Effect of supermolecular structure of cellulosic materials on chiral discrimination

纤维素材料超分子结构对手性辨别的影响

基本信息

批准号：
14560130
负责人：
KASUYA Natsuki
金额：
$ 1.92万
依托单位：
National University Corporation Tokyo University of Agriculture and Technology
依托单位国家：
日本
项目类别：
Grant-in-Aid for Scientific Research (C)
财政年份：
2002
资助国家：
日本
起止时间：
2002 至 2003
项目状态：
已结题

来源：
https://kaken.nii.ac.jp/en/grant/KAKENHI-PROJECT-14560130/
关键词：
cellulose chiral HPLC structure キラル分離液晶性

项目摘要

Studies on the hysteretic effect of coating were investigated using cellulose triphenylcarbamate as a chiral separating phase of chiral support for HPLC. According to the previous paper by Shibata et al., the different kinds of coating solvent resulted in the different elution order of enantiomers with the use of cellulose acetate as a chiral separating phase. For further investigations of the relationship between coating solvents and chiral selecting polymers, we have selected the combination of cellulose trhiphenylcarbamate and its organic solvents reported to from alyotropic liquid crystal.Firstly, we have synthesized cellulose triphenylcarbamate according to the method of Schroeder and his coworker, dissolved it in the organic solvent such as methylpropylketone (MPK), diglyme, and e.t.c., and checked if the system forms a cholesteric liquid crystal. Because the resultant solution of cellulose derivative seemed to show a poor cholesteric nature, we repeated the synthetic reaction fo … More r the already derivatized cellulosic material and obtained typical cholesteric liquid crystals. Degree of polymerization could have changed during the repeated reaction. Cholesteric nature was recognized by observations using polarizing microscope, and the measurements of spectrum of UV, ORD.Then, the dilute solution (10wt%) of cellulose triphenylcarbamate either in MPK or in diglyme was poured onto porous silica gel (mean particle size 7 μm and mean pore diameters 100 nm), and the solvent was removed. The evaporation of the solvent was performed ether in a draft chamber for the MPK or in a vacuum oven at 30℃ for the diglyme, and the duration required for the evaporation was more than 1weeks for both solvents. After obtaining the chiral support, we prepared the laboratory-made columns for optical resolution by packing it into stain-less steel columns, and estimated their chiral recognizing ability.The chiral resolving column prepared by using MPK as a coating solvent showed a prominent resolving power and comparable to the commercial column in terms of resolution factors (α) and theoretical plate numbers, although the other column showed poor results due to the insufficient evaporation of the coating solvent. The order of elution for enantiomer was found to be the same among the tested colums. Less

根据Shibata等人的前一篇论文，使用纤维素三烯基培养基对纤维素分离的研究进行了研究。细胞钙化和IS或Ganic溶剂的组合是根据Alyotropic液体的结合，根据Schroeder及其同事的方法，我们将其溶解在有机甲基甲基酮（MPK）和E.T.C.如果是Acc. Acc. Acc. Acc. Acc.胆汁灰质的液体。将MPK中的细胞糖三烯基氨基盐倒入多孔二氧化硅（平均粒径为7μm，平均孔径为100 nm），然后除去溶剂，并去除溶剂的蒸发量。在30°C下的真空烤箱，对于两种溶剂，蒸发量超过1周。在分辨率因子（α）方面，明显的分辨率和与商业柱相媲美，Althooth的另一列显示出较差的结果，因为发现了对元素的元素的不足。在经过测试的柱中。