The SOFAST-HMBC-HMQC experiment for pairing geminal methyl groups in valine and leucine side-chains.

Valine; Leucine; Proteins; Valine/chemistry; Leucine/chemistry; Nuclear Magnetic Resonance, Biomolecular/methods; Proteins/chemistry; Nuclear Magnetic Resonance, Biomolecular; Biochemistry; Spectroscopy

Abstract :

[en] Methyl groups are essential probes for characterising interactions and dynamics in large proteins. HN-based triple-resonance NMR experiments are often too insensitive for methyl assignments, making a NOESY-based approach an efficient strategy. Linking geminal methyl groups in leucine and valine residues is a crucial step in such NOESY-based methyl resonance assignment strategies. This link can be established unambiguously with the 3D-HMBC-HMQC experiment, introduced for large U-[12C, 2H] LV-[13CH3]2-labelled proteins. Here, we introduce the SOFAST variant of the 3D-HMBC-HMQC experiment which provides spectra with fewer artefacts arising from the water signal and a mean increase in signal-to-noise ratio per unit time of 16% compared to the original experiment with an optimised recovery delay.

Disciplines :

Chemistry

Author, co-author :

Aguilar Alva, Ana Paula; Chimie Physique et Chimie du Vivant, Département de Chimie, UMR 8228, École Normale Supérieure, PSL University, Sorbonne Université, CNRS, 24 Rue Lhomond, Paris Cedex 05, 75005, France

Siemons, Lucas; Chimie Physique et Chimie du Vivant, Département de Chimie, UMR 8228, École Normale Supérieure, PSL University, Sorbonne Université, CNRS, 24 Rue Lhomond, Paris Cedex 05, 75005, France. Lucas.Siemons@ens.psl.eu

le Paige, Ulric B; Chimie Physique et Chimie du Vivant, Département de Chimie, UMR 8228, École Normale Supérieure, PSL University, Sorbonne Université, CNRS, 24 Rue Lhomond, Paris Cedex 05, 75005, France

Wiame, Coline ; Université de Liège - ULiège

Cordier, Florence; Biological NMR & HDX-MS Technological Platform, Institut Pasteur, Université Paris Cité, CNRS UMR 3528, Paris, France ; Structural Bioinformatics Unit, Institut Pasteur, Université Paris Cité, CNRS UMR 3528, Paris, France

Wolff, Nicolas; Signaling and Receptors Dynamics Unit, Institut Pasteur, Université Paris Cité, CNRS UMR 3571, Paris, France

Bouvignies, Guillaume; Chimie Physique et Chimie du Vivant, Département de Chimie, UMR 8228, École Normale Supérieure, PSL University, Sorbonne Université, CNRS, 24 Rue Lhomond, Paris Cedex 05, 75005, France

Pelupessy, Philippe; Chimie Physique et Chimie du Vivant, Département de Chimie, UMR 8228, École Normale Supérieure, PSL University, Sorbonne Université, CNRS, 24 Rue Lhomond, Paris Cedex 05, 75005, France

Ferrage, Fabien; Chimie Physique et Chimie du Vivant, Département de Chimie, UMR 8228, École Normale Supérieure, PSL University, Sorbonne Université, CNRS, 24 Rue Lhomond, Paris Cedex 05, 75005, France. Fabien.Ferrage@ens.psl.eu

Language :

English

Title :

The SOFAST-HMBC-HMQC experiment for pairing geminal methyl groups in valine and leucine side-chains.

Publication date :

2025

Journal title :

Journal of Biomolecular NMR

ISSN :

0925-2738

eISSN :

1573-5001

Publisher :

Springer Science and Business Media B.V., Netherlands

Volume :

Issue :

Pages :

163 - 170

Peer reviewed :

Peer Reviewed verified by ORBi

Additional URL :

https://link.springer.com/content/pdf/10.1007/s10858-025-00464-z.pdf

Funders :

CNRS - Centre National de la Recherche Scientifique
EU - European Union

Funding text :

The authors acknowledge financial support by the European Commission through the FET-Open program, Grant agreement 899683 (HIRES-MULTIDYN). Financial support from the IR INFRANALYTICS FR2054 for conducting the research is gratefully acknowledged. The funders had no role in the design of the study, data collection or preparation of the manuscript.

Available on ORBi :

since 29 June 2026

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