New and old NMR experiments for the resonance assignment of complex oligosaccharides-application to a cyclodextrin derivative

Plainchont, B.; Martinez, Alexandre; Tisse, S.; Bouillon, J.-P.; Pilard, F.; Wieruszeski, J.-M.; Lippens, G.; Jeannerat, Damien; Nuzillard, J.-M.

doi:10.1002/mrc.2828

Scientific article

English

New and old NMR experiments for the resonance assignment of complex oligosaccharides-application to a cyclodextrin derivative

Contributors

Plainchont, B.; Martinez, Alexandre; Tisse, S.; Bouillon, J.-P.; Pilard, F.; Wieruszeski, J.-M.; Lippens, G.; Jeannerat, Damien; Nuzillard, J.-M.

Published in

Magnetic resonance in chemistry, vol. 49, no. 12, p. 781-787

Publication date

2011

Abstract

The complete assignment of the 1H and 13C sugar resonances in mono-3,6-anhydro-heptakis(2,3-O-methyl)-hexakis(6-O-methyl)-β-cyclodextrin, an asymmetrically functionalized β-cyclodextrin, was carried out by means of 2D NMR experiments. The TOCSY and the homonuclear multiple relay COSY spectra provided most of the 1H assignments. The multiplicity edited HSQC and a set of F1 selective HSQC-TOCSY and multiple relay HSQC-COSY spectra gave access to most of the 13C 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 F1 selective F1 decoupled version of the TOCSY-ROESY experiment was recorded.

Keywords

NMR
1H
13C
Cyclodextrin
Assignment
Selective pulses
Resolution enhancement
Aliasing
Sequential assignment

UNIGE affiliation entities

Faculté des sciences / Section de chimie et biochimie / Département de chimie organique

Citation (ISO format)

PLAINCHONT, B. et al. New and old NMR experiments for the resonance assignment of complex oligosaccharides-application to a cyclodextrin derivative. In: Magnetic resonance in chemistry, 2011, vol. 49, n° 12, p. 781–787. doi: 10.1002/mrc.2828

Article (Published version)

Identifiers

PID : unige:17801
DOI : 10.1002/mrc.2828

Journal ISSN

0749-1581

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Creation

14/12/2011 16:46:00

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14/12/2011 16:46:00

Update

14/03/2023 17:05:46

Status update

14/03/2023 17:05:46

Last indexation

29/10/2024 18:43:49

New and old NMR experiments for the resonance assignment of complex oligosaccharides-application to a cyclodextrin derivative

Contributors

Published in

Publication date

Abstract

Keywords

UNIGE affiliation entities

Citation (ISO format)

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Identifiers

Journal ISSN

Technical informations

Creation

First validation

Update

Status update

Last indexation