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Filtering the NMR Spectra of Mixtures by Coordination to Paramagnetic Cu(2+)

[Image: see text] The paramagnetic spin relaxation (PSR) filter allows the selective NMR signal suppression of components in mixtures according to their complexation ability to a paramagnetic ion. It relies on the faster relaxation of nuclei in paramagnetic environments and thus is complementary to...

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Autores principales: Correa, Juan, Garcia-Barandela, Ana, Socias-Pinto, Llorenç, Fernandez-Megia, Eduardo
Formato: Online Artículo Texto
Lenguaje:English
Publicado: American Chemical Society 2022
Acceso en línea:https://www.ncbi.nlm.nih.gov/pmc/articles/PMC9366733/
https://www.ncbi.nlm.nih.gov/pubmed/35895678
http://dx.doi.org/10.1021/acs.analchem.2c01983
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author Correa, Juan
Garcia-Barandela, Ana
Socias-Pinto, Llorenç
Fernandez-Megia, Eduardo
author_facet Correa, Juan
Garcia-Barandela, Ana
Socias-Pinto, Llorenç
Fernandez-Megia, Eduardo
author_sort Correa, Juan
collection PubMed
description [Image: see text] The paramagnetic spin relaxation (PSR) filter allows the selective NMR signal suppression of components in mixtures according to their complexation ability to a paramagnetic ion. It relies on the faster relaxation of nuclei in paramagnetic environments and thus is complementary to classical diffusion and relaxation filters. So far, the PSR filter has established Gd(3+) as the sole PSR agent, restricting the paramagnetic filtering repertoire. Herein, we present Cu(2+) as a robust PSR agent with characteristic filtering properties. While Gd(3+) depends on unspecific ion-pair interactions with anionic components, Cu(2+) stands out for filtering species via ordered coordination complexes. An evaluation of the paramagnetic effect of Cu(2+) over more than 50 small molecules and polymers has unveiled different sensitivities to Cu(2+) (especially high for pyridines, diamines, polyamines, and amino alcohols) and precise filtering conditions for mixtures ((1)H, COSY, and HMQC) that were challenged with a test bed of commercial drugs. The advantage of integrating Cu(2+) and Gd(3+) for the stepwise PSR filtering of complex mixtures is also shown.
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spelling pubmed-93667332022-08-12 Filtering the NMR Spectra of Mixtures by Coordination to Paramagnetic Cu(2+) Correa, Juan Garcia-Barandela, Ana Socias-Pinto, Llorenç Fernandez-Megia, Eduardo Anal Chem [Image: see text] The paramagnetic spin relaxation (PSR) filter allows the selective NMR signal suppression of components in mixtures according to their complexation ability to a paramagnetic ion. It relies on the faster relaxation of nuclei in paramagnetic environments and thus is complementary to classical diffusion and relaxation filters. So far, the PSR filter has established Gd(3+) as the sole PSR agent, restricting the paramagnetic filtering repertoire. Herein, we present Cu(2+) as a robust PSR agent with characteristic filtering properties. While Gd(3+) depends on unspecific ion-pair interactions with anionic components, Cu(2+) stands out for filtering species via ordered coordination complexes. An evaluation of the paramagnetic effect of Cu(2+) over more than 50 small molecules and polymers has unveiled different sensitivities to Cu(2+) (especially high for pyridines, diamines, polyamines, and amino alcohols) and precise filtering conditions for mixtures ((1)H, COSY, and HMQC) that were challenged with a test bed of commercial drugs. The advantage of integrating Cu(2+) and Gd(3+) for the stepwise PSR filtering of complex mixtures is also shown. American Chemical Society 2022-07-27 2022-08-09 /pmc/articles/PMC9366733/ /pubmed/35895678 http://dx.doi.org/10.1021/acs.analchem.2c01983 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 Correa, Juan
Garcia-Barandela, Ana
Socias-Pinto, Llorenç
Fernandez-Megia, Eduardo
Filtering the NMR Spectra of Mixtures by Coordination to Paramagnetic Cu(2+)
title Filtering the NMR Spectra of Mixtures by Coordination to Paramagnetic Cu(2+)
title_full Filtering the NMR Spectra of Mixtures by Coordination to Paramagnetic Cu(2+)
title_fullStr Filtering the NMR Spectra of Mixtures by Coordination to Paramagnetic Cu(2+)
title_full_unstemmed Filtering the NMR Spectra of Mixtures by Coordination to Paramagnetic Cu(2+)
title_short Filtering the NMR Spectra of Mixtures by Coordination to Paramagnetic Cu(2+)
title_sort filtering the nmr spectra of mixtures by coordination to paramagnetic cu(2+)
url https://www.ncbi.nlm.nih.gov/pmc/articles/PMC9366733/
https://www.ncbi.nlm.nih.gov/pubmed/35895678
http://dx.doi.org/10.1021/acs.analchem.2c01983
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