Sequential assignment of NMR spectra of peptides at natural isotopic abundance with zero- and ultra-low-field total correlation spectroscopy (ZULF-TOCSY)

Sequential assignment of NMR spectra of peptides at natural isotopic abundance with zero- and ultra-low-field total correlation spectroscopy (ZULF-TOCSY) Full article

Journal

Physical Chemistry Chemical Physics
ISSN: 1463-9076

Output data

Year: 2021, Volume: 23, Number: 16, Pages: 9715-9720 Pages count : 6 DOI: 10.1039/D0CP06337A

Authors

Kiryutin Alexey S. ¹ , Zhukov Ivan V. ¹ , Ferrage Fabien ² , Bodenhausen Geoffrey ² , Yurkovskaya Alexandra V. ¹ , Ivanov Konstantin L. ¹

Affiliations

1	International Tomography Center, Siberian Branch of the Russian Academy of Sciences and Novosibirsk State University, Novosibirsk, 630090, Russia.
2	Laboratoire des Biomolecules, LBM, Departement de Chimie, Ecole Normale Superieure, PSL University, Sorbonne Universite, CNRS, 75005 Paris, France

A novel method dubbed ZULF-TOCSY results from the combination of Zero and Ultra-Low Field (ZULF) with high-field, high-resolution NMR, leading to a generalization of the concept of total correlation spectroscopy (TOCSY). ZULF-TOCSY is a new building block for NMR methods, which has the unique property that the polarization is evenly distributed among all NMR-active nuclei such as 1H, 13C, 15N, 31P, etc., provided that they belong to the same coupling network, and provided that their relaxation is not too fast at low fields, as may occur in macromolecules. Here, we show that ZULF-TOCSY correlations can be observed for peptides at natural isotopic abundance, such as the protected hexapeptide Boc-Met-enkephalin. The analysis of ZULF-TOCSY spectra readily allows one to make sequential assignments, thus offering an alternative to established heteronuclear 2D experiments like HMBC. For Boc-Met-enkephalin, we show that ZULF-TOCSY allows one to observe all expected cross-peaks between carbonyl carbons and α-CH protons, while the popular HMBC method provides insufficient information.

Kiryutin A.S. , Zhukov I.V. , Ferrage F. , Bodenhausen G. , Yurkovskaya A.V. , Ivanov K.L.
Sequential assignment of NMR spectra of peptides at natural isotopic abundance with zero- and ultra-low-field total correlation spectroscopy (ZULF-TOCSY)
Physical Chemistry Chemical Physics. 2021. V.23. N16. P.9715-9720. DOI: 10.1039/D0CP06337A OpenAlex

Submitted:	Dec 8, 2020
Accepted:	Apr 9, 2021
Published online:	Apr 9, 2021

OpenAlex:

W3155568369

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