高等学校化学学报 ›› 2019, Vol. 40 ›› Issue (4): 733.doi: 10.7503/cjcu20180583

• 有机化学 • 上一篇    下一篇

一种刺松藻来源的硫酸阿拉伯聚糖的制备及特征结构表征

金鑫, 嵇国利, 赵小亮, 李国云, 于广利()   

  1. 山东省糖科学与糖工程重点实验室, 海洋药物教育部重点实验室, 中国海洋大学医药学院, 青岛 266003
  • 收稿日期:2018-08-20 出版日期:2019-03-11 发布日期:2019-03-11
  • 作者简介:

    联系人简介: 于广利, 男, 博士, 教授, 博士生导师, 主要从事糖化学和糖药物学方面的研究. E-mail: glyu@ouc.edu.cn

  • 基金资助:
    国家自然科学基金-山东海洋科学研究中心联合基金(批准号: U1606403)、 青岛海洋科学与技术国家实验室鳌山科技创新计划项目(批准号: 2016ASKJ08)和泰山学者工程专项基金(批准号: TS201511011)资助.

Sulfated Arabinose from Codium fragile: Preparation and Extensive Structural Characterization

JIN Xin, JI Guoli, ZHAO Xiaoliang, LI Guoyun, YU Guangli*()   

  1. Shandong Provincial Key Laboratory of Glycoscience and Glycotechnology, Key Laboratory of Marine Drugs of Ministry of Education, School of Medicine and Pharmacy, Ocean University of China, Qingdao 266003, China
  • Received:2018-08-20 Online:2019-03-11 Published:2019-03-11
  • Contact: YU Guangli E-mail:glyu@ouc.edu.cn
  • Supported by:
    † Supported by the National Natural Science Foundation of China-Shangdong Joint Fund for Marine Science Research Centers of China(No.U1606403), the Qingdao National Laboratory for Marine Science and Technology, China(No.2016ASKJ08) and the Taishan Scholar Project Special Funds of China(No.TS201511011).

摘要:

刺松藻(Codium fragile)经水提-醇沉获得粗多糖, 进一步将刺松藻粗多糖(CFP) 通过Q-Sepharose Fast Flow(QFF) 阴离子交换柱纯化得到6个多糖组分CFP1CFP6, 其中, 在CFP6中发现纯度较高的阿拉伯聚糖. 采用高效凝胶渗透色谱与十八角激光散射仪联用法和1-苯基-3-甲基-5-吡唑啉酮(PMP)柱前衍生高效液相色谱法对CFP6的分子量及单糖组成进行了分析. 结果表明, CFP6是一种分子量为79290的多糖, 由阿拉伯糖(Ara)和半乳糖(Gal)组成, 二者摩尔比为14.8:1.0. 通过多维核磁共振波谱、 液相色谱-质谱联用及二级质谱等方法对CFP6的糖苷键连接方式及其寡糖序列结构进行表征, 进一步阐明了该复杂多糖的特征结构. 经判断, CFP6主链由Ara组成, 通过 β-(1→3)糖苷键连接, 在Ara的C2位存在分支结构, 硫酸基位于Ara的C4或C2位.

关键词: 刺松藻, 多糖, 结构分析, 寡糖序列分析, 二级质谱

Abstract:

The crude polysaccharide was obtained from Codium fragile by water extracted and alcohol precipitated, and further 6 fractions purified by Q-Sepharose fast flow column were named CFP1—CFP6, respectively. CFP6 is a higher purity arabinose of them. The absolute molecular mass of the main fraction CFP6 was determined by high performance gel permeation chromatography and laser scattering instrument. The monosaccharide composition was analyzed by reversed phase high-performance liquid chromatography(RP-HPLC) labeled with 1-phenyl-3-methyl-5-pyrazolone(PMP). The results showed that CFP6 is a homogeneous polysaccharide component with a molecular weight of 79290 and consists of arabinose(Ara) and galactose(Gal) with a molar ratio of 14.8:1.0. Subsequently, the structural features and oligosaccharide sequence composition were identified by multi-dimensional nuclear magnetic resonance spectroscopy and liquid chromatography-mass spectrometry, further to elucidate the fine structure of the complex polysaccharide. The results revealed that the backbone of CFP6 is β-(1→3)-linked arabinan and sulfate group is located at the C4 or C2 positions. CFP6 is a higher purity arabinose and its extensive structure information can enrich the marine carbohydrate data and provides a methodological reference for the study of complex polysaccharide structures.

Key words: Codium fragile, Polysaccharide, Structural analysis, Oligosaccharide sequence analysis, MS/MS spectrometry

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