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林产化学与工业 ›› 2021, Vol. 41 ›› Issue (3): 85-94.doi: 10.3969/j.issn.0253-2417.2021.03.012

• 研究报告 • 上一篇    下一篇

竹柏叶中黄酮类成分的分离与鉴定

郭婕, 王欢, 张祁, 宋科()   

  1. 吉首大学 林产化工工程湖南省重点实验室, 湖南 张家界 427000
  • 收稿日期:2020-09-30 出版日期:2021-06-28 发布日期:2021-07-01
  • 通讯作者: 宋科 E-mail:kesong0608@163.com
  • 作者简介:宋科, 副教授, 硕士生导师, 主要从事天然产物分离方法的研究与开发; E-mail: kesong0608@163.com
    郭婕(1981-), 女, 内蒙古包头人, 副教授, 博士, 主要从事天然产物分离与鉴定工作
  • 基金资助:
    国家自然科学基金资助项目(31560105);国家自然科学基金资助项目(32060326)

Separation and Identification of Flavonoids from Leaves of Nageia nagi(Thunberg) Kuntze

Jie GUO, Huan WANG, Qi ZHANG, Ke SONG()   

  1. Key Laboratory of Hunan Forest Product and Chemical Industry Engineering, Jishou University, Zhangjiajie 427000, China
  • Received:2020-09-30 Online:2021-06-28 Published:2021-07-01
  • Contact: Ke SONG E-mail:kesong0608@163.com

摘要:

在静态吸附-解吸、动态吸附-解吸实验的基础上,对比了AB-8和D101大孔吸附树脂、聚酰胺树脂-1号(PLA-1)和聚酰胺树脂-2号(PLA-2)对竹柏总黄酮及穗花杉双黄酮的吸附-解吸性能,并对筛选出的AB-8型大孔吸附树脂纯化竹柏总黄酮的工艺进行探讨。在实验设计范围内,最佳工艺条件为:上样液中总黄酮质量浓度为1.5~3.0 g/L、上样流速22 mL/h、上样量220 mL;洗脱剂为体积分数80%的乙醇、洗脱流速44 mL/h、洗脱剂用量140 mL;竹柏总黄酮质量分数从13.6%提高到52.8%,穗花杉双黄酮质量分数从0.1%提高到2.37%。采用多种色谱分离纯化技术,从竹柏叶提取物的正丁醇萃取物中分离得到8个单体化合物,借助UV、FT-IR、MS、1H NMR及13C NMR鉴定出化合物的结构分别为:儿茶素(1)、芹菜素(2)、表儿茶素(3)、牡荆苷(4)、牡荆苷鼠李糖苷(5)、穗花杉双黄酮(6)、罗汉松双黄酮A(7)和白果黄素(8)。其中化合物458为首次从竹柏属植物中分离得到。

关键词: 竹柏叶, 总黄酮, 双黄酮, 黄酮碳苷, 大孔树脂纯化

Abstract:

Based on the adsorption-desorption tests of total flavonoids and amentoflavone from leaves of Nageia nagi(Thunberg) Kuntze on different resins, AB-8 resin with the preferable adsorption and desorption performances was selected from four kinds of resins, which were AB-8 and D101 resins, and polyamide resins(PLA-1 and PLA-2). The optimum process was recommended as follows: for the adsorption tests, the mass concentration of total flavonoids was 1.5-3.0 g/L, the load rate was 22 mL/h and volume of loading solution was 220 mL; desorption tests was sequentially operated with 140 mL 80% ethanol-water solution as eluent at the wash rate of 44 mL/h. As a result, with the optimized processes, the content of total flavonoid and amentoflavone was significantly increased from 13.6% to 52.8% and 0.1% to 2.37%, respectively. Varieties of chromatographic techniques were used to separate and purify the extract fromleaves of N. nagi. The structures of the compounds were identified by UV, FT-IR, MS, 1D NMR and 2D NMR. Eight compounds were isolated from the n-butanol extract from branches and leaves of N. nagi alcohol extract. They were catechin(1), apigenin(2), epi-catechin(3), vitexin(4), vitexin rhamnoside(5), amentoflavone(6), podocarpus flavone A(7), and bilobetin(8). Among them, compounds4, 5 and 8 were isolated from genus Nageia for the first time.

Key words: Nageia nagi leaves, flavonoids, biflavones, flavone glycosides, purification with macroporous resin

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