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Multiple-step relayed correlation spectroscopy: sequential resonance assignments in oligosaccharides.

S W Homans, R A Dwek, D L Fernandes

    Proceedings of the National Academy of Sciences of the United States of America
    |October 1, 1984
    PubMed
    Summary
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    This study introduces a novel three-step relayed correlation spectroscopy method for precise proton NMR spectral assignments in oligosaccharides. This technique resolves ambiguities, enabling accurate determination of three-dimensional structures.

    Area of Science:

    • Carbohydrate Chemistry
    • Nuclear Magnetic Resonance Spectroscopy
    • Structural Biology

    Background:

    • Proton NMR spectra of oligosaccharides typically show well-resolved anomeric (H1) and H2 proton resonances.
    • Skeletal protons (3-4 ppm) often form poorly resolved envelopes, leading to assignment ambiguities.
    • Standard 1H-1H correlated spectroscopy can link H1/H2 to H2/H3 but struggles with distant couplings.

    Purpose of the Study:

    • To develop a general solution for assigning proton NMR resonances in complex oligosaccharides.
    • To overcome spectral dispersion limitations and assignment ambiguities in standard NMR methods.
    • To enable subsequent determination of three-dimensional solution conformations.

    Main Methods:

    • Utilized three-step two-dimensional relayed correlation spectroscopy.

    Related Experiment Videos

  • Employed sequential magnetization transfer around oligosaccharide rings.
  • Correlated resolved anomeric (H1) and H2 protons with remote protons (H4, H5) via coupling networks.

    • Main Results:

    • Successfully correlated resolved and remote protons through a linear coupling network.
    • Obtained resonance assignments by analyzing cross-peaks in well-resolved spectral regions.
    • Demonstrated a general approach to solving oligosaccharide NMR assignment problems.

    Conclusions:

    • The described method provides a general solution for oligosaccharide proton NMR assignment.
    • Accurate assignments facilitate the determination of three-dimensional solution structures using Nuclear Overhauser Effect experiments.
    • This technique enhances the structural elucidation of complex carbohydrates.