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

Autor: Stefano Caldarelli, Marie Renault, Martial Piotto, Laetitia Shintu
Přispěvatelé: Bruker Biospin, bruker, Institut de Chimie des Substances Naturelles (ICSN), Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)
Rok vydání: 2013
Předmět:
Zdroj: Scientific Reports
Scientific Reports, Nature Publishing Group, 2013, 3, pp.3349. ⟨10.1038/srep03349⟩
ISSN: 2045-2322
DOI: 10.1038/srep03349⟩
Popis: International audience; 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.
Databáze: OpenAIRE