Sensitive and simplified: a combinatorial acquisition of five distinct 2D constant-time(13)C-H-1 NMR protein correlation spectra

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  • Yuichi Yoshimura, Lifemat West Japan Branch, Chuo Ku, Osaka University, Hiroshima University
  • ,
  • Frans A. A. Mulder

A procedure is presented for the substantial simplification of 2D constant-time(13)C-H-1 heteronuclear single-quantum correlation (HSQC) spectra of(13)C-enriched proteins. In this approach, a single pulse sequence simultaneously records eight sub-spectra wherein the phases of the NMR signals depend on spin topology. Signals from different chemical groups are then stratified into different sub-spectra through linear combination based on Hadamard encoding of(13)CH(n)multiplicity (n = 1, 2, and 3) and the chemical nature of neighboring(13)C nuclei (aliphatic, carbonyl/carboxyl, aromatic). This results in five sets of 2D NMR spectra containing mutually exclusive signals from: (i)C-13(beta)-(1)H(beta)correlations of asparagine and aspartic acid,C-13(gamma)-(1)H(gamma)correlations of glutamine and glutamic acid, and(13)C(alpha)-(1)H(alpha)correlations of glycine, (ii)C-13(alpha)-(1)H(alpha)correlations of all residues but glycine, and (iii)C-13(beta)-(1)H(beta)correlations of phenylalanine, tyrosine, histidine, and tryptophan, and the remaining (iv) aliphatic(13)CH(2)and (v) aliphatic(13)CH/(13)CH(3)resonances. As HSQC is a common element of many NMR experiments, the spectral simplification proposed in this article can be straightforwardly implemented in experiments for resonance assignment and structure determination and should be of widespread utility.

Original languageEnglish
JournalJournal of Biomolecular NMR
Number of pages12
ISSN0925-2738
DOIs
Publication statusE-pub ahead of print - 2020

    Research areas

  • C-13 chemical shifts, Constant-time HSQC, Multiplicity editing, Scalar coupling, Selective observation, HETERONUCLEAR SHIFT-CORRELATION, SELECTIVE H-1-N-15 CORRELATIONS, TRIPLE-RESONANCE EXPERIMENTS, SPIN-SYSTEM TOPOLOGIES, DEPT SEQUENCE, C-H, ACID, ASSIGNMENT, MUSIC, SPECTROSCOPY

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