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目的建立手性液-液萃取拆分普罗帕酮对映体的方法,探讨液-液平衡手性萃取拆分中的相关理论。方法考察有机溶剂,手性试剂,L-酒石酸正丁酯浓度,水相pH值,硼酸浓度等因素对手性萃取拆分的影响。结果优化的萃取拆分条件:以含0.1 mol·L-1硼酸的0.05 mol·L-1醋酸-三乙胺缓冲溶液(pH 3.4)为水相,含0.1 mol·L-1L-酒石酸正丁酯的氯仿溶液为有机相,平衡温度10℃,样品浓度1 mmol·L-1;确定了普罗帕酮对映体与硼酸及酒石酸酯形成的络合物比例为1∶1∶2。结论在最优化条件下,得到分布系数D-=0.175,D+=0.261,对映体分离因子α=1.495。
OBJECTIVE To establish a method for the resolution of propafenone enantiomers by liquid-liquid extraction and to explore the related theories in liquid-liquid equilibrium chiral extraction. Methods The effects of organic solvents, chiral reagents, the concentration of n-butyl L-tartrate, the pH value of aqueous phase and the concentration of boric acid on the resolution of chiral extraction were investigated. Results The optimum conditions of extraction and separation were: 0.05 mol·L-1 acetic acid-triethylamine buffer solution (pH 3.4) containing 0.1 mol·L-1 boric acid as the aqueous phase and 0.1 mol·L-1 L-t- The chloroform solution of the ester was an organic phase with an equilibrium temperature of 10 ° C and a concentration of 1 mmol·L-1. The ratio of propafenone enantiomer to boric acid and tartrate was determined to be 1: 1: 2. Conclusion Under the optimal conditions, the distribution coefficient D = 0.175, D + = 0.261 and the enantiomeric separation factor α = 1.495 were obtained.