Carbohydrate Polymers ( IF 11.2 ) Pub Date : 2021-09-22 , DOI: 10.1016/j.carbpol.2021.118694 Zizhe An 1 , Zhaohui Zhang 1 , Xiaomei Zhang 2 , Huicheng Yang 3 , Haiyan Lu 1 , Mengyang Liu 1 , Ying Shao 1 , Xue Zhao 1 , Hongwei Zhang 2
The elucidation of precise structure of fucoidan is essential for understanding their structure-function relationship and promoting the development of marine drugs. In this work, we firstly reported the oligosaccharide mapping of fucoidan from Holothuria floridana using a combination of hydrothermal depolymerization, hydrophilic interaction liquid chromatography (HILIC) coupled with electrospray mass spectrometry (ESI-FTMS) and high energy collision-induced dissociation (HCD-MS/MS) and 2D NMR analysis. With careful selection of fully deprotonated molecular ions of fucoidan oligosaccharides and their NaBD4 reduced alditols, HILIC-ESI-HCD-MS/MS provided structurally relevant glycosidic product ions with no sulfate loss for definitive assignment of sequence and sulfation pattern of all the oligosaccharides and their isomers from dp2 to dp7 from hydrothermal depolymerization. The oligosaccharide mapping clarified the structure of fucoidan with various oligosaccharide domains with 2,4-di-O-sulfated and 2-O sulfated fucose residues.
中文翻译:
HILIC-ESI-HCD-MS/MS 寡糖作图分析海参海参中褐藻糖胶的结构解析
阐明褐藻糖胶的精确结构对于了解其构效关系、促进海洋药物的开发具有重要意义。在这项工作中,我们首次报道了结合水热解聚、亲水相互作用液相色谱(HILIC)结合电喷雾质谱(ESI-FTMS)和高能碰撞诱导解离(HCD-MS)对佛罗里达海参中褐藻糖胶的寡糖图谱。/MS) 和 2D NMR 分析。仔细选择完全去质子化的褐藻糖胶寡糖分子离子及其 NaBD 4减少糖醇,HILIC-ESI-HCD-MS/MS 提供了结构相关的糖苷产物离子,没有硫酸盐损失,用于确定水热解聚中所有寡糖及其异构体从 dp2 到 dp7 的序列和硫酸化模式。寡糖作图阐明了具有 2,4-二-O-硫酸化和 2 - O-硫酸化岩藻糖残基的各种寡糖结构域的岩藻依聚糖结构。