高效液相色谱中的手性两相协同作用  

Chiral Two-Phase Synergistic Effect in High Performance Liquid Chromatography

作　　者：孟磊[1] 李方楼[2] 袁黎明[2] 

机构地区：[1]河南农业大学基础科学院,河南郑州450002 [2]云南师范大学化学化工学院,云南昆明650092

出　　处：《色谱》2004年第2期124-127,共4页Chinese Journal of Chromatography

基　　金：国家自然科学基金资助项目(批准号:30160092).

摘　　要：在高效液相色谱中,以纤维素三苯基甲酸酯、纤维素三苯基氨基甲酸酯为手性固定相,以正己烷 异丙醇(体积比为9∶1)为流动相,柱温25℃,分别以β 环糊精(β CD)、2,6 二甲基 β 环糊精(DM β CD)、2,3,6 三甲基 β 环糊精(TM β CD)为流动相添加剂,分离了DL 色氨酸和DL 苯丙氨酸两种手性化合物,考察是否存在手性固定相和手性添加剂的协同作用。实验结果表明,在流动相中添加β CD或DM β CD至饱和,协同作用不明显;在流动相中添加少量TM β CD(即浓度小于0.60mmol/L)时,分离促进作用不明显;当TM β CD浓度高于0.60mmol/L时,手性两相协同作用明显;表明在一定浓度条件下TM β CD与两种固定相存在明显的手性两相协同作用。Cellulose tribenzoate (CTB) and cellulose triphenylcarbamate (CTPC) were synthesized for the coating of high performance liquid chromatographic stationary phases. Elemental analysis and IR spectra indicated that most of the hydroxy groups of the microcrystalline cellulose had been converted into ester groups. The silanized gel was coated with CTB/CTPC by (using) tetrahydrofuran as solvent. The enantiomeric resolutions of phenylalanine (flow rate: 0.5 mL/min) and tryptophan were carried out with a hexane/2-propanol (9∶1,v/v) mixture at 25 (℃,) when β-cyclodextrin(β-CD), dimethyl - β-cyclodextrin (DM-β-CD) and trimethyl-β-cyclodextrin (TM-β-CD) were used as mobile phase additives. The results showed that TM-β-CD at the concentrations higher than 0.60 mmol/L had an explicit chiral two-phase synergistic effect with chiral stationary phase, but β-CD and DM-β-CD at any concentrations and TM-β-CD at low concentrations had no effect.

关 键 词：高效液相色谱 手性固定相 手性流动相添加剂 手性两相协同作用 纤维素衍生物 Β-环糊精衍生物 

分 类 号：O658[理学—分析化学] O657.72[理学—化学]