大孔吸附树脂吸附法结合氯仿溶解法分离混合二元酸

建立利用大孔吸附树脂吸附法结合氯仿溶解法分离混合二元酸中丁二酸、戊二酸和己二酸的方法并使其分别达到一定的纯度和收率。首先利用LC-ESI-MS方法测定了混合二元酸中丁二酸、戊二酸和己二酸含量,然后通过对3种大孔吸附树脂AB-8、NKA-Ⅱ和D-380吸附性能的综合比较,筛选出AB-8大孔吸附树脂作为吸附剂,以水、10%、30%和95%乙醇水溶液作为洗脱剂对混合二元酸进行初步的分离,得到A、B、C和D4个分离部位,再利用氯仿对二元酸溶解度的不同,将该4个分离部位在55℃水浴恒温分别用氯仿进行溶解、过滤,通过LC-ESI-MS方法测定确定相应部位的组成情况后进行适当合并,最终达到将混合二元酸分离的目的。丁二酸纯度:70.3%,收率:92.7%;戊二酸纯度:94.1%,收率89.2%;己二酸纯度:90.7%,收率:88.7%。

Separation of Admixture of Biprotic Acid by Method of Macroporous Adsorptive Resins and Dissolving of Chloroform

A method for separating admixture of biprotic acid by macroporous adsorptive resins and the dissolving of chloroform was established.First,the contents of butane diacid,pentane diacid and adipic acid in admixture of biprotic acid were determined by LC-ESI-MS.Then the adsorption performances of macroporous adsorptive resins AB-8,NKA-Ⅱ and D-380 were compared,and AB-8 macroporous adsorptive resins was determined as the sorbent.And then water,10%,30% and 95% ethanol were used as the eluent to isolate admixture of biprotic acid preliminarily,four parts （A,B,C and D） were obtained.Because the solubilities of butane diacid,pentane diacid and adipic acid in CHCl3 were different,the four free parts A,B,C and D were threw into quantitative CHCl3 solution with constant temperature of 55℃ respectively to obtain some parts ,the parts were incorporated properly through analysis and comparison to complete the isolation of admixture of biprotic acid.The purity quotient of butane diacid is 70.3% and the recovery rate is 92.7%.The purity quotient of pentane diacid is 94.1% and the recovery rate is 89.2%.The purity quotient of adipic acid is 90.7% and the recovery rate is 88.7%.