A facile and efficient one-step strategy for the preparation of β-cyclodextrin monoliths.
A facile and efficient one-step strategy for the preparation of β-cyclodextrin monoliths.
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DOI：
10.1002/jssc.201300374
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发表时间：
2013-08
影响因子：
3.1
通讯作者：
Jialiang Guo;Qiaoxuan Zhang;Yongbo Peng;Zhenghua Liu;Longyi Rao;Teng He;J. Crommen;Pinghua Sun;Zhengjin Jiang
中科院分区：
文献类型：
--
作者：
Jialiang Guo;Qiaoxuan Zhang;Yongbo Peng;Zhenghua Liu;Longyi Rao;Teng He;J. Crommen;Pinghua Sun;Zhengjin Jiang
研究了一种新型、简便、高效的一步共聚方法，用于制备β-环糊精（β-CD）甲基丙烯酸酯整体柱。通过甲基丙烯酸丙酯与单6-叠氮-β- cd的连锁反应合成了新型单体（1h -1,2,3-三唑-4-甲基）-2-甲基丙烯基-β- cd，然后将单体（1h -1,2,3-三唑-4-甲基甲基）-2-甲基丙烯基-β- cd与二甲基丙烯酸乙酯一步原位共聚制备了整体柱。采用元素分析、扫描电镜（SEM）和微高效液相色谱（hplc）对制备的整体柱的理化性质和柱性能进行了表征。优化后的聚单-（1h -1,2,3-三唑-4-甲基甲基）-2-甲基丙烯酸基-β- cd -二甲基丙烯酸乙酯)整体柱的柱透性、效率和分离性能均较好。此外，在高乙腈含量的流动相中，观察到典型的亲水相互作用色谱保留行为。虽然我们的整体柱的对映体选择性没有达到其他报道的β-CD整体柱的水平，但这种基于点击化学的一步策略仍然提供了一个有趣而有效的模型，因为它提供了通过一步共聚策略轻松制备相关新型甲基丙烯酸镉单体的可能性。
A novel, facile, and efficient one-step copolymerization strategy was developed for the preparation of β-cyclodextrin (β-CD) methacrylate monolithic columns using click chemistry. The novel mono-(1H-1,2,3-triazol-4-ylmethyl)-2-methylacryl-β-CD monomer was synthesized by a click reaction between propargyl methacrylate and mono-6-azido-β-CD, and then monolithic columns were prepared through a one-step in situ copolymerization of the mono-(1H-1,2,3-triazol-4-ylmethyl)-2-methylacryl-β-CD monomer and ethylene dimethacrylate. The physicochemical properties and column performance of the fabricated monolithic columns were characterized by elemental analysis, SEM, and micro-HPLC. Satisfactory column permeability, efficiency, and separation performance were obtained for the optimized poly(mono-(1H-1,2,3-triazol-4-ylmethyl)-2-methylacryl-β-CD-co-ethylene dimethacrylate) monolithic columns. Additionally, typical hydrophilic interaction chromatography retention behavior was observed on the monoliths at high acetonitrile content in the mobile phase. Although the enantioselectivity of our monolithic columns did not meet the level of other reported β-CD monolithic columns, this one-step strategy based on click chemistry still provides an interesting and effective model as it offers the possibility to easily prepare related novel CD methacrylate monoliths through a one-step copolymerization strategy.