烯酸3-氯-2-羟丙酯和二甲基丙烯酸乙二酯而合成的。熔融石英毛细管。致孔剂混合物由甲苯和十二烷醇组成。通过压汞法测定所得整料的孔径分布轮廓,并通过扫描电子显微镜研究所制备整料的形态。在具有纳米流的整体式色谱柱上观察到良好的渗透性,稳定性和色谱柱效率。然后通过与N,N-二甲基-N-十二烷基胺反应来修饰所产生的包含反应性氯基的整体式柱,从而获得阴离子交换/疏水整体式固定相。官能化的整体结构包含可电离的胺基和疏水基团,可用于阴离子交换/疏水混合模式色谱。关于阴离子交换和疏水相互作用的最终整体柱性能分别通过烷基苯衍生物,酚类化合物和无机阴离子的分离来评估。在分离无机阴离子中,理论塔板数成功达到23,000塔板/米。 (C)2015 Elsevier B.V.保留所有权利。

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