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Slow-spinning low-sideband HR-MAS NMR spectroscopy: delicate analysis of biological samples

High-Resolution Magic-Angle Spinning (HR-MAS) NMR spectroscopy has become an extremely versatile analytical tool to study heterogeneous systems endowed with liquid-like dynamics. Spinning frequencies of several kHz are however required to obtain NMR spectra, devoid of spinning sidebands, with a reso...

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Autores principales: Renault, Marie, Shintu, Laetitia, Piotto, Martial, Caldarelli, Stefano
Formato: Online Artículo Texto
Lenguaje:English
Publicado: Nature Publishing Group 2013
Materias:
Acceso en línea:https://www.ncbi.nlm.nih.gov/pmc/articles/PMC3842542/
https://www.ncbi.nlm.nih.gov/pubmed/24284435
http://dx.doi.org/10.1038/srep03349
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author Renault, Marie
Shintu, Laetitia
Piotto, Martial
Caldarelli, Stefano
author_facet Renault, Marie
Shintu, Laetitia
Piotto, Martial
Caldarelli, Stefano
author_sort Renault, Marie
collection PubMed
description High-Resolution Magic-Angle Spinning (HR-MAS) NMR spectroscopy has become an extremely versatile analytical tool to study heterogeneous systems endowed with liquid-like dynamics. Spinning frequencies of several kHz are however required to obtain NMR spectra, devoid of spinning sidebands, with a resolution approaching that of purely isotropic liquid samples. An important limitation of the method is the large centrifugal forces that can damage the structure of the sample. In this communication, we show that optimizing the sample preparation, particularly avoiding air bubbles, and the geometry of the sample chamber of the HR-MAS rotor leads to high-quality low-sideband NMR spectra even at very moderate spinning frequencies, thus allowing the use of well-established solution-state NMR procedures for the characterization of small and highly dynamic molecules in the most fragile samples, such as live cells and intact tissues.
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spelling pubmed-38425422013-12-03 Slow-spinning low-sideband HR-MAS NMR spectroscopy: delicate analysis of biological samples Renault, Marie Shintu, Laetitia Piotto, Martial Caldarelli, Stefano Sci Rep Article High-Resolution Magic-Angle Spinning (HR-MAS) NMR spectroscopy has become an extremely versatile analytical tool to study heterogeneous systems endowed with liquid-like dynamics. Spinning frequencies of several kHz are however required to obtain NMR spectra, devoid of spinning sidebands, with a resolution approaching that of purely isotropic liquid samples. An important limitation of the method is the large centrifugal forces that can damage the structure of the sample. In this communication, we show that optimizing the sample preparation, particularly avoiding air bubbles, and the geometry of the sample chamber of the HR-MAS rotor leads to high-quality low-sideband NMR spectra even at very moderate spinning frequencies, thus allowing the use of well-established solution-state NMR procedures for the characterization of small and highly dynamic molecules in the most fragile samples, such as live cells and intact tissues. Nature Publishing Group 2013-11-28 /pmc/articles/PMC3842542/ /pubmed/24284435 http://dx.doi.org/10.1038/srep03349 Text en Copyright © 2013, Macmillan Publishers Limited. All rights reserved http://creativecommons.org/licenses/by-nc-nd/3.0/ This work is licensed under a Creative Commons Attribution-NonCommercial-NoDerivs 3.0 Unported License. To view a copy of this license, visit http://creativecommons.org/licenses/by-nc-nd/3.0/
spellingShingle Article
Renault, Marie
Shintu, Laetitia
Piotto, Martial
Caldarelli, Stefano
Slow-spinning low-sideband HR-MAS NMR spectroscopy: delicate analysis of biological samples
title Slow-spinning low-sideband HR-MAS NMR spectroscopy: delicate analysis of biological samples
title_full Slow-spinning low-sideband HR-MAS NMR spectroscopy: delicate analysis of biological samples
title_fullStr Slow-spinning low-sideband HR-MAS NMR spectroscopy: delicate analysis of biological samples
title_full_unstemmed Slow-spinning low-sideband HR-MAS NMR spectroscopy: delicate analysis of biological samples
title_short Slow-spinning low-sideband HR-MAS NMR spectroscopy: delicate analysis of biological samples
title_sort slow-spinning low-sideband hr-mas nmr spectroscopy: delicate analysis of biological samples
topic Article
url https://www.ncbi.nlm.nih.gov/pmc/articles/PMC3842542/
https://www.ncbi.nlm.nih.gov/pubmed/24284435
http://dx.doi.org/10.1038/srep03349
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