3D accordion spectroscopy for measuring 15N and 13CO relaxation rates in poorly resolved NMR spectra

J Magn Reson. 1998 May;132(1):25-33. doi: 10.1006/jmre.1998.1374.

Abstract

An experimental approach for the measurement of nuclear magnetic spin relaxation rate constants that combines triple-resonance techniques and accordion spectroscopy is described. Pulse sequences are discussed for the measurement of backbone 15N and 13CO R1 relaxation rate constants. The three-dimensional HNCO triple-resonance technique is employed to gain improved spectral resolution over conventional two-dimensional methods by frequency labeling both the 15N and 13CO spins. Accordion spectroscopy is used to reduce the dimensionality of the relaxation experiment. The "negative-time accordion" approach (A. M. Mandel and A. G. Palmer (1994), J. Magn. Reson. A 110, 62-72) is used for extracting rate constants from the t1 interferograms. The experiments are demonstrated using a 13C/15N isotopically enriched sample of the third fibronectin type III domain of human tenascin.

Publication types

  • Research Support, Non-U.S. Gov't
  • Research Support, U.S. Gov't, P.H.S.

MeSH terms

  • Algorithms
  • Amino Acids / analysis
  • Carbon / analysis*
  • Carbon Isotopes
  • Carbon Monoxide / analysis*
  • Electron Spin Resonance Spectroscopy
  • Fibronectins / analysis*
  • Humans
  • Interferometry
  • Magnetic Resonance Spectroscopy*
  • Nitrogen / analysis*
  • Nitrogen Isotopes
  • Spectrum Analysis / methods
  • Tenascin / analysis*

Substances

  • Amino Acids
  • Carbon Isotopes
  • Fibronectins
  • Nitrogen Isotopes
  • Tenascin
  • Carbon
  • Carbon Monoxide
  • Nitrogen