酸解法制取甘草次酸及其纯化工艺

以甘草酸单铵盐为原料,酸解制取甘草次酸并利用低温冷析法对其进行精制纯化.通过L9(34)正交试验,确定了酸解甘草次酸的最佳条件:H2SO4体积分数8％、料液比(g/mL)1:100、温度100℃、12 h,在此条件下,转化率可达80.24％:通过对比实验,获得了低温冷析法精制甘草次酸的纯化工艺:酸解产物经水洗、氯仿溶提后,在体积分数30％乙醇溶液中80℃热溶15 min,再在冰水中冷析10 min,最终得到甘草次酸的质量分数为95.79％,得率40.87％.

Separation and purification of glycyrrhetinic acid by acid hydrolysis of monoammoniun glycrrhizinate

Through acid hydrolysis of monoammoniun glycrrhizinate, glycyrrhetinic acid was obtained, and refined by low temperature crystallization in alcohol water. The optimum acid hydrolysis conditions found by the orthogonal design with three levels and four factors were as follows： 8% sulphuric acid, temperature 100 ℃, reflux for 12 h, solid-to-liquid ratio （g/mL） 1： 100; and the conversion was 80. 24%. The crude glycyrrhetinic acid was washed by water and extracted by hot chloroform, dried, dissolved in hot 30% alcohol at 80 ℃ for 15 min, and then crystallized in ice water for 10 min, the purity and the yield of glycyrrhetinic acid were 95.79% and 40. 87% , respectively.