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Remarkable Levels of (15)N Polarization Delivered through SABRE into Unlabeled Pyridine, Pyrazine, or Metronidazole Enable Single Scan NMR Quantification at the mM Level

[Image: see text] While many drugs and metabolites contain nitrogen, harnessing their diagnostic (15)N NMR signature for their characterization is underutilized because of inherent detection difficulties. Here, we demonstrate how precise ultralow field signal amplification by reversible exchange (±0...

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Autores principales: Fekete, Marianna, Ahwal, Fadi, Duckett, Simon B.
Formato: Online Artículo Texto
Lenguaje:English
Publicado: American Chemical Society 2020
Acceso en línea:https://www.ncbi.nlm.nih.gov/pmc/articles/PMC7277555/
https://www.ncbi.nlm.nih.gov/pubmed/32383603
http://dx.doi.org/10.1021/acs.jpcb.0c02583
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author Fekete, Marianna
Ahwal, Fadi
Duckett, Simon B.
author_facet Fekete, Marianna
Ahwal, Fadi
Duckett, Simon B.
author_sort Fekete, Marianna
collection PubMed
description [Image: see text] While many drugs and metabolites contain nitrogen, harnessing their diagnostic (15)N NMR signature for their characterization is underutilized because of inherent detection difficulties. Here, we demonstrate how precise ultralow field signal amplification by reversible exchange (±0.2 mG) in conjunction parahydrogen and an iridium precatalyst of the form IrCl(COD)(NHC) with the coligand d(9)-benzylamine allows the naturally abundant (15)N NMR signatures of pyridine, pyrazine, metronidazole, and acetonitrile to be readily detected at 9.4 T in single NMR observations through >50% (15)N polarization levels. These signals allow for rapid and precise reagent quantification via a response that varies linearly over the 2–70 mM concentration range.
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spelling pubmed-72775552020-06-15 Remarkable Levels of (15)N Polarization Delivered through SABRE into Unlabeled Pyridine, Pyrazine, or Metronidazole Enable Single Scan NMR Quantification at the mM Level Fekete, Marianna Ahwal, Fadi Duckett, Simon B. J Phys Chem B [Image: see text] While many drugs and metabolites contain nitrogen, harnessing their diagnostic (15)N NMR signature for their characterization is underutilized because of inherent detection difficulties. Here, we demonstrate how precise ultralow field signal amplification by reversible exchange (±0.2 mG) in conjunction parahydrogen and an iridium precatalyst of the form IrCl(COD)(NHC) with the coligand d(9)-benzylamine allows the naturally abundant (15)N NMR signatures of pyridine, pyrazine, metronidazole, and acetonitrile to be readily detected at 9.4 T in single NMR observations through >50% (15)N polarization levels. These signals allow for rapid and precise reagent quantification via a response that varies linearly over the 2–70 mM concentration range. American Chemical Society 2020-05-08 2020-06-04 /pmc/articles/PMC7277555/ /pubmed/32383603 http://dx.doi.org/10.1021/acs.jpcb.0c02583 Text en Copyright © 2020 American Chemical Society This is an open access article published under a Creative Commons Attribution (CC-BY) License (http://pubs.acs.org/page/policy/authorchoice_ccby_termsofuse.html) , which permits unrestricted use, distribution and reproduction in any medium, provided the author and source are cited.
spellingShingle Fekete, Marianna
Ahwal, Fadi
Duckett, Simon B.
Remarkable Levels of (15)N Polarization Delivered through SABRE into Unlabeled Pyridine, Pyrazine, or Metronidazole Enable Single Scan NMR Quantification at the mM Level
title Remarkable Levels of (15)N Polarization Delivered through SABRE into Unlabeled Pyridine, Pyrazine, or Metronidazole Enable Single Scan NMR Quantification at the mM Level
title_full Remarkable Levels of (15)N Polarization Delivered through SABRE into Unlabeled Pyridine, Pyrazine, or Metronidazole Enable Single Scan NMR Quantification at the mM Level
title_fullStr Remarkable Levels of (15)N Polarization Delivered through SABRE into Unlabeled Pyridine, Pyrazine, or Metronidazole Enable Single Scan NMR Quantification at the mM Level
title_full_unstemmed Remarkable Levels of (15)N Polarization Delivered through SABRE into Unlabeled Pyridine, Pyrazine, or Metronidazole Enable Single Scan NMR Quantification at the mM Level
title_short Remarkable Levels of (15)N Polarization Delivered through SABRE into Unlabeled Pyridine, Pyrazine, or Metronidazole Enable Single Scan NMR Quantification at the mM Level
title_sort remarkable levels of (15)n polarization delivered through sabre into unlabeled pyridine, pyrazine, or metronidazole enable single scan nmr quantification at the mm level
url https://www.ncbi.nlm.nih.gov/pmc/articles/PMC7277555/
https://www.ncbi.nlm.nih.gov/pubmed/32383603
http://dx.doi.org/10.1021/acs.jpcb.0c02583
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