New and old NMR experiments for the resonance assignment of complex oligosaccharides--application to a cyclodextrin derivative.
Fiche publication
Date publication
décembre 2011
Auteurs
Membres identifiés du Cancéropôle Est :
Dr NUZILLARD Jean-Marc
Tous les auteurs :
Plainchont B, Martinez A, Tisse S, Bouillon JP, Pilard F, Wieruszeski JM, Lippens G, Jeannerat D, Nuzillard JM
Lien Pubmed
Résumé
The complete assignment of the (1)H and (13)C sugar resonances in mono-3,6-anhydro-heptakis(2,3-O-methyl)-hexakis(6-O-methyl)-beta-cyclodextrin, an asymmetrically functionalized beta-cyclodextrin, was carried out by means of 2D NMR experiments. The TOCSY and the homonuclear multiple relay COSY spectra provided most of the (1)H assignments. The multiplicity edited HSQC and a set of F(1) selective HSQC-TOCSY and multiple relay HSQC-COSY spectra gave access to most of the (13)C chemical shifts. The latter were fully and accurately determined by means of a pair of complementary, highly folded HSQC-TOCSY spectra. The TOCSY-ROESY and ROESY-TOCSY spectra yielded the sequential assignment of the sugar units. A high resolution F(1) selective F(1) decoupled version of the TOCSY-ROESY experiment was recorded.
Référence
Magn Reson Chem. 2011 Dec;49(12):781-7