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Blahut, J.* ; Brandl, M.J.* ; Pradhan, T.* ; Reif, B. ; Tošner, Z.*

Sensitivity-enhanced multidimensional solid-state NMR spectroscopy by optimal-control-based transverse mixing sequences.

J. Am. Chem. Soc. 144, 17336-17340 (2022)
Postprint DOI PMC
Open Access Green
Recently, proton-detected magic-angle spinning (MAS) solid-state nuclear magnetic resonance (NMR) spectroscopy has become an attractive tool to study the structure and dynamics of insoluble proteins at atomic resolution. The sensitivity of the employed multidimensional experiments can be systematically improved when both transversal components of the magnetization are transferred simultaneously after an evolution period. The method of preservation of equivalent pathways has been explored in solution-state NMR; however, it does not find widespread application due to relaxation issues connected with increased molecular size. We present here for the first time heteronuclear transverse mixing sequences for correlation experiments at moderate and fast MAS frequencies. Optimal control allows to boost the signal-to-noise ratio (SNR) beyond the expected factor of 2 for each indirect dimension. In addition to the carbon-detected sensitivity-enhanced 2D NCA experiment, we present a novel proton-detected, doubly sensitivity-enhanced 3D hCANH pulse sequence for which we observe a 3-fold improvement in SNR compared to the conventional experimental implementation. The sensitivity gain turned out to be essential to unambiguously characterize a minor fibril polymorph of a human lambda-III immunoglobulin light chain protein that escaped detection so far.
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Publikationstyp Artikel: Journalartikel
Dokumenttyp Wissenschaftlicher Artikel
Korrespondenzautor
ISSN (print) / ISBN 0002-7863
e-ISSN 1520-5126
Zeitschrift Journal of the American Chemical Society
Quellenangaben Band: 144, Heft: 38, Seiten: 17336-17340 Artikelnummer: , Supplement: ,
Verlag American Chemical Society (ACS)
Nichtpatentliteratur Publikationen
Begutachtungsstatus Peer reviewed
Institut(e) Institute of Structural Biology (STB)
Förderungen Leibniz-Rechenzentrum
Grantová Agentura České Republiky
Ministerstvo Školství, Mládeže a Tělovýchovy
Deutsche Forschungsgemeinschaft
Helmholtz-Gemeinschaft
European Regional Development Fund-Project “UP CIISB