Boosting the resolution of multidimensional NMR spectra by complete removal of proton spin multiplicities

Abstract Over decades multidimensional NMR spectroscopy has become an indispensable tool for structure elucidation of natural products, peptides and medium sized to large proteins. Heteronuclear single quantum coherence (HSQC) spectroscopy is one of the work horses in that field often used to map st...

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Autores principales:	Peyman Sakhaii, Bojan Bohorc, Uwe Schliedermann, Wolfgang Bermel
Formato:	article
Lenguaje:	EN
Publicado:	Nature Portfolio 2021
Materias:	Medicine R Science Q
Acceso en línea:	https://doaj.org/article/a23813772e2a48ecaf1ad1749b0892f6
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spelling	oai:doaj.org-article:a23813772e2a48ecaf1ad1749b0892f62021-11-08T10:54:52ZBoosting the resolution of multidimensional NMR spectra by complete removal of proton spin multiplicities10.1038/s41598-021-01041-82045-2322https://doaj.org/article/a23813772e2a48ecaf1ad1749b0892f62021-11-01T00:00:00Zhttps://doi.org/10.1038/s41598-021-01041-8https://doaj.org/toc/2045-2322Abstract Over decades multidimensional NMR spectroscopy has become an indispensable tool for structure elucidation of natural products, peptides and medium sized to large proteins. Heteronuclear single quantum coherence (HSQC) spectroscopy is one of the work horses in that field often used to map structural connectivity between protons and carbons or other hetero nuclei. In overcrowded HSQC spectra, proton multiplet structures of cross peaks set a limit to the power of resolution and make a straightforward assignment difficult. In this work, we provide a solution to improve these penalties by completely removing the proton spin multiplet structure of HSQC cross peaks. Previously reported sideband artefacts are diminished leading to HSQC spectra with singlet responses for all types of proton multiplicities. For sideband suppression, the idea of restricted random delay (RRD) in chunk interrupted data acquisition is introduced and exemplified. The problem of irreducible residual doublet splitting of diastereotopic CH2 groups is simply solved by using a phase sensitive JRES approach in conjunction with echo processing and real time broadband homodecoupling (BBHD) HSQC, applied as a 3D experiment. Advantages and limitations of the method is presented and discussed.Peyman SakhaiiBojan BohorcUwe SchliedermannWolfgang BermelNature PortfolioarticleMedicineRScienceQENScientific Reports, Vol 11, Iss 1, Pp 1-9 (2021)
institution	DOAJ
collection	DOAJ
language	EN
topic	Medicine R Science Q
spellingShingle	Medicine R Science Q Peyman Sakhaii Bojan Bohorc Uwe Schliedermann Wolfgang Bermel Boosting the resolution of multidimensional NMR spectra by complete removal of proton spin multiplicities
description	Abstract Over decades multidimensional NMR spectroscopy has become an indispensable tool for structure elucidation of natural products, peptides and medium sized to large proteins. Heteronuclear single quantum coherence (HSQC) spectroscopy is one of the work horses in that field often used to map structural connectivity between protons and carbons or other hetero nuclei. In overcrowded HSQC spectra, proton multiplet structures of cross peaks set a limit to the power of resolution and make a straightforward assignment difficult. In this work, we provide a solution to improve these penalties by completely removing the proton spin multiplet structure of HSQC cross peaks. Previously reported sideband artefacts are diminished leading to HSQC spectra with singlet responses for all types of proton multiplicities. For sideband suppression, the idea of restricted random delay (RRD) in chunk interrupted data acquisition is introduced and exemplified. The problem of irreducible residual doublet splitting of diastereotopic CH2 groups is simply solved by using a phase sensitive JRES approach in conjunction with echo processing and real time broadband homodecoupling (BBHD) HSQC, applied as a 3D experiment. Advantages and limitations of the method is presented and discussed.
format	article
author	Peyman Sakhaii Bojan Bohorc Uwe Schliedermann Wolfgang Bermel
author_facet	Peyman Sakhaii Bojan Bohorc Uwe Schliedermann Wolfgang Bermel
author_sort	Peyman Sakhaii
title	Boosting the resolution of multidimensional NMR spectra by complete removal of proton spin multiplicities
title_short	Boosting the resolution of multidimensional NMR spectra by complete removal of proton spin multiplicities
title_full	Boosting the resolution of multidimensional NMR spectra by complete removal of proton spin multiplicities
title_fullStr	Boosting the resolution of multidimensional NMR spectra by complete removal of proton spin multiplicities
title_full_unstemmed	Boosting the resolution of multidimensional NMR spectra by complete removal of proton spin multiplicities
title_sort	boosting the resolution of multidimensional nmr spectra by complete removal of proton spin multiplicities
publisher	Nature Portfolio
publishDate	2021
url	https://doaj.org/article/a23813772e2a48ecaf1ad1749b0892f6
work_keys_str_mv	AT peymansakhaii boostingtheresolutionofmultidimensionalnmrspectrabycompleteremovalofprotonspinmultiplicities AT bojanbohorc boostingtheresolutionofmultidimensionalnmrspectrabycompleteremovalofprotonspinmultiplicities AT uweschliedermann boostingtheresolutionofmultidimensionalnmrspectrabycompleteremovalofprotonspinmultiplicities AT wolfgangbermel boostingtheresolutionofmultidimensionalnmrspectrabycompleteremovalofprotonspinmultiplicities
_version_	1718442552808439808

Boosting the resolution of multidimensional NMR spectra by complete removal of proton spin multiplicities

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