Titre :

Expedited NMR Assignment of Small- to Medium-Sized Molecules with Improved HSQC−CLIP−COSY Experiments

Auteur(s) :

Gyöngyösi, Tamás [Auteur]
University of Debrecen
Timári, István [Auteur correspondant]
University of Debrecen
Sinnaeve, Davy [Auteur]
Facteurs de Risque et Déterminants Moléculaires des Maladies liées au Vieillissement - U 1167 [RID-AGE]
Biologie Structurale Intégrative [ERL 9002 - INSERM U1167 - BSI]
Luy, Burkhard [Auteur]
Karlsruhe Institute of Technology = Karlsruher Institut für Technologie [KIT]
Kövér, Katalin [Auteur correspondant]
University of Debrecen

Titre de la revue :

Analytical Chemistry

Pagination :

3096-3102

Éditeur :

American Chemical Society

Date de publication :

2021-02-03

ISSN :

0003-2700

Mot(s)-clé(s) en anglais :

NMR
Peptides and proteins

Discipline(s) HAL :

Chimie/Chimie analytique

Résumé en anglais : [en]

Resonance assignment is a pivotal step for any nuclear magnetic resonance (NMR) analysis, such as structure elucidation or the investigation of protein–ligand interactions. Both 1H-13C heteronuclear single quantum correlation ...
Lire la suite >Resonance assignment is a pivotal step for any nuclear magnetic resonance (NMR) analysis, such as structure elucidation or the investigation of protein–ligand interactions. Both 1H-13C heteronuclear single quantum correlation (HSQC) and 1H-1H correlation spectroscopy (COSY) two-dimensional (2D) experiments are invaluable for 1H NMR assignment, by extending the high signal dispersion of 13C chemical shifts onto 1H resonances and by providing a high amount of through-bond 1H-1H connectivity information, respectively. The recently introduced HSQC−CLIP(Clean In-Phase)−COSY method combines these two experiments, providing COSY correlations along the high-resolution 13C dimension with clean in-phase multiplets. However, two experiments need to be recorded to unambiguously identify COSY cross-peaks. Here, we propose novel variants of the HSQC–CLIP–COSY pulse sequence that edit cross-peak signs so that direct HSQC responses can be distinguished from COSY relay peaks, and/or the multiplicities of the 13C nuclei are reflected, allowing the assignment of all the peaks in a single experiment. The advanced HSQC–CLIP–COSY variants have the potential to accelerate and simplify the NMR structure-elucidation process of both synthetic and natural products and to become valuable tools for high-throughput computer-assisted structure determination.Lire moins >

Langue :

Anglais

Comité de lecture :

Oui

Audience :

Internationale

Vulgarisation :

Non

Projet ANR :

Développement de stratégies innovantes pour une approche transdisciplinaire de la maladie d'Alzheime

Collections :

• Facteurs de risque et déterminants moléculaires des maladies liées au vieillissement (RID-AGE) - U1167

Source :

Harvested from HAL