Expedited NMR Assignment of Small- to ...
Document type :
Article dans une revue scientifique: Article original
PMID :
Title :
Expedited NMR Assignment of Small- to Medium-Sized Molecules with Improved HSQC−CLIP−COSY Experiments
Author(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
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
Journal title :
Analytical Chemistry
Pages :
3096-3102
Publisher :
American Chemical Society
Publication date :
2021-02-03
ISSN :
0003-2700
English keyword(s) :
NMR
Peptides and proteins
Peptides and proteins
HAL domain(s) :
Chimie/Chimie analytique
English abstract : [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 ...
Show more >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.Show less >
Show more >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.Show less >
Language :
Anglais
Peer reviewed article :
Oui
Audience :
Internationale
Popular science :
Non
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