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第 36 卷第 4 期                             精   细   化   工                                  Vol.36, No.4
             201 9 年 4 月                             FINE CHEMICALS                                 Apr.    2019


              中药现代化技术
                            大孔吸附树脂纯化东北岩高兰总黄酮



                                                                                       *
                                 刘晓燕,李   凤,李爱峰,孙爱玲,柳仁民
                                        (聊城大学  化学化工学院,山东  聊城    252059)


                 摘要:依据东北岩高兰总黄酮的吸附和解吸能力,采用静态吸附和解吸实验对 8 种型号的大孔吸附树脂进行筛选。
                 结果显示,AB-8 型大孔吸附树脂对东北岩高兰总黄酮具有较好的吸附和解吸性能。经 HPLC 分析提取出的东北岩
                 高兰主要有 5 种成分。进一步探究了总黄酮的纯化工艺,得到 5 种成分的最佳静态吸附解吸条件为:吸附平衡时
                 间 1.0 h,解吸溶剂为体积分数 95%的乙醇,解吸平衡时间 1.5 h。不同温度(25、30、35 ℃)下,AB-8 型大孔吸
                 附树脂对东北岩高兰不同成分的吸附等温线均符合 Freundlich 模型和 Langmuir 模型。5 种成分的最佳动态吸附洗
                 脱工艺条件为:上样液质量浓度为 5 g/L,最大上样量  400 mL,5 倍柱体积(BV)的体积分数为 20%的乙醇洗脱
                 杂质,5 倍 BV 的体积分数为 95%的乙醇洗脱成分,洗脱流速 3  mL/min。在最佳实验条件下,东北岩高兰总黄酮
                 的质量分数由纯化前的 49.16%提高到纯化后的 89.59%,表明 AB-8 型大孔吸附树脂能够有效纯化东北岩高兰。
                 关键词:东北岩高兰;总黄酮;大孔吸附树脂;高效液相色谱;纯化;中药现代化技术
                 中图分类号:R284.2      文献标识码:A     文章编号:1003-5214 (2019) 04-0664-07



                       Purification of Total Flavonoids from Empetrum nigrum L. var.
                                      japonicum with Macroreticular Resin


                                                                                        *
                                LIU Xiao-yan, LI Feng, LI Ai-feng, SUN Ai-ling, LIU Ren-min
                     (College of Chemistry and Chemical Engineering, Liaocheng University, Liaocheng 252059, Shandong, China)


                 Abstract: Eight types of macroporous resins were compared via static adsorption-desorption methods with
                 adsorption capacity and desorption capacity as dexes. Result indicated that AB-8 resin performed better
                 adsorption and desorption properties to total flavonoids from Empetrum nigrum L. var. japonicum. There
                 are five main components of Empetrum nigrum L. var. Japonicum extracted by HPLC analysis. Then, the
                 purification process of total flavonoids was studied by static and dynamic adsorption-desorption experiments.
                 The  optimal  static  adsorption  and  desorption  conditions  for  the  five  components  were  as  follow:  static
                 adsorption equilibrium time was 1.0 h, desorption solvent was 95%(volume fraction) ethanol and desorption
                 equilibrium  time  was  1.5  h.  Adsorption  isotherm  of  five  components  from  Empetrum nigrum  L.  var.
                 japonicum by AB-8 macroporous adsorption resin according with Freundlich model and Langmuir model at
                 different  temperatures  (25、30、35 ℃).  The  optimal  dynamic  adsorption  elution  conditions  for  the  five
                 components were as follow:mass concentration of loading buffer was 5 g/L,the maximum sample volume
                 was 400 mL, the impurities were washed by 5 BV 20%(volume fraction) ethanol, the components eluted
                 with 95%(volume fraction) ethanol, elution volume was 5 BV, and elution flow rate was 3 mL/min. Finally,
                 the purity of total flavonoids from Empetrum nigrum L. var. japonicum increased from 49.16% to 89.59%
                 at the optimal experimental conditions. This experiment provides a reference for further study of Empetrum
                 nigrum L. var. japonicum.
                 Key words: Empetrum nigrum L. var. japonicum; total flavonoids; macroporous resin; high performance
                 liquid chromatography; purification; modernization technology of traditional Chinese medicines
                 Foundation items: National Natural Science Foundation of China (21675071); Major Research Projuct of
                 Shandong Province (2016GSF202007)


                 收稿日期:2018-06-13;  定用日期:2018-12-11; DOI: 10.13550/j.jxhg.20180434
                 基金项目:国家自然科学基金(21675071);山东省重点研发计划(2016GSF202007)
                 作者简介:刘晓燕(1992—),女,硕士生。联系人:柳仁民(1963—),男,教授,硕士生导师,E-mail:Renminliu@126.com。
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