连续离子交换色谱分离甘草酸和甘草黄酮
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摘要
以甘草酸和甘草黄酮的吸附率及解析率为指标,探究了6种树脂对二者吸附和解析性能,筛选了最佳分离树脂。考察了影响二者分离效果的条件,确定了连续离子交换色谱分离二者的最佳工艺。结果表明,D941是分离甘草酸和甘草黄酮的最佳树脂。最佳分离工艺为:上样质量浓度1.0mg/mL,体积2.70L,体积流量12.5mL/min;乙醇洗脱体积分数70%,体积1.80L,体积流量12.50mL/min;NaOH洗脱浓度0.50mol/L,体积0.6L,体积流量5.0mL/min。在最佳工艺条件下制得甘草酸纯度为76.53%,得率2.09%;甘草黄酮纯度为67.33%,得率2.68%。结果说明连续离子交换色谱可以实现甘草酸与甘草黄酮的同时分离,提高生产效率。
With the adsorption and desorption rates of glycyrrhizic acid(GA)and licorice flavonoids(LF)as indicators,the adsorption and desorption properties of six resins were investigated,and the optimum separation resin was selected.The parameters affecting the separation efficiency were investigated,and the optimum process for separation of the two compounds by continuous ion exchange chromatography(CIEC)were determined.The result showed that D941 was the best resin for separating GA and LF. The optimum separation processes of continuous ion exchange chromatography are as follows:the mass concentration of sample of 1.0mg/mL,volume of 2.70 L,volume flow of 12.5 mL/min;the volume fraction of ethanol elution of 70%,volume of 1.80 L,volume flow of 12.50mL/min;NaOH elution concentration of 0.50mol/L,volume of 0.6L,volume flow of 5.0mL/min.Under the optimum conditions,GA was obtained with purity of 76.53% and yield of 2.09%,while LF was obtained with purity of 67.33% and yield of 2.68%.The results indicated that CIEC can separate GA and LF simultaneously and improve production efficiency.
With the adsorption and desorption rates of glycyrrhizic acid(GA)and licorice flavonoids(LF)as indicators,the adsorption and desorption properties of six resins were investigated,and the optimum separation resin was selected.The parameters affecting the separation efficiency were investigated,and the optimum process for separation of the two compounds by continuous ion exchange chromatography(CIEC)were determined.The result showed that D941 was the best resin for separating GA and LF. The optimum separation processes of continuous ion exchange chromatography are as follows:the mass concentration of sample of 1.0mg/mL,volume of 2.70 L,volume flow of 12.5 mL/min;the volume fraction of ethanol elution of 70%,volume of 1.80 L,volume flow of 12.50mL/min;NaOH elution concentration of 0.50mol/L,volume of 0.6L,volume flow of 5.0mL/min.Under the optimum conditions,GA was obtained with purity of 76.53% and yield of 2.09%,while LF was obtained with purity of 67.33% and yield of 2.68%.The results indicated that CIEC can separate GA and LF simultaneously and improve production efficiency.
引文
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[11]李晖,卢定强,肖洁瑾,等.335弱碱性阴离子交换树脂对甘草酸的吸附过程[J].生物加工过程,2006,4(4):46-50.
[2]CURRELI F,FRIEDMAN-KIEN A E,FLORE O.Glycyrrhizic acid alters Kaposi sarcoma-associated herpesvirus latency,triggering p53-mediated apoptosis in transformed B lymphocytes[J].The Journal of Clinical Investigation,2005,115(3):642-652.
[3]李宏智.甘草查尔酮类化合物的制备及体外抗宫颈癌活性研究[D].乌鲁木齐:新疆医科大学,2010.
[4]王芸芸,刘利军.超滤膜技术用于甘草总黄酮的分离纯化[J].化学研究与应用,2012,24(4):646-649.
[5]郑云枫,杨锦强,魏娟花,等.多指标测定优化聚酰胺树脂分离甘草黄酮的工艺[J].中国中药杂志,2013,38(22):3902-3906.
[6]CHARPE T W,RATHOD V K.Separation of glycyrrhizic acid from licorice root extract using macroporous resin[J].Food and Bioproducts Processing,2015,93:51-57.
[7]袁延强,王祖林,刘秀河,等.高速逆流色谱分离制备甘草中的甘草黄酮和芒柄花苷[J].天然产物研究与开发,2011,23(6):1148-1150.
[8]何秀娟.溶剂萃取耦合大孔吸附树脂纯化甘草酸[D].石河子:石河子大学,2013.
[9]赵黎明,黄阿根.食品工程原理[M].北京:中国纺织出版社,2013.
[10]李洪飞,李良玉,张丽萍,等.模拟移动床色谱技术应用的研究进展[J].农产品加工学刊,2011(5):62-65.
[11]李晖,卢定强,肖洁瑾,等.335弱碱性阴离子交换树脂对甘草酸的吸附过程[J].生物加工过程,2006,4(4):46-50.