基于壳聚糖-3,6-二(苯基氨基甲酸酯)-2-(苄基脲)手性固定相的制备及其分离性能  

Preparation and Separation Performance of Chiral Stationary Phases Based on Chitosan-3,6-Bis (phenylcarbamate)-2-(benzylurea)

作　　者：蔡明兰 熊金辉 郝菊芳[2] 何保江[3] 柏正武 CAI Minglan;XIONG Jinhui;HAO Jufang;HE Baojiang;BAI Zhengwu(School of Chemistry and Environmental Engineering,Wuhan Institute of Technology,Wuhan 430205;Staff Development Institute of China National Tobacco Corporation,Zhengzhou 450008;Zhengzhou Tobacco Research Institute of China National Tobacco Corporation,Zhengzhou 450001)

机构地区：[1]武汉工程大学化学与环境工程学院,湖北武汉430205 [2]中国烟草总公司职工进修学院,河南郑州450008 [3]中国烟草总公司郑州烟草研究院,河南郑州450001

出　　处：《分析科学学报》2020年第6期795-800,共6页Journal of Analytical Science

基　　金：国家自然科学基金(No.51373127)。

摘　　要：为研制手性识别能力强且对流动相耐受性能好的多糖衍生物手性固定相,制备了壳聚糖苄基脲,再用4-甲基苯基异氰酸酯和4-氯苯基异氰酸酯修饰壳聚糖苄基脲上的羟基,得到两种手性选择体,以红外光谱和核磁共振谱对其结构进行了表征。将这两种手性选择体涂敷在大孔氨丙基硅胶表面制备成相应的手性固定相,以17种手性化合物为分析物,用高效液相色谱法评价了这两种手性固定相的分离性能。结果显示含甲基和含氯的固定相分别识别了14和15种手性分析物的对映体,均基线分离了其中的8种,而含甲基的固定相对手性分析物有更大的分离度。The goal of this study was to develop polysaccharide-type chiral stationary phases(CSPs) with high chiral recognition ability and high tolerability towards mobile phases.Hence,chitosan benzylurea was prepared and modified with 4-methylphenyl and 4-chlorophenyl isocyanates to obtain two chiral selectors(CSs).The CSs were characterized by IR and ~1H NMR,and coated on macroporous 3-aminopropyl silica gel to provide corresponding CSPs.The enantioseparation ability of the CSPs was evaluated by high-performance liquid chromatography with 17 chiral compounds.The results showed that the CSP containing methyl group and the one containing chloro group,respectively,recognized the enantiomers of 14 and 15 analytes,and the both baseline separated 8 analytes.Meanwhile,the CSP with methyl group showed higher resolution towards chiral analytes.

关 键 词：壳聚糖 手性选择体 手性固定相 对映体分离 高效液相色谱 

分 类 号：O658[理学—分析化学]