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• 成分分析 •    下一篇

高纯度亚麻木酚素的分离纯化和分析方法研究

王尉1,贺天雨1,赵新颖1,席兴军2,兰韬2,杜宁1,张经华1   

  1. 1. 北京市理化分析测试中心
    2. 中国标准化研究院
  • 收稿日期:2018-03-02 修回日期:2019-01-29 出版日期:2019-04-25 发布日期:2019-05-05
  • 通讯作者: 赵新颖 E-mail:zhaoxinying_123@sina.com
  • 基金资助:
    国家重点研发计划

Study on Purification and Analysis of Highly Pure Flax Lignan

2, 2, 2, 2,   

  • Received:2018-03-02 Revised:2019-01-29 Online:2019-04-25 Published:2019-05-05

摘要: 为了开展高纯度亚麻木酚素的分离纯化和分析方法研究,本实验选取亚麻籽为研究对象,通过正己烷脱脂、乙醇提取、AB-8大孔吸附树脂分离、高速逆流色谱(high-speed countercurrent chromatography,HSCCC)纯化制备得到高纯度亚麻木酚素。其中,大孔吸附树脂的洗脱溶剂为80%乙醇,HSCCC溶剂体系为叔丁基甲醚-正丁醇-乙腈-水(1:3:1:5,v/v)。分离得到的亚麻木酚素经薄层色谱(thin-layer chromatography,TLC)、高效液相色谱-二极管阵列-蒸发光散射检测器联用(HPLC-DAD-ELSD)和高效液相色谱-质谱联用(HPLC-MS)纯度分析,结果显示杂质含量均低于0.5%。通过采用多种高效液相色谱(high performance liquid chromatography,HPLC)条件分析,峰面积归一化法进行纯度计算,其纯度值在99.3%~99.5%之间。最后采用紫外光谱(UV)、红外光谱(IR)、高分辨质谱(HRMS)、核磁共振波谱(NMR)和元素分析等方法鉴定其结构为亚麻木酚素。结果表明,该分离纯化方法简单可行,纯度分析方法准确可靠,制备得到的样品具有纯度高的优点,可以应用于相关产品的质量控制和方法验证。

关键词: 亚麻籽, 木酚素, 分离纯化, 纯度分析, 结构鉴定

Abstract: The objective was to study on purification and analysis of Flax Lignan. Highly pure flax lignan was purified by n-hexane defatting, ethanol extraction, AB-8 macroporous adsorption resin separation and HSCCC purification from flaxseed. Flax lignan was eluted with 80% ethanol in AB-8, and HSCCC solvent system was composed of tert-butyl methyl ether-n-butanol-acetonitrile-water (1:3:1:5, v/v). The results show that the impurity content is less than 0.5 % by TLC, HPLC, HPLC-DAD-ELSD and HPLC-MS. The purity of flax lignan were 99.3%~99.5% calculated by area normalization by various HPLC analytical conditions. The structures were identified by UV, IR, HRMS, NMR and elemental analysis. These results indicated that the purification method is simple and feasible, and the purity analysis method is accurate and reliable. Flax lignin has the advantages of high purity, which can be used for method validation and quality control of regarding products.

Key words: flaxseed, lignan, purification, purity analysis, structural identification

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