4.7 Article

Oligosaccharide mapping analysis by HILIC-ESI-HCD-MS/MS for structural elucidation of fucoidan from sea cucumber Holothuria floridana

Journal

CARBOHYDRATE POLYMERS
Volume 275, Issue -, Pages -

Publisher

ELSEVIER SCI LTD
DOI: 10.1016/j.carbpol.2021.118694

Keywords

Fucoidan; Oligosaccharide mapping; Sulfation pattern; HILIC-ESI-FTMS; HILIC-ESI-HCD-MS; MS; 2D NMR

Funding

  1. National Key R&D Program of China [2020YFD0900202, 2018YFC0311200]
  2. Scientific Program of The General Administration of Customs of China [2020HK209]
  3. Natural Science Foundation of Zhejiang Province [LY19C200001]
  4. Research Project of General Administration of Quality Supervision Inspection and Quarantine of the People's Republic of China [2016IK204]

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This work elucidated the structure of fucoidan from Holothuria floridana through oligosaccharide mapping, revealing various oligosaccharide domains with specific sulfation patterns.
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.

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