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十六烷基三甲基溴化铵在硅胶基HPLC介孔分离介质制备中的应用

     

摘要

在阳离子表面活性剂十六烷基三甲基溴化铵(CTAB)存在下,以3-氨丙基三乙氧基硅烷(APTES)和正硅酸乙酯(TEOS)为硅源,氨水调节溶液pH,制得了硅胶基HPLC介孔分离介质,并通过FTIR,SEM和氮气物理吸附-脱附等手段对所得产物进行了表征,考察了表面活性剂用量对材料结构的影响.结果表明,制备的材料在硅胶骨架中引入了氨基,粒径为0.5~2 μm,孔径为3.8~6.7 nm;以制备的分离材料装柱,用于混合后的4种有机化合物的分离,液相色谱分离结果表明,在6 min内实现了样品中各组分的基线分离,有较好的识别能力.%Starting from 3 -aminopropyl triethoxysilane (APTES) and tetraethyl orthosilicate (TEOS) as the silica sources, and using ammonia to regulate the pH of the reaction solution, silica based mesoporous separation medium for HPLC was synthesized in the presence of cetyltrimethylammonium bromide ( CTAB). The synthesized material was characterized by FTIR, SEM and nitrogen adsorption - desorption measurement. Results indicated that amino - group has been introduced in silica gel skeleton, whose particle size is around 0. 5 ~2 |im,and pore diameter is around 3. 8 ~6. 7 nm. The synthesized material was used to fill the HPLC column for separation of a mixed sample composed of 4 kinds of organic compound; and the results of HPLC analysis showed that the synthesized material displays good recognition capacity. The baseline separation of components in the mixed sample achieves within 6 min.

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