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Polyethyleneimine Immobilized on Silica Endcapped with Octadecyl Groups as a Stationary Phase for RP-LC

机译:固定在以十八烷基为端基的硅胶上的聚乙烯亚胺作为RP-LC的固定相

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A new reversed stationary phase was prepared, based on thermal immobilization of trimethoxysilylpropyl modified polyethyleneimine onto silica particles endcapped with octadecyl molecules. The physicochemical and morphological properties of the stationary phase were characterized by solid state cross-polarization and magic angle spinning ~(29)Si nuclear magnetic resonance, infrared spectroscopy, porosimetry, and elemental analysis. For the studies on reversed phase high-performance liquid chromatography (HPLC) retention, separation of the established Tanaka and Engelhardt test mixtures was performed. The stationary phase showed a typical partition mechanism for the reversed phase; however, the low hydrophobicity required a low organic content solvent in the mobile phase for chromatographic separation of more hydrophobic compounds. The stationary phase also showed low residual silanol activity for the elution of basic compounds due to the protection offered by octadecyl endcapped molecules and the competition provided by the imine groups of the polymeric layer. The proposed stationary phase possesses interesting selectivity and is convenient for applications requiring the separation of more retentive compounds in conventional HPLC columns using more aqueous mobile phases.
机译:基于将三甲氧基甲硅烷基丙基改性的聚乙烯亚胺热固定在以十八烷基分子封端的二氧化硅颗粒上,制备了新的反相固定相。通过固态交叉极化和魔角旋转〜(29)Si核磁共振,红外光谱,孔隙率法和元素分析表征了固定相的理化和形态特性。为了研究反相高效液相色谱(HPLC)保留,对已建立的Tanaka和Engelhardt测试混合物进行了分离。固定相显示出典型的反相分配机理。但是,低疏水性要求流动相中有机物含量低的溶剂才能色谱分离更多疏水性化合物。由于十八烷基封端的分子提供的保护作用以及聚合物层的亚胺基提供的竞争作用,固定相对于碱性化合物的洗脱也显示出较低的残留硅烷醇活性。所提出的固定相具有令人感兴趣的选择性,并且对于需要在使用更多水性流动相的常规HPLC色谱柱中分离更具保留性的化合物的应用场合十分方便。

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