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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
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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
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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。