模拟移动床色谱分离甘草苷和甘草素  

Separation of Liquiritin and Liquiritigenin by Simulated Moving Bed Chromatography

作　　者：王绍艳[1] 魏伯峰[1] 丛景香[1] 梁悦 

机构地区：[1]辽宁科技大学化学工程学院,辽宁鞍山114051

出　　处：《精细化工》2017年第11期1260-1264,共5页Fine Chemicals

基　　金：国家自然科学基金(21576127);高等学校博士学科点专项科研基金(20132120110002);鞍山市科委基金(3126)~~

摘　　要：以十八烷基硅烷键合硅胶(ODS)为固定相,V(乙醇)∶V(水)=30∶70为流动相的模拟移动床色谱(SMBC)体系对甘草黄酮中甘草苷与甘草素进行连续分离。SMBC体系设置洗脱带Ⅰ:1根色谱柱;精制带Ⅱ:2根色谱柱;吸附带Ⅲ:2根色谱柱,Ⅰ带独立,Ⅰ带洗脱液为乙醇。按照理想三角形理论选择SMBC操作参数,操作参数包括流动相流速、进料液流速和切换时间。结果表明:接近三角形底边选择SMBC的操作条件,在萃余液出口得到甘草苷,HPLC纯度高于70.44%,收率高于95.17%,同时在萃取液出口得到甘草素,HPLC纯度高于73.10%,收率高于90.74%,SMBC能有效分离甘草苷和甘草素。甘草苷萃余液和甘草素萃取液分别经浓缩、重结晶后,两种产品HPLC纯度均超过96%。Liquiritin and liquiritigenin were continuously separated from liquorice flavonoids by simulated moving bed chromatography（SMBC） with ostade-cylsilane（ODS） as stationary phase and a mixture of ethanol and water（30/70,v/v） as mobile phase.The SMBC system contained three zones including the independent eluting zone Ⅰ with one column,the refining zone Ⅱ with two columns and the adsorbing zone Ⅲ with two columns,wherein,the mobile phase of zone Ⅰ was ethanol.The SMBC operating parameters,such as the flow rate of mobile phase,the flow rate of feeding solution and the switching time,were chosen according to ideal triangle theory.When the separation was carried out under the experiment points along the bottom margin of the triangle,the purity（70.44%） of liquiritin from raffinate was checked by HPLC and the recovery of liquiritin was over 95.17%.Meanwhile,the purity and recovery of liquiritigenin from extract were over 73.10% and 90.74%,respectively.The results indicate that it is efficient to separate liquiritin and liquiritigenin in liquorice flavonoids by SMBC.After the raffinate and extract from SMBC were concentrated and recrystallized,eventually over 96% purities of both liquiritin and liquiritigenin were obtained.

关 键 词：分离 模拟移动床色谱 甘草苷 甘草素 甘草黄酮 中药现代化技术 

分 类 号：TQ041.8[化学工程]