A 13C-detected 15N double-quantum NMR experiment to probe arginine side-chain guanidinium 15Nη chemical shifts

Arginine side-chains are often key for enzyme catalysis, protein–ligand and protein–protein interactions. The importance of arginine stems from the ability of the terminal guanidinium group to form many key interactions, such as hydrogen bonds and salt bridges, as well as its perpetual positive char...

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Bibliographic Details
Published inJournal of biomolecular NMR Vol. 69; no. 3; pp. 123 - 132
Main Authors Mackenzie, Harold W., Hansen, D. Flemming
Format Journal Article
LanguageEnglish
Published Dordrecht Springer Netherlands 01.11.2017
Springer Nature B.V
Subjects
Arginine
Biochemistry
Biological and Medical Physics
Biophysics
Catalysis
Chains
Chemical bonds
Coherence
Deuterium
Evolution
Experiments
Hydrogen bonding
Hydrogen bonds
Hydrogen storage
Lysozyme
NMR
Nuclear magnetic resonance
Nuclei
Physics
Physics and Astronomy
Protein interaction
Proteins
Quantum phenomena
Spectroscopy/Spectrometry
Double-quantum coherence
Isotope shifts
Arginine side-chains
Conformational exchange
13-Carbon-detected NMR
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Summary:Arginine side-chains are often key for enzyme catalysis, protein–ligand and protein–protein interactions. The importance of arginine stems from the ability of the terminal guanidinium group to form many key interactions, such as hydrogen bonds and salt bridges, as well as its perpetual positive charge. We present here an arginine 13 C ζ -detected NMR experiment in which a double-quantum coherence involving the two 15 N η nuclei is evolved during the indirect chemical shift evolution period. As the precession frequency of the double-quantum coherence is insensitive to exchange of the two 15 N η ; this new approach is shown to eliminate the previously deleterious line broadenings of 15 N η resonances caused by the partially restricted rotation about the C ζ –N ε bond. Consequently, sharp and well-resolved 15 N η resonances can be observed. The utility of the presented method is demonstrated on the L99A mutant of the 19 kDa protein T4 lysozyme, where the measurement of small chemical shift perturbations, such as one-bond deuterium isotope shifts, of the arginine amine 15 N η nuclei becomes possible using the double-quantum experiment.
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ISSN:0925-2738
1573-5001
DOI:10.1007/s10858-017-0137-2