用于碱性物质分离的酰胺型反相色谱键合相的制备及评价

Preparation and Evaluation of Amide-Octyl-Bonded Phase for the Separation of Basic Substances in Reversed-Phase Liquid Chromatography

采用先对硅胶进行氨丙基化 ,然后与辛酰氯键合的方法 ,在国内首次制备了“内嵌”极性官能团酰胺键的反相色谱填料。以甲醇 水为二元流动相 ,用含有中性、酸性和碱性有机化合物的混合物评价了该固定相的疏水性、选择性和亲硅醇基效应 ,并考察了该填料适用的 pH值范围及水解稳定性。结果表明 ,该固定相具有较好的色谱性能 ,且在 pH 2 5～ 7 5时稳定性能良好 。

A new bonded phase, amide octyl bonded phase (AOBP), with an internal polar functional group amide was firstly prepared in domestic by two step reaction process The amino phase was formed in the first step and further modified in the second step by attaching an alkyl chain via reaction of an acid chloride with the amino ligand. Characterization of prepared packing was carried out with elemental analysis and Fourier transform infrared (FTIR) spectrometry. Hydrophobicity, selectivity and silanophilic activity of AOBP were evaluated by using organic components including acidic, bascic and neutral analytes and methanol water as binary mobile phase The applicable ranges of pH and stability of AOBP were also evaluated The results showed that AOBP has excellent chromatographic properties and resistance to hydrolysis between pH=2 5 7 5, It can be used for the separation of basic solutes efficiently