天然产物研究与开发 ›› 2016, Vol. 28 ›› Issue (7): 1093-1101.doi: 10.16333/j.1001-6880.2016.7.019

• 开发研究 • 上一篇    下一篇

设计柱层析过程从兴安落叶松锯末中分离纯化花旗松素

刘婷婷,袁其朋*   

  1. 北京化工大学生命科学与技术学院化工资源有效利用重点实验,北京 100029
  • 出版日期:2016-07-30 发布日期:2017-01-17

Separation and Purification of Taxifolin from Larix gmelini Sawdust Using Process Planning of Column Chromatography

LIU Ting-ting,YUAN Qi-peng*   

  1. State Key Laboratory of Chemical Resource Engineering,College of Life Science and Technology,Beijing University of Chemical Technology,Beijing 100029,China
  • Online:2016-07-30 Published:2017-01-17

摘要: 以兴安落叶松锯末为主要提取原料,柱层析为基础单元建立了花旗松素的制备工艺。分别以分离和纯化为目的,工艺中联用了AB-8型大孔树脂柱层析及制备色谱两个单元。大孔树脂动态吸附中,上样液中花旗松素的浓度0.5 mg/mL;流速为4 BV/h;上样体积为169 mL;床层的径高比为1/10。洗脱过程中,用5 BV去离子水清洗柱子后,用体积比为20%乙醇水溶液洗脱含有花旗松素的分离产品。洗脱过程中,在流速为3 BV/h条件下,收集8 BV的洗脱液。经过分离,花旗松素的纯度从6.0%提升至56.75%,该步骤的回收率为88.71%。含有40 mg花旗松素的分离产品经旋蒸干后,溶解于10 mL体积比为35%的甲醇水溶液中作为制备色谱单元中的上样液。该步骤中,在洗脱流速为8 mL/min条件下,收集得到纯度为95.02%的花旗松素。控制收集时间为33.0~40.5 min,花旗松素的纯度可以被进一步提高到98.02%,并通过NMR确证其结构。在整个研究中,过程设计的思想引入了两个柱单元的操作条件筛选中,结果表明了工艺中确定的操作条件是最优的。

关键词: 柱层析过程, 兴安落叶松锯末, 分离, 纯化, 花旗松素

Abstract: In this study, Larix gmelini sawdust was used as raw material for the purification of taxfolin with column process as the basic unit.With separation and purification as the purposes of the two units arranged in present technology,respectively,the column packed with AB-8 macroporous adsorption resins(MARs)and the preparative high performance liquid chromatography(prep-HPLC)were combined together.In the dynamic experiments carried out on AB-8 MARs column,the concentration of taxifolin contained in the sample solution was 0.5 mg/mL;the flow rate was 4 BV/h;the volume of the sample solutions was 169 mL,and the ratio of the diameter of the bed to the length of the bed was 1/10.In the eluting process,the flow rate was set at 3 BV/h.Five BV of deionized water was used for washing the adsorption column firstly.Then,8 BV of 20%(volume concentration)aqueous ethanol was used for eluting the separated products containing taxifolin.Through separation,the purity of taxifolin products was improved from 6.0% to 56.78%,with recovery of 88.71%.After being dried by the rotary evaporator,the separating products,in which the amount of taxifolin was 40 mg,were re-dissolved into 10 mL of 35%(volume concentration)aqeous ethanol to prepare the solutions for prep-HPLC unit.In this step,the eluting rate was 8 mL/min.The purity of taxifolin collected in this step was 95.02%.Setting the collection time range from 33.00 min to 40.50 min in the above method,the purity of taxifolin was further improved to 98.02%.

Key words: column process, Larix gmelini sawdust;separation;purification;taxifolin

中图分类号: 

TQ423