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Measurement of inter-glycosidic 13C-1H coupling constants in a cyclic β(1→2)-glucan by 13C-filtered 2D {1H,1H}ROESY

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Summary

A method for measuring three-bond 13C-1H scalar coupling constants across glycosidic bonds in a cyclic β(1→2)-glucan icosamer is presented. This oligosaccharide molecule, with its high degree of symmetry, represents a particular challenge for NMR spectroscopy to distinguish inter-residue from intra-residue heteronuclear coupling effects. Chemically equivalent H2 protons in adjacent glucosyl residues are distinguished on the basis of their different through-space, dipolar interactions with the anomeric protons (H1). The strong NOE contact between anomeric (H1) and aglyconic (H2′) protons permits the selective observation of the inter-residue heteronuclear couplings 3JC1H2′ and 3JC2′H1 in a natural-abundance 13C-ω1-half-filtered {1H,1H} ROESY experiment.

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Abbreviations

COSY:

scalar correlated spectroscopy

NOE:

nuclear Overhauser effect

NOESY:

NOE spectroscopy

ROESY:

rotating-frame NOE spectroscopy

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Authors and Affiliations

  1. Complex Carbohydrate Research Center, The University of Georgia, 220 Riverbend Road, 30602, Athens, GA, U.S.A.

    Leszek Poppe, William S. York & Herman van Halbeek

  2. Department of Biochemistry, The University of Georgia, 220 Riverbend Road, 30602, Athens, GA, U.S.A.

    Leszek Poppe, William S. York & Herman van Halbeek

Authors
  1. Leszek Poppe
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  2. William S. York
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  3. Herman van Halbeek
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Poppe, L., York, W.S. & van Halbeek, H. Measurement of inter-glycosidic 13C-1H coupling constants in a cyclic β(1→2)-glucan by 13C-filtered 2D {1H,1H}ROESY. J Biomol NMR 3, 81–89 (1993). https://doi.org/10.1007/BF00242477

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  • DOI: https://doi.org/10.1007/BF00242477

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