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  • 1D trNOESY-TOCSY  (1)
  • Polysaccharide  (1)
  • 1
    Electronic Resource
    Electronic Resource
    Application of homonuclear 3D NMR experiments and 1D analogs to study the conformation of sialyl Lewisx bound to E-selectin (1997)
    Springer
    Journal of biomolecular NMR 9 (1997), S. 423-436 
    Details
    ISSN: 1573-5001
    Keywords: 3D TOCSY-trNOESY ; 1D TOCSY-trNOESY ; 1D trNOESY-TOCSY ; trNOE ; trROE ; E-selectin ; sialyl Lewisx
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Chemistry and Pharmacology
    Notes: Abstract The conformation of the sialyl Lewis x tetrasaccharidebound to E-selectin was previously determined from transfer NOE (trNOE)experiments in conjunction with a distance-geometry analysis. However, theorientation of the tetrasaccharide ligand in the binding site of E-selectinis still unknown. It can be predicted that the accurate quantitativeanalysis of all trNOEs, including those originating from spin diffusion, isone key to analyze the orientation of sialyl Lewisx in thebinding pocket of E-selectin. Therefore, we applied homonuclear 3D NMRexperiments and 1D analogs to obtain trNOEs that could not unambiguously beassigned from previous 2D trNOESY spectra, due to severe resonance-signaloverlap. A 3D TOCSY-trNOESY experiment, a 1D TOCSY-trNOESY experiment, and a1D trNOESY-TOCSY experiment of the sialyl Lewisx/E-selectincomplex furnished new interglycosidic trNOEs and provided additionalinformation for the interpretation of trNOEs that have been describedbefore. A 2D trROESY spectrum of the sialyl Lewisx/E-selectincomplex allowed one to identify the amount of spin-diffusion contributionsto trNOEs. Finally, an unambiguous assignment of all trNOEs, and an analysisof spin-diffusion pathways, was obtained, creating a basis for aquantitative analysis of trNOEs in the sialylLewisx/E-selectin complex.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1018358929268
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  • 2
    Electronic Resource
    Electronic Resource
    Application of 1D and 2D NMR techniques to the structure elucidation of the O-polysaccharide from Proteus mirabilis O: 57 (1994)
    Springer
    Journal of biomolecular NMR 4 (1994), S. 615-630 
    Details
    ISSN: 1573-5001
    Keywords: Polysaccharide ; Selective excitation ; Long-range proton-carbon couplings
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Chemistry and Pharmacology
    Notes: Summary The LPS O-polysaccharide (O-PS) produced by Proteus mirabilis serotype O: 57 (ATCC 49995) was shown by NMR spectroscopy and chemical analysis to be a high-molecular-weight acidic branched polymer of pentasaccharide repeating units, composed of d-glucose, d-galactose, 2-acetamido-2-deoxy-d-galactose and glycerophosphate residues (1:2:2:2:1). Application of one-and two-dimensional NMR methods allowed the complete assignment of notoriously crowded 1H and 13C spectra of the O-PS, leading to the determination of its structure. Several of the NMR techniques used were applied for the first time to the structure elucidation of polysaccharides. The resonances of galactose H5, H6 and H6′ were identified by a 1D analog of 3D NOESY-TOCSY and 2D {1H, 1H} triple-quantum experiments. The position and the nature of the phosphate group were determined from 2D 31P (ω1)-half-filtered COSY and 2D 31P-relayed COSY spectra. 2D HMQC-TOCSY and 2D single-quantum proton-carbon long-range correlation techniques were used to overcome the difficulties of severe overlap and higher order effects in the 1H NMR spectrum of the O-PS. The latter technique, together with 2D NOESY, enabled us to identify the substitution positions, the anomeric configurations and the sequence of the component glycose residues in the O-PS.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00404273
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