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运用Cu(I)催化的1,3-偶极环加成反应(点击化学),以乙酸酐修饰单叠氮环糊精为底层,炔基衍生的天然环糊精为顶层,在硅胶表面通过自下而上的方式构建了一种新型“天然-乙酰基衍生化”三唑桥联杂化复式环糊精手性固定相材料(ANCDCSP),并通过红外光谱、热重和元素分析等测试手段对其结构进行了表征.该固定相材料可提供包合作用、氢键给体、氢键受体、偶极-偶极作用等多重识别位点以及底层和顶层环糊精间的协同效应.在HPLC反相分离模式下,该固定相材料对10种丹磺酰氨基酸类(Dns amino acids)、10种小分子芳香酸(phenyl carboxylic acids)、5种异噁唑啉类(isoxazolines)以及多种其它手性对映体具有良好的手性拆分效果.其中Dns-Phe、DL-3Ph Lac A以及Bendroflumethiazide的分离度分别达到5.3、4.1和4.1,且多数手性对映体的分离度优于课题组先前制备的复式天然环糊精手性固定相(DCDCSP).
Using Cu (I) -catalyzed 1,3-dipolar cycloaddition reaction (click chemistry), acetic anhydride modified single azido cyclodextrin as the bottom, alkynyl-derived natural cyclodextrin as the top layer on the silica gel surface by A new type of “natural-acetyl derivatization” triazole bridged hybrid cyclodextrin chiral stationary phase material (ANCDCSP) was constructed in a bottom-up manner and characterized by IR, TG and elemental analysis And other test methods to characterize the structure of the stationary phase material can provide inclusions, hydrogen bond donor, hydrogen bond acceptors, dipole-dipole interaction and other multiple recognition sites and between the bottom and top cyclodextrin Synergetic effect.Under HPLC reversed-phase separation mode, this stationary phase material is sensitive to 10 kinds of Dns amino acids, 10 kinds of small-molecule phenyl carboxylic acids, 5 kinds of isoxazolines ), As well as many other chiral enantiomers with resolution of Dns-Phe, DL-3Ph Lac A and Bendroflumethiazide of 5.3, 4.1 and 4.1, respectively, and most of the chiral enantiomers The separation is superior to the compound cyclodextrin chiral stationary phase previously prepared by the research group (DCDCSP ).