On the measurement of 15N-{1H} nuclear Overhauser effects. 2. Effects of the saturation scheme and water signal suppression

Fabien Ferrage, Amy Reichel, Shibani Battacharya, David Cowburn, Ranajeet Ghose

Research output: Contribution to journalArticle

30 Citations (Scopus)

Abstract

Measurement of steady-state 15N-{1H} nuclear Overhauser effects forms a cornerstone of most methods to determine protein backbone dynamics from spin-relaxation data, since it is the most reliable probe of very fast motions on the ps-ns timescale. We have, in two previous publications (J. Magn. Reson. 192 (2008) 302-313; J. Am. Chem. Soc. 131 (2009) 6048-6049) reevaluated spin-dynamics during steady-state (or "saturated") and reference experiments, both of which are required to determine the NOE ratio. Here we assess the performance of several windowed and windowless sequences to achieve effective saturation of protons in steady-state experiments. We also evaluate the influence of the residual water signal due to radiation damping on the NOE ratio. We suggest a recipe that allows one to determine steady-state 15N-{1H} NOE's without artifacts and with the highest possible accuracy.

Original languageEnglish (US)
Pages (from-to)294-303
Number of pages10
JournalJournal of Magnetic Resonance
Volume207
Issue number2
DOIs
StatePublished - Dec 2010

Fingerprint

Overhauser effect
Artifacts
Protons
retarding
Radiation
saturation
Spin dynamics
Water
water
Proteins
Damping
Experiments
spin dynamics
artifacts
damping
proteins
protons
probes
radiation

Keywords

  • Composite-pulse decoupling
  • Homogeneous master equation
  • Nuclear Overhauser effect
  • Protein dynamics
  • Radiation damping

ASJC Scopus subject areas

  • Nuclear and High Energy Physics
  • Biochemistry
  • Biophysics
  • Condensed Matter Physics
  • Medicine(all)

Cite this

On the measurement of 15N-{1H} nuclear Overhauser effects. 2. Effects of the saturation scheme and water signal suppression. / Ferrage, Fabien; Reichel, Amy; Battacharya, Shibani; Cowburn, David; Ghose, Ranajeet.

In: Journal of Magnetic Resonance, Vol. 207, No. 2, 12.2010, p. 294-303.

Research output: Contribution to journalArticle

Ferrage, Fabien ; Reichel, Amy ; Battacharya, Shibani ; Cowburn, David ; Ghose, Ranajeet. / On the measurement of 15N-{1H} nuclear Overhauser effects. 2. Effects of the saturation scheme and water signal suppression. In: Journal of Magnetic Resonance. 2010 ; Vol. 207, No. 2. pp. 294-303.
@article{c236a93191e64a54922e725af5ac1e85,
title = "On the measurement of 15N-{1H} nuclear Overhauser effects. 2. Effects of the saturation scheme and water signal suppression",
abstract = "Measurement of steady-state 15N-{1H} nuclear Overhauser effects forms a cornerstone of most methods to determine protein backbone dynamics from spin-relaxation data, since it is the most reliable probe of very fast motions on the ps-ns timescale. We have, in two previous publications (J. Magn. Reson. 192 (2008) 302-313; J. Am. Chem. Soc. 131 (2009) 6048-6049) reevaluated spin-dynamics during steady-state (or {"}saturated{"}) and reference experiments, both of which are required to determine the NOE ratio. Here we assess the performance of several windowed and windowless sequences to achieve effective saturation of protons in steady-state experiments. We also evaluate the influence of the residual water signal due to radiation damping on the NOE ratio. We suggest a recipe that allows one to determine steady-state 15N-{1H} NOE's without artifacts and with the highest possible accuracy.",
keywords = "Composite-pulse decoupling, Homogeneous master equation, Nuclear Overhauser effect, Protein dynamics, Radiation damping",
author = "Fabien Ferrage and Amy Reichel and Shibani Battacharya and David Cowburn and Ranajeet Ghose",
year = "2010",
month = "12",
doi = "10.1016/j.jmr.2010.09.014",
language = "English (US)",
volume = "207",
pages = "294--303",
journal = "Journal of Magnetic Resonance",
issn = "1090-7807",
publisher = "Academic Press Inc.",
number = "2",

}

TY - JOUR

T1 - On the measurement of 15N-{1H} nuclear Overhauser effects. 2. Effects of the saturation scheme and water signal suppression

AU - Ferrage, Fabien

AU - Reichel, Amy

AU - Battacharya, Shibani

AU - Cowburn, David

AU - Ghose, Ranajeet

PY - 2010/12

Y1 - 2010/12

N2 - Measurement of steady-state 15N-{1H} nuclear Overhauser effects forms a cornerstone of most methods to determine protein backbone dynamics from spin-relaxation data, since it is the most reliable probe of very fast motions on the ps-ns timescale. We have, in two previous publications (J. Magn. Reson. 192 (2008) 302-313; J. Am. Chem. Soc. 131 (2009) 6048-6049) reevaluated spin-dynamics during steady-state (or "saturated") and reference experiments, both of which are required to determine the NOE ratio. Here we assess the performance of several windowed and windowless sequences to achieve effective saturation of protons in steady-state experiments. We also evaluate the influence of the residual water signal due to radiation damping on the NOE ratio. We suggest a recipe that allows one to determine steady-state 15N-{1H} NOE's without artifacts and with the highest possible accuracy.

AB - Measurement of steady-state 15N-{1H} nuclear Overhauser effects forms a cornerstone of most methods to determine protein backbone dynamics from spin-relaxation data, since it is the most reliable probe of very fast motions on the ps-ns timescale. We have, in two previous publications (J. Magn. Reson. 192 (2008) 302-313; J. Am. Chem. Soc. 131 (2009) 6048-6049) reevaluated spin-dynamics during steady-state (or "saturated") and reference experiments, both of which are required to determine the NOE ratio. Here we assess the performance of several windowed and windowless sequences to achieve effective saturation of protons in steady-state experiments. We also evaluate the influence of the residual water signal due to radiation damping on the NOE ratio. We suggest a recipe that allows one to determine steady-state 15N-{1H} NOE's without artifacts and with the highest possible accuracy.

KW - Composite-pulse decoupling

KW - Homogeneous master equation

KW - Nuclear Overhauser effect

KW - Protein dynamics

KW - Radiation damping

UR - http://www.scopus.com/inward/record.url?scp=78649444679&partnerID=8YFLogxK

UR - http://www.scopus.com/inward/citedby.url?scp=78649444679&partnerID=8YFLogxK

U2 - 10.1016/j.jmr.2010.09.014

DO - 10.1016/j.jmr.2010.09.014

M3 - Article

C2 - 20951618

AN - SCOPUS:78649444679

VL - 207

SP - 294

EP - 303

JO - Journal of Magnetic Resonance

JF - Journal of Magnetic Resonance

SN - 1090-7807

IS - 2

ER -