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作 者:李来生[1] 刘旭[1] 黄志兵[1] 葛小辉[1] 李艳平[1]
出 处:《南昌大学学报(理科版)》2005年第4期353-357,362,共6页Journal of Nanchang University(Natural Science)
基 金:江西省教委基金资助项目(JJ2003-73-16);江西省自然科学基金资助项目(9920024)
摘 要:采用固液相连续反应,以N-(β-氨乙基)-γ-氨丙基甲基二甲氧基硅烷和γ-(环氧丙氧基)丙基三甲氧基硅烷为偶联剂,分别制备了二硝基苯甲酰胺基(DNB)、喹啉醚基(QBS)和联萘酚醚基(DNP)三种芳基键合硅胶固定相。采用元素分析、红外光谱和热分析表征了固定相的结构,并用于磺胺类药物的分离,较系统地研究了磺胺类药物在三种芳基键合固定相上的色谱行为,探讨了色谱分离机理。研究表明,三种新固定相与上述溶质间存在弱的疏水、π-π、氢键和络合作用,与ODS柱相比,多分离机制改变了芳基固定相的色谱分离选择性,其中大的芳基配体在分离磺胺类药物时具有优势。The solid-liquid reaction method was used for the preparation of HPLC aryl-bonded silica gel stationary phases, including 3,5-dinitrobenzyl ( DNB ), quinolinyl ether (QBS) and 1,1 '-di (2 - naphthol ) ether (DNP) bonded silica gel stationary phases by using N-(β-aminoethyl)-γ-aminopropylmethyldimethoxy silane and 3 -glycidoxypropyl trimethoxylsilane as coupling reagents, respectively. Their structures were characterized by elemental analysis, diffuse reflectance infared fourier transform spectroscopy and thermal analysis. The new bonded phases were employed in the separation of sulfonamides. The chromatographic behaviors of sulfonamides on three kinds of aryl-bonded silica gel stationary phases were systematically studied. The chromatographic separation mechanism was proposed. The results show that various interactions occur between the analytes and the bonded phases, such as hydrophobic, π - π, hydrogen-bonding and complex interactions, which are different from those on ODS. The interactions improve the selectivity of aryl-bonded phases for sulfonamides. The big aryl ligand has advantage over the others in the separation of suifonamides.
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