甘草酸单铵盐的制备及纯化新工艺研究

Study on new process for the production and purification of monoammoniun glycrrhizinate

考察了以甘草为原料,采用溶剂法制得甘草酸单铵盐,并利用工业乙醇和80%乙醇为重结晶溶剂对其精制纯化。通过对比实验,确定了新的溶剂法工艺条件为:热回流法提取的甘草酸,经工业乙醇浸提、浓氨水氨化,在酸化过程中,先加一定量冰乙酸调节pH到4.5,再加前述2倍量冰乙酸制得甘草酸单铵盐粗品,其含量达66.7%,得率为2.58%。获得了结晶精制纯化工艺为:经工业乙醇、80%的乙醇和工业乙醇对粗品交替重结晶三次,固液比分别为1:40、1:15和1:40,最终甘草酸单铵盐含量达80.1%,得率为1.36%。

Through solvent process, monoammoniun glycrrhizinate was gained from radix glycyrrhizae, and it was refined through recrystallization method using the solvent--industrial alcohol and 80% alcohol. The improve conditions of solvent process were found by the contrast experiment,they were glycrrhizin extracted hot reflux,and then digestioned by industrial alcohol, aminateed by stronger ammonia water, treated through first dropwise a certain quality of glacial acetic acid into triammonium glycyrrhizinate at pH 4.5 and then dropwise 2. times of glacial acetic acid mentioned earlier, purity and yield of crude monoammoniun glycrrhizinate were 63.3% and 2.58%. Following the optimum conditions, recrystallization were tested,they were treated by recrystaled in sequence of industrial alcohol,80% alcohol and industrial alcohol with solid-to-liqid ratio of 1：40, 1：15, 1：40 for crude monoammoniun glycrrhizinate, purity and yield of monoammoniun glycrrhizinate were 80.1% and 1.36% after all.