高效液相色谱中的手性两相协同作用

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0.60 mmol/

Chiral Two-Phase Synergistic Effect in High Performance Liquid Chromatography

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 degrees C, when beta-cyclodextrin (beta-CD), dimethyl-beta-cyclodextrin (DM-beta-CD) and trimethyl-beta-cyclodextrin (TM-beta-CD) were used as mobile phase additives. The results showed that TM-beta-CD at the concentrations higher than 0.60 mmol/L had an explicit chiral two-phase synergistic effect with chiral stationary phase, but beta-CD and DM-beta-CD at any concentrations and TM-beta-CD at low concentrations had no effect.