酰胺型键合相的简便制备及评价

Simple Preparation and Evaluations of Amide-Octyl-Bonded Phase

提供了一种酰胺型键合相的简便合成方法 ,即氨丙基三乙氧基硅烷先与烷基酰氯反应 ,然后再键合到硅胶上。该合成路径具有很好的重复性 ,得到的最后产物的硅胶表面键合链均一。用元素分析、核磁共振和红外光谱对最后产物进行了表征。以甲醇和水为二元流动相 ,用包括碱性、酸性和中性有机化合物在内的混合物对该键合相进行了色谱评价 ,并考察了该键合相的适用pH范围及水解稳定性。结果表明 ,该键合相具有较好的色谱性能 ,且在 pH 2 5～ 7 5时稳定性能良好 ,可有效地用于碱性化合物的分析分离。

A simple preparation process of amide octyl bonded phase (AOBP) is described. In the process aminopropyltriethoxysilane first reacted with octanoyl chloride and then the obtained intermediate was bonded onto porous silica. Characterization of prepared packing was carried out with elemental analysis, solid state nuclear magnetic resonance ( 13 C NMR) and Fourier transform infrared (FTIR) spectroscopy. Chromatographic evaluations were carried out by testing with a mixture including acidic, basic and neutral organic compounds using methanol water as binary mobile phase. The results show that the stationary phase has excellent chromatographic properties and resistance to hydrolysis between pH 2 5-7 5. It can be used for the efficient separation of basic compounds.