The Chemical Shift Baseline for High-Pressure NMR Spectra of Proteins

Angew Chem Int Ed Engl. 2016 Jul 18;55(30):8757-60. doi: 10.1002/anie.201602054. Epub 2016 Jun 10.

Abstract

High-pressure (HP) NMR spectroscopy is an important method for detecting rare functional states of proteins by analyzing the pressure response of chemical shifts. However, for the analysis of the shifts it is mandatory to understand the origin of the observed pressure dependence. Here we present experimental HP NMR data on the (15) N-enriched peptide bond model, N-methylacetamide (NMA), in water, combined with quantum-chemical computations of the magnetic parameters using a pressure-sensitive solvation model. Theoretical analysis of NMA and the experimentally used internal reference standard 4,4-dimethyl-4-silapentane-1-sulfonic (DSS) reveal that a substantial part of observed shifts can be attributed to purely solvent-induced electronic polarization of the backbone. DSS is only marginally responsive to pressure changes and is therefore a reliable sensor for variations in the local magnetic field caused by pressure-induced changes of the magnetic susceptibility of the solvent.

Keywords: NMR spectroscopy; computational chemistry; high-pressure chemistry; isotopes; proteins.

Publication types

  • Research Support, Non-U.S. Gov't

MeSH terms

  • Acetamides / chemistry
  • Alkanesulfonic Acids / chemistry
  • Nitrogen Isotopes / chemistry
  • Nuclear Magnetic Resonance, Biomolecular*
  • Pressure
  • Proteins / chemistry*
  • Quantum Theory
  • Solvents / chemistry
  • Trimethylsilyl Compounds / chemistry

Substances

  • Acetamides
  • Alkanesulfonic Acids
  • Nitrogen Isotopes
  • Nitrogen-15
  • Proteins
  • Solvents
  • Trimethylsilyl Compounds
  • 3-(trimethylsilyl)propanesulfonic acid
  • N-methylacetamide