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Off-the-Shelf Gd(NO(3))(3) as an Efficient High-Spin Metal Ion Polarizing Agent for Magic Angle Spinning Dynamic Nuclear Polarization

[Image: see text] Magic angle spinning nuclear magnetic resonance spectroscopy experiments are widely employed in the characterization of solid media. The approach is incredibly versatile but deleteriously suffers from low sensitivity, which may be alleviated by adopting dynamic nuclear polarization...

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Autores principales: Elliott, Stuart J., Duff, Benjamin B., Taylor-Hughes, Ashlea R., Cheney, Daniel J., Corley, John P., Paul, Subhradip, Brookfield, Adam, Pawsey, Shane, Gajan, David, Aspinall, Helen C., Lesage, Anne, Blanc, Frédéric
Formato: Online Artículo Texto
Lenguaje:English
Publicado: American Chemical Society 2022
Acceso en línea:https://www.ncbi.nlm.nih.gov/pmc/articles/PMC9421651/
https://www.ncbi.nlm.nih.gov/pubmed/35973071
http://dx.doi.org/10.1021/acs.jpcb.2c04184
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author Elliott, Stuart J.
Duff, Benjamin B.
Taylor-Hughes, Ashlea R.
Cheney, Daniel J.
Corley, John P.
Paul, Subhradip
Brookfield, Adam
Pawsey, Shane
Gajan, David
Aspinall, Helen C.
Lesage, Anne
Blanc, Frédéric
author_facet Elliott, Stuart J.
Duff, Benjamin B.
Taylor-Hughes, Ashlea R.
Cheney, Daniel J.
Corley, John P.
Paul, Subhradip
Brookfield, Adam
Pawsey, Shane
Gajan, David
Aspinall, Helen C.
Lesage, Anne
Blanc, Frédéric
author_sort Elliott, Stuart J.
collection PubMed
description [Image: see text] Magic angle spinning nuclear magnetic resonance spectroscopy experiments are widely employed in the characterization of solid media. The approach is incredibly versatile but deleteriously suffers from low sensitivity, which may be alleviated by adopting dynamic nuclear polarization methods, resulting in large signal enhancements. Paramagnetic metal ions such as Gd(3+) have recently shown promising results as polarizing agents for (1)H, (13)C, and (15)N nuclear spins. We demonstrate that the widely available and inexpensive chemical agent Gd(NO(3))(3) achieves significant signal enhancements for the (13)C and (15)N nuclear sites of [2-(13)C,(15)N]glycine at 9.4 T and ∼105 K. Analysis of the signal enhancement profiles at two magnetic fields, in conjunction with electron paramagnetic resonance data, reveals the solid effect to be the dominant signal enhancement mechanism. The signal amplification obtained paves the way for efficient dynamic nuclear polarization without the need for challenging synthesis of Gd(3+) polarizing agents.
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spelling pubmed-94216512022-08-30 Off-the-Shelf Gd(NO(3))(3) as an Efficient High-Spin Metal Ion Polarizing Agent for Magic Angle Spinning Dynamic Nuclear Polarization Elliott, Stuart J. Duff, Benjamin B. Taylor-Hughes, Ashlea R. Cheney, Daniel J. Corley, John P. Paul, Subhradip Brookfield, Adam Pawsey, Shane Gajan, David Aspinall, Helen C. Lesage, Anne Blanc, Frédéric J Phys Chem B [Image: see text] Magic angle spinning nuclear magnetic resonance spectroscopy experiments are widely employed in the characterization of solid media. The approach is incredibly versatile but deleteriously suffers from low sensitivity, which may be alleviated by adopting dynamic nuclear polarization methods, resulting in large signal enhancements. Paramagnetic metal ions such as Gd(3+) have recently shown promising results as polarizing agents for (1)H, (13)C, and (15)N nuclear spins. We demonstrate that the widely available and inexpensive chemical agent Gd(NO(3))(3) achieves significant signal enhancements for the (13)C and (15)N nuclear sites of [2-(13)C,(15)N]glycine at 9.4 T and ∼105 K. Analysis of the signal enhancement profiles at two magnetic fields, in conjunction with electron paramagnetic resonance data, reveals the solid effect to be the dominant signal enhancement mechanism. The signal amplification obtained paves the way for efficient dynamic nuclear polarization without the need for challenging synthesis of Gd(3+) polarizing agents. American Chemical Society 2022-08-16 2022-08-25 /pmc/articles/PMC9421651/ /pubmed/35973071 http://dx.doi.org/10.1021/acs.jpcb.2c04184 Text en © 2022 The Authors. Published by American Chemical Society https://creativecommons.org/licenses/by/4.0/Permits the broadest form of re-use including for commercial purposes, provided that author attribution and integrity are maintained (https://creativecommons.org/licenses/by/4.0/).
spellingShingle Elliott, Stuart J.
Duff, Benjamin B.
Taylor-Hughes, Ashlea R.
Cheney, Daniel J.
Corley, John P.
Paul, Subhradip
Brookfield, Adam
Pawsey, Shane
Gajan, David
Aspinall, Helen C.
Lesage, Anne
Blanc, Frédéric
Off-the-Shelf Gd(NO(3))(3) as an Efficient High-Spin Metal Ion Polarizing Agent for Magic Angle Spinning Dynamic Nuclear Polarization
title Off-the-Shelf Gd(NO(3))(3) as an Efficient High-Spin Metal Ion Polarizing Agent for Magic Angle Spinning Dynamic Nuclear Polarization
title_full Off-the-Shelf Gd(NO(3))(3) as an Efficient High-Spin Metal Ion Polarizing Agent for Magic Angle Spinning Dynamic Nuclear Polarization
title_fullStr Off-the-Shelf Gd(NO(3))(3) as an Efficient High-Spin Metal Ion Polarizing Agent for Magic Angle Spinning Dynamic Nuclear Polarization
title_full_unstemmed Off-the-Shelf Gd(NO(3))(3) as an Efficient High-Spin Metal Ion Polarizing Agent for Magic Angle Spinning Dynamic Nuclear Polarization
title_short Off-the-Shelf Gd(NO(3))(3) as an Efficient High-Spin Metal Ion Polarizing Agent for Magic Angle Spinning Dynamic Nuclear Polarization
title_sort off-the-shelf gd(no(3))(3) as an efficient high-spin metal ion polarizing agent for magic angle spinning dynamic nuclear polarization
url https://www.ncbi.nlm.nih.gov/pmc/articles/PMC9421651/
https://www.ncbi.nlm.nih.gov/pubmed/35973071
http://dx.doi.org/10.1021/acs.jpcb.2c04184
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