钡盐法从二氯苯磺酸-亮氨酸复合物制备亮氨酸的研究

Preparation of Leucine from the Dichlorobenzenesulfonic Acid-leucine Complex by Barium Salt Method

二氯苯磺酸可选择性地从毛发水解液中沉淀亮氨酸,得到二氯苯磺酸-亮氨酸复合物。本文研究了二氯苯磺酸-亮氨酸复合物提纯的方法及二氯苯磺酸与亮氨酸分离的方法,最终得到符合质量要求的亮氨酸产品。实验结果表明,采用水中重结晶法可大幅度提高二氯苯磺酸-亮氨酸复合物的纯度;复合物中亮氨酸占氨基酸总量的比例由粗品的49.0%提高到94.8%。Ba 2+可与二氯苯磺酸结合生成二氯苯磺酸钡沉淀,采用钡盐脱除二氯苯磺酸沉淀剂法方法简单,脱除沉淀剂的效果较好,脱除率达92.2%;亮氨酸产品质量达到美国药典(USP34)标准,产品收率为4.1%。二氯苯磺酸沉淀剂容易再生,再生回收率不低于97%。

Dichlorobenzenesulfonic acid selectively precipitates leucine from the hair hydrolysate to give a dichlorobenzenesulfonic acid-leucine complex.In this paper,the purification method of dichlorobenzenesulfonic acid-leucine complex and the separation method of dichlorobenzenesulfonic acid and leucine were studied,and finally the leucine product meeting the quality requirements was obtained.The experimental results show that the purity of the dichlorobenzenesulfonic acid-leucine complex can be greatly improved by the recrystallization method in water;the ratio of leucine to the total amino acid in the complex is increased from 49.0%of the crude product to 94.8%.Ba 2+can be combined with dichlorobenzenesulfonic acid to form barium dichlorobenzenesulfonate precipitate.The method for removing dichlorobenzenesulfonic acid precipitant by using barium salt is simple,and the effect of removing precipitant is good with the removal rate at 92.2%;The quality of the leucine product reached the United States Pharmacopoeia(USP34)standard and the product yield was 4.1%.The dichlorobenzenesulfonic acid precipitant is easily regenerated,and the recovery recovery rate is not less than 97%.