新型L-羟脯氨酸聚合物键合手性固定相的制备及对手性化合物的拆分  

Preparation of Polymer-bonded Chiral Ligand Exchange Chromatographic Stationary Phase and Resolution of Racemates

作　　者：马桂娟[1] 龚波林[1] 阎超 

机构地区：[1]宁夏大学能源化工重点实验室,银川750021 [2]上海通微分析技术有限公司,上海201203

出　　处：《分析化学》2008年第3期275-279,共5页Chinese Journal of Analytical Chemistry

基　　金：科技部国际科技合作重点项目(No.2006DFA3690);教育部新世纪优秀人才支持计划(No.NCET-04-0986);上海市博士后科研基金(No.06R214202)资助

摘　　要：以单分散亲水性交联聚甲基丙烯酸环氧丙酯-甲基丙烯酸乙二醇双酯(PGMA/EDMA)树脂为载体,制备新型L-羟脯氨酸聚合物键合高效手性配体交换固定相。该固定相在配体交换分离模式下,以0.2mol/LNaAc和0.1mmol/LCu(Ac)2水溶液(pH5.2)为流动相,柱温为30℃～50℃,对衍生和非衍生的D,L-氨基酸和α-羟基酸等9种手性化合物进行了高效液相色谱拆分。详细考察了流动相pH值、温度、流速和进样量对手性分离的影响,选择了合适的色谱分离条件。结果表明,所拆分的9种手性化合物,有5种手性化合物能得到基线分离,最好的分离因子α=2.32。A new stationary phase was synthesized for chiral-ligand-exchange chromatography by treating the monodisperse poly （ glycidylmethacrylate-co-ethylenedimethacrylate ） particles with L-hydroxyproline. The enantiomeric resolutions of some D,L-amino acids and α-hydroxy acids were achieved on the synthesized chiral ligand exchange chromatographic stationary phase using 0.2 mol/L NaAc and 0.1 mmol/L Cu（Ac） 2 solution pH 5, 2 as mobile phase, 30℃ and 50℃ as the column temperature. The influence of the mobile phase pH,temperature of column, flow rate of eluent and sample concentration on the resolution of D,L-amino acids by ligand exchange chromatography were investigated. The results showed that five of the nine enantiomers could be separated from baseline and the best value of enantioselectivity（α） was 2.32.

关 键 词：手性配体交换色谱固定相 单分散树脂 L-羟脯氨酸 对映体分离 

分 类 号：O657.7[理学—分析化学]