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将(葡聚糖-金刚烷-COOH)聚合物固定到β-环糊精修饰的二氧化硅上。

Immobilization of a (dextran-adamantane-COOH) polymer onto beta-cyclodextrin-modified silica.

作者信息

Karakasyan Carole, Millot Marie-Claude, Vidal-Madjar Claire

机构信息

Laboratoire de Recherche sur les Polymères, CNRS-Université Paris XII, 2 rue Henri Dunant, Thiais 94320, France.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2004 Aug 25;808(1):63-7. doi: 10.1016/j.jchromb.2004.05.025.

Abstract

Adamantane-modified compounds are known to form stable complexes with beta-cyclodextrins (beta-CD) by host-guest interactions. In this study, the inclusion complex formed between beta-CD cavities and the adamantane group was evaluated for the elaboration of a cation-exchange support. The synthesis of the chromatographic supports involved three steps: (i) a polymer of beta-CD was grafted to diol-modified silica, (ii) a dextran polymer was modified by both adamantane groups and ionizable COOH functions, (iii) the dextran derivative (Ad-Dex-COOH) was bound to the chromatographic support by complexation between the adamantane groups of the dextran and beta-CD cavities of the support. The polymer immobilization on the beta-CD support was successful as the resulting support exhibited weak cation-exchange properties. The stationary phase was easy to prepare under mild conditions (aqueous media, room temperature) and was quite stable when using aqueous mobile phases. The chromatographic behaviour of model proteins was studied in isocratic elution by examining the effect of salt concentration in the buffer on retention. A mixed retention mode was found for lysozyme, revealing both electrostatic and hydrophobic interactions with the stationary phase.

摘要

金刚烷修饰的化合物通过主客体相互作用与β-环糊精(β-CD)形成稳定的复合物。在本研究中,评估了β-CD空腔与金刚烷基团之间形成的包合物,以制备阳离子交换载体。色谱载体的合成涉及三个步骤:(i)将β-CD聚合物接枝到二醇修饰的硅胶上,(ii)用金刚烷基团和可离子化的COOH官能团修饰葡聚糖聚合物,(iii)通过葡聚糖的金刚烷基团与载体的β-CD空腔之间的络合作用,将葡聚糖衍生物(Ad-Dex-COOH)结合到色谱载体上。聚合物成功固定在β-CD载体上,因为所得载体表现出弱阳离子交换性能。固定相在温和条件下(水介质,室温)易于制备,并且在使用水性流动相时相当稳定。通过检查缓冲液中盐浓度对保留的影响,在等度洗脱中研究了模型蛋白的色谱行为。发现溶菌酶具有混合保留模式,揭示了与固定相的静电和疏水相互作用。

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