Dynamic Nuclear Polarization NMR as a new tool to investigate the nature of organic compounds occluded in plant silica particles

Abstract The determination of the chemical nature of the organic matter associated with phytoliths remains a challenge. This difficulty mainly stems from amounts of organic carbon (C) that are often well below the detection limit of traditional spectroscopic tools. Conventional solid-state 13C Nucle...

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Autores principales: Armand Masion, Anne Alexandre, Fabio Ziarelli, Stéphane Viel, Guaciara M. Santos
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Publicado: Nature Portfolio 2017
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Acceso en línea:https://doaj.org/article/4daaa52d1a8445c29e643323b605d5cd
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spelling oai:doaj.org-article:4daaa52d1a8445c29e643323b605d5cd2021-12-02T12:32:39ZDynamic Nuclear Polarization NMR as a new tool to investigate the nature of organic compounds occluded in plant silica particles10.1038/s41598-017-03659-z2045-2322https://doaj.org/article/4daaa52d1a8445c29e643323b605d5cd2017-06-01T00:00:00Zhttps://doi.org/10.1038/s41598-017-03659-zhttps://doaj.org/toc/2045-2322Abstract The determination of the chemical nature of the organic matter associated with phytoliths remains a challenge. This difficulty mainly stems from amounts of organic carbon (C) that are often well below the detection limit of traditional spectroscopic tools. Conventional solid-state 13C Nuclear Magnetic Resonance (NMR) is widely used to examine the nature and structure of organic molecules, but its inherent low sensitivity prohibits the observation of diluted samples. The recent advent of commercial microwave source in the terahertz range triggered a renewed interest in the Dynamic Nuclear Polarization (DNP) technique to improve the signal to noise ratio of solid-state NMR experiments. With this technique, the 13C spectrum of a phytolith sample containing 0.1% w/w C was obtained overnight with sufficient quality to permit a semi-quantitative analysis of the organic matter, showing the presence of peptides and carbohydrates as predominant compounds. Considering the natural abundance of the 13C isotope, this experiment demonstrates that DNP NMR is sufficiently sensitive to observe spin systems present in amounts as low as a few tens of ppm.Armand MasionAnne AlexandreFabio ZiarelliStéphane VielGuaciara M. SantosNature PortfolioarticleMedicineRScienceQENScientific Reports, Vol 7, Iss 1, Pp 1-7 (2017)
institution DOAJ
collection DOAJ
language EN
topic Medicine
R
Science
Q
spellingShingle Medicine
R
Science
Q
Armand Masion
Anne Alexandre
Fabio Ziarelli
Stéphane Viel
Guaciara M. Santos
Dynamic Nuclear Polarization NMR as a new tool to investigate the nature of organic compounds occluded in plant silica particles
description Abstract The determination of the chemical nature of the organic matter associated with phytoliths remains a challenge. This difficulty mainly stems from amounts of organic carbon (C) that are often well below the detection limit of traditional spectroscopic tools. Conventional solid-state 13C Nuclear Magnetic Resonance (NMR) is widely used to examine the nature and structure of organic molecules, but its inherent low sensitivity prohibits the observation of diluted samples. The recent advent of commercial microwave source in the terahertz range triggered a renewed interest in the Dynamic Nuclear Polarization (DNP) technique to improve the signal to noise ratio of solid-state NMR experiments. With this technique, the 13C spectrum of a phytolith sample containing 0.1% w/w C was obtained overnight with sufficient quality to permit a semi-quantitative analysis of the organic matter, showing the presence of peptides and carbohydrates as predominant compounds. Considering the natural abundance of the 13C isotope, this experiment demonstrates that DNP NMR is sufficiently sensitive to observe spin systems present in amounts as low as a few tens of ppm.
format article
author Armand Masion
Anne Alexandre
Fabio Ziarelli
Stéphane Viel
Guaciara M. Santos
author_facet Armand Masion
Anne Alexandre
Fabio Ziarelli
Stéphane Viel
Guaciara M. Santos
author_sort Armand Masion
title Dynamic Nuclear Polarization NMR as a new tool to investigate the nature of organic compounds occluded in plant silica particles
title_short Dynamic Nuclear Polarization NMR as a new tool to investigate the nature of organic compounds occluded in plant silica particles
title_full Dynamic Nuclear Polarization NMR as a new tool to investigate the nature of organic compounds occluded in plant silica particles
title_fullStr Dynamic Nuclear Polarization NMR as a new tool to investigate the nature of organic compounds occluded in plant silica particles
title_full_unstemmed Dynamic Nuclear Polarization NMR as a new tool to investigate the nature of organic compounds occluded in plant silica particles
title_sort dynamic nuclear polarization nmr as a new tool to investigate the nature of organic compounds occluded in plant silica particles
publisher Nature Portfolio
publishDate 2017
url https://doaj.org/article/4daaa52d1a8445c29e643323b605d5cd
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