An efficient NMR method for the characterisation of 14N sites through indirect 13C detection

Nitrogen is one of the most abundant elements and plays a key role in the chemistry of biological systems. Despite its widespread distribution, the study of the naturally occurring isotope of nitrogen, 14 N (99.6%), has been relatively limited as it is a spin-1 nucleus that typically exhibits a larg...

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Bibliographic Details
Published in:Physical chemistry chemical physics : PCCP 2013-05, Vol.15 (2), p.7613-762
Main Authors: Jarvis, James A, Haies, Ibraheem M, Williamson, Philip T. F, Carravetta, Marina
Format: Article
Language:English
Subjects:
Biological and medical sciences
Biological Products - chemistry
Biopolymers - chemistry
Carbon Isotopes
Chemistry
Fundamental and applied biological sciences. Psychology
Glycine - chemistry
Magnetic Resonance Spectroscopy
Molecular biophysics
Nitrogen - chemistry
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Summary:Nitrogen is one of the most abundant elements and plays a key role in the chemistry of biological systems. Despite its widespread distribution, the study of the naturally occurring isotope of nitrogen, 14 N (99.6%), has been relatively limited as it is a spin-1 nucleus that typically exhibits a large quadrupolar interaction. Accordingly, most studies of nitrogen sites in biomolecules have been performed on samples enriched with 15 N, limiting the application of NMR to samples which can be isotopically enriched. This precludes the analysis of naturally occurring samples and results in the loss of the wealth of structural and dynamic information that the quadrupolar interaction can provide. Recently, several experimental approaches have been developed to characterize 14 N sites through their interaction with neighboring spy nuclei. Here we describe a novel version of these experiments whereby coherence between the 14 N site and the spy nucleus is mediated by the application of a moderate rf field to the 14 N. The resulting 13 C/ 14 N spectra show good sensitivity on natural abundance and labeled materials; whilst the 14 N lineshapes permit the quantitative analysis of the quadrupolar interaction. An efficient NMR methods for the characterisation of 14 N sites has been developed with efficiencies suitable for the quantitative analysis of biomolecular and natural abundance systems.
ISSN:1463-9076
1463-9084
DOI:10.1039/c3cp50787d