Ligand-aided 1H Nuclear Magnetic Resonance Spectroscopy for Non-destructive Estimation of Sulfate Content in Sulfated Saccharides

Sulfated saccharides exhibit diverse physiological activities, but a lack of any convenient assay hinders their evaluation. Herein, an assay for the analysis of sulfated saccharides is described using 1H nuclear magnetic resonance (NMR) spectroscopy by employing ligands that can form ionic complexes...

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Bibliographic Details
Published in:Analytical Sciences 2020/10/10, Vol.36(10), pp.1269-1274
Main Authors: BAK, Juneha, MIYAZAKI, Yoshiyuki, NAKANO, Hayato, MATSUI, Toshiro
Format: Article
Language:English
Subjects:
1H NMR
Analytical Chemistry
Assaying
Carbohydrates
Chemical equilibrium
Chemistry
Fucoidan
Imidazole
ligand
Ligands
Magnetic resonance spectroscopy
NMR
NMR spectroscopy
non-destructive assay
Nuclear magnetic resonance
Polysaccharides
Resonance
Saccharides
Spectroscopy
Spectrum analysis
Sulfated saccharide
Sulfates
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Summary:Sulfated saccharides exhibit diverse physiological activities, but a lack of any convenient assay hinders their evaluation. Herein, an assay for the analysis of sulfated saccharides is described using 1H nuclear magnetic resonance (NMR) spectroscopy by employing ligands that can form ionic complexes with the sulfate groups. Based on the change in the chemical shift (Δδ) of the ligands by sulfated mono- to tetrasaccharide, imidazole was found to be a good ligand, showing the maximum Δδ; neutral saccharides do not show any change in the δ value. A marked and constant downfield δ value observed was changed dramatically at a molar ratio of >1:1 (imidazole:sulfated saccharides), allowing a sulfate content estimation based on the concentration of imidazole at the Δδ inflection point. By the proposed ligand-aided 1H NMR assay, the sulfate content of natural sulfated polysaccharide, fucoidan, was non-destructively estimated to be 2.1 mmol/g-fucoidan.
ISSN:0910-6340
1348-2246
DOI:10.2116/analsci.20P163