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An Optimized NMR Stripline for Sensitive Supercritical Fluid Chromatography-Nuclear Magnetic Resonance of Microliter Sample Volumes

[Image: see text] To optimize sensitivity, there has been an increasing interest in the miniaturization of NMR detectors. In our lab, a stripline NMR detector has been developed, which provides high resolution and is scalable to a large range of sample volumes. These features make it an ideal detect...

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Autores principales: van Meerten, Sebastiaan, van Zelst, Fleur, Tijssen, Koen, Kentgens, Arno
Formato: Online Artículo Texto
Lenguaje:English
Publicado: American Chemical Society 2020
Acceso en línea:https://www.ncbi.nlm.nih.gov/pmc/articles/PMC7547862/
https://www.ncbi.nlm.nih.gov/pubmed/32865394
http://dx.doi.org/10.1021/acs.analchem.0c01827
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author van Meerten, Sebastiaan
van Zelst, Fleur
Tijssen, Koen
Kentgens, Arno
author_facet van Meerten, Sebastiaan
van Zelst, Fleur
Tijssen, Koen
Kentgens, Arno
author_sort van Meerten, Sebastiaan
collection PubMed
description [Image: see text] To optimize sensitivity, there has been an increasing interest in the miniaturization of NMR detectors. In our lab, a stripline NMR detector has been developed, which provides high resolution and is scalable to a large range of sample volumes. These features make it an ideal detector for hyphenated techniques. In this manuscript, we demonstrate a stripline probe, which is designed for combining supercritical fluid chromatography (SFC) experiments with NMR. It features a novel stripline chip, designed to reduce the signal from the contact pads, which results in an improved lineshape. An external lock circuit provides stability over time to perform signal averaging or multidimensional experiments. As proof of concept, we demonstrate the SFC-NMR technique with this stripline probe using a mixture of cholesterol and cholestanol, which is relevant for studying cerebrotendinous xanthomatosis. Additionally, this probe makes it possible to record high-resolution spectra of samples with a high spin density. This means that it is possible to directly observe shifts due to the nuclear demagnetizing field in the “homomolecular” case, which is challenging using conventional probes due to broadening effects from radiation damping.
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spelling pubmed-75478622020-10-13 An Optimized NMR Stripline for Sensitive Supercritical Fluid Chromatography-Nuclear Magnetic Resonance of Microliter Sample Volumes van Meerten, Sebastiaan van Zelst, Fleur Tijssen, Koen Kentgens, Arno Anal Chem [Image: see text] To optimize sensitivity, there has been an increasing interest in the miniaturization of NMR detectors. In our lab, a stripline NMR detector has been developed, which provides high resolution and is scalable to a large range of sample volumes. These features make it an ideal detector for hyphenated techniques. In this manuscript, we demonstrate a stripline probe, which is designed for combining supercritical fluid chromatography (SFC) experiments with NMR. It features a novel stripline chip, designed to reduce the signal from the contact pads, which results in an improved lineshape. An external lock circuit provides stability over time to perform signal averaging or multidimensional experiments. As proof of concept, we demonstrate the SFC-NMR technique with this stripline probe using a mixture of cholesterol and cholestanol, which is relevant for studying cerebrotendinous xanthomatosis. Additionally, this probe makes it possible to record high-resolution spectra of samples with a high spin density. This means that it is possible to directly observe shifts due to the nuclear demagnetizing field in the “homomolecular” case, which is challenging using conventional probes due to broadening effects from radiation damping. American Chemical Society 2020-08-31 2020-10-06 /pmc/articles/PMC7547862/ /pubmed/32865394 http://dx.doi.org/10.1021/acs.analchem.0c01827 Text en This is an open access article published under a Creative Commons Non-Commercial No Derivative Works (CC-BY-NC-ND) Attribution License (http://pubs.acs.org/page/policy/authorchoice_ccbyncnd_termsofuse.html) , which permits copying and redistribution of the article, and creation of adaptations, all for non-commercial purposes.
spellingShingle van Meerten, Sebastiaan
van Zelst, Fleur
Tijssen, Koen
Kentgens, Arno
An Optimized NMR Stripline for Sensitive Supercritical Fluid Chromatography-Nuclear Magnetic Resonance of Microliter Sample Volumes
title An Optimized NMR Stripline for Sensitive Supercritical Fluid Chromatography-Nuclear Magnetic Resonance of Microliter Sample Volumes
title_full An Optimized NMR Stripline for Sensitive Supercritical Fluid Chromatography-Nuclear Magnetic Resonance of Microliter Sample Volumes
title_fullStr An Optimized NMR Stripline for Sensitive Supercritical Fluid Chromatography-Nuclear Magnetic Resonance of Microliter Sample Volumes
title_full_unstemmed An Optimized NMR Stripline for Sensitive Supercritical Fluid Chromatography-Nuclear Magnetic Resonance of Microliter Sample Volumes
title_short An Optimized NMR Stripline for Sensitive Supercritical Fluid Chromatography-Nuclear Magnetic Resonance of Microliter Sample Volumes
title_sort optimized nmr stripline for sensitive supercritical fluid chromatography-nuclear magnetic resonance of microliter sample volumes
url https://www.ncbi.nlm.nih.gov/pmc/articles/PMC7547862/
https://www.ncbi.nlm.nih.gov/pubmed/32865394
http://dx.doi.org/10.1021/acs.analchem.0c01827
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