Three-dimensional heteronuclear NMR techniques for assignment and conformational analysis using exchangeable protons in uniformly 13C-enriched oligosaccharides |
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Authors: | R. Harris T.J. Rutherford M.J. Milton S.W. Homans |
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Affiliation: | (1) Centre for Biomolecular Sciences, University of St. Andrews, The Purdie Building, St. Andrews, KY16 9ST, U.K |
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Abstract: | We present heteronuclear three-dimensional gradient-NMR techniques for the resonanceassignment of exchangeable (-OH and -NH) protons in uniformly 13C isotopically enrichedoligosaccharides and for the measurement of 1H-1H nuclear Overhauser enhancementsinvolving these protons. These techniques are derived from conventional HOHAHA-HSQCand NOESY(ROESY)-HSQC experiments, and are illustrated in application to a sample ofuniformly 13C-enriched Gal1-4GlcNAc, and demonstrate that a total of 35 ROEs involvingexchangeable protons can be detected and assigned. We present a quantitative analysis ofthese ROEs that can only be accommodated in a model of the solution behaviour of theoligosaccharide that involves considerable internal motion. |
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Keywords: | Oligosaccharide 3D heteronuclear NMR N-Acetyllactosamine |
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