食品科学 ›› 2014, Vol. 35 ›› Issue (6): 30-35.doi: 10.7506/spkx1002-6630-201406006

• 工艺技术 • 上一篇    下一篇

AB-8大孔吸附树脂精制芦柑皮总黄酮及黄酮类化合物的分离

骆党委,叶 静,黄雅燕,肖美添*   

  1. 华侨大学化工学院,福建 厦门 361021
  • 收稿日期:2013-04-12 修回日期:2014-03-06 出版日期:2014-03-25 发布日期:2014-04-04
  • 通讯作者: 肖美添 E-mail:kukuleleyunyun@126.com
  • 基金资助:

    泉州市重大科技专项(2008ZD17)

Purification of Total Flavonoids Extracted from Ponkan (Citrus reticulata Blanco cv. Ponkan) Peel by AB-8 Macroporous Adsorption Resin and Separation of Flavonoid Constituents

LUO Dang-wei, YE Jing, HUANG Ya-yan, XIAO Mei-tian*   

  1. College of Chemical Engineering, Huaqiao University, Xiamen 361021, China
  • Received:2013-04-12 Revised:2014-03-06 Online:2014-03-25 Published:2014-04-04
  • Contact: XIAO Mei-tian E-mail:kukuleleyunyun@126.com

摘要:

目的:研究AB-8大孔吸附树脂精制芦柑皮总黄酮的工艺条件及芦柑皮黄酮类化合物的分离纯化。方法:采用AB-8大孔吸附树脂动态法精制芦柑皮总黄酮,考察上样液总黄酮质量浓度、pH值、上样流速、洗脱液乙醇体积分数对吸附解吸性能的影响;然后将精制的芦柑皮总黄酮经硅胶柱层析、半制备高效液相等技术进行分离纯化,并根据理化性质和波谱数据鉴定化学结构。结果:AB-8大孔树脂精制芦柑皮总黄酮的最佳工艺条件为上样液总黄酮质量浓度3.03 mg/mL、上样液pH 3.0、上样流速3.0 BV/h、洗脱液乙醇体积分数为90%,最优条件下可使芦柑皮总黄酮的纯度从17.8%提高到63.1%;此外,从精制的芦柑皮黄酮中分离到8 个黄酮类化合物,分别鉴定为:橘皮素、川陈皮素、4’,5,7,8-四甲氧基黄酮、5-去甲基-橘皮素、橙黄酮、橙浸膏、柚皮苷、橙皮苷。结论:AB-8大孔树脂能很好地富集纯化芦柑皮总黄酮,该法简单、可行;从精制的芦柑皮黄酮中分离到8 个黄酮类化合物,其中,4’,5,7,8-四甲氧基黄酮、5-去甲基-橘皮素、橙浸膏、柚皮苷、橙皮苷首次从芦柑皮中分得。

关键词: 芦柑皮, 总黄酮, AB-8大孔吸附树脂

Abstract:

Objective: To propose an optimal purification process for flavonoids extracted from ponkan (Citrus Reticulata
Blanco cv. Ponkan) peel. Methods: The dynamic adsorption and desorption performance of AB-8 macroporous resin towards
flavonoids extracted from ponkan peel was investigated. Major process parameters including sample concentration, pH,
flow rate, and elution ethanol concentration were evaluated. Then the purified flavonoids were isolated by chromatographic
methods with silica gel and semi-preparative HPLC, and the structures were elucidated on the basis of physicochemical
properties and spectral data analysis. Results: The optimal purification process was determined as follows: samples at pH 3.0
containing 3.03 mg/mL ponan peel flavonoids were loaded onto the column at a flow rate of 3.0 BV/h, and then 90% ethanol
was passed through the column to elute the bound flavonoids. After the purification, the purity of ponan peel flavonoids
was increased from 17.8% to 63.1%. In addition, eight compounds were isolated from the purified flavonoids and identified
as tangeretin, nobiletin, 4′,5,7,8-tetramethyl-O-isoscutellarein, 5-demethyl-tangeretin, sinetsetin, aurantine, naringin, and
hesperidin. Conclusion: AB-8 macroporous resin has a high performance in enriching and purifying flavonoids from ponkan
peel, providing a simple and feasible method. Eight compounds can be isolated from the purified flavonoids. Moreover,
4′,5,7,8-tetramethyl-O-isoscutellarein, 5-demethyl-tangeretin, aurantine, naringin, and hesperidin are first reported from
ponkan peel.

Key words: Citrus reticulata Blanco cv. Ponkan peel, flavonoids, AB-8 macroporous adsorption resin

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