TY - JOUR

T1 - Total Correlation Spectroscopy across All NMR-Active Nuclei by Mixing at Zero Field

AU - Zhukov, Ivan V.

AU - Kiryutin, Alexey S.

AU - Ferrage, Fabien

AU - Buntkowsky, Gerd

AU - Yurkovskaya, Alexandra V.

AU - Ivanov, Konstantin L.

N1 - Publisher Copyright: Copyright © 2020 American Chemical Society. Copyright: Copyright 2020 Elsevier B.V., All rights reserved.

PY - 2020/9/3

Y1 - 2020/9/3

N2 - Multidimensional nuclear magnetic resonance (NMR) is based on a combination of well-established building blocks for polarization transfer. These blocks are used to design correlation experiments through one or a few chemical bonds or through space. Here, we introduce a building block that enables polarization transfer across all NMR-active nuclei in a coupled network of spins: isotropic mixing at zero and ultralow field (ZULF). Exploiting mixing under ZULF-NMR conditions, heteronuclear TOtal Correlation SpectroscopY (TOCSY) experiments were developed to highlight coupled spin networks. We demonstrate 1H-13C and 1H-15N correlations in ZULF-TOCSY spectra of labeled amino acids, which allow one to obtain cross-peaks among all heteronuclei belonging to the same coupled network, even when the direct interaction between them is negligible. We also demonstrate the potential of ZULF-TOCSY to analyze complex mixtures on a growth medium of isotope-labeled biomolecules. ZULF-TOCSY enables the quick identification of individual compounds in the mixture by their coupled spin networks. The ZULF-TOCSY method will lead to the development of a new toolbox of experiments to analyze complex mixtures by NMR.

AB - Multidimensional nuclear magnetic resonance (NMR) is based on a combination of well-established building blocks for polarization transfer. These blocks are used to design correlation experiments through one or a few chemical bonds or through space. Here, we introduce a building block that enables polarization transfer across all NMR-active nuclei in a coupled network of spins: isotropic mixing at zero and ultralow field (ZULF). Exploiting mixing under ZULF-NMR conditions, heteronuclear TOtal Correlation SpectroscopY (TOCSY) experiments were developed to highlight coupled spin networks. We demonstrate 1H-13C and 1H-15N correlations in ZULF-TOCSY spectra of labeled amino acids, which allow one to obtain cross-peaks among all heteronuclei belonging to the same coupled network, even when the direct interaction between them is negligible. We also demonstrate the potential of ZULF-TOCSY to analyze complex mixtures on a growth medium of isotope-labeled biomolecules. ZULF-TOCSY enables the quick identification of individual compounds in the mixture by their coupled spin networks. The ZULF-TOCSY method will lead to the development of a new toolbox of experiments to analyze complex mixtures by NMR.

KW - SENSITIVITY-ENHANCED DETECTION

KW - MAGNETIC-RESONANCE

KW - HYDROGEN-BONDS

KW - SPECTRA

KW - RELAXATION

KW - COHERENCE

KW - NETWORKS

KW - C-13

KW - H-1

UR - http://www.scopus.com/inward/record.url?scp=85090280809&partnerID=8YFLogxK

U2 - 10.1021/acs.jpclett.0c02032

DO - 10.1021/acs.jpclett.0c02032

M3 - Article

C2 - 32787308

AN - SCOPUS:85090280809

VL - 11

SP - 7291

EP - 7296

JO - Journal of Physical Chemistry Letters

JF - Journal of Physical Chemistry Letters

SN - 1948-7185

IS - 17

ER -