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

doi:10.1016/j.jmr.2010.09.014

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

Biochemistry

Research output: Contribution to journal › Article › peer-review

35 Scopus citations

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 language	English (US)
Pages (from-to)	294-303
Number of pages	10
Journal	Journal of Magnetic Resonance
Volume	207
Issue number	2
DOIs	https://doi.org/10.1016/j.jmr.2010.09.014
State	Published - Dec 2010

Keywords

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

ASJC Scopus subject areas

Biophysics
Biochemistry
Nuclear and High Energy Physics
Condensed Matter Physics

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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",

note = "Funding Information: We thank Geoffrey Bodenhausen for his careful reading of and critical comments on this manuscript. This work has been partially supported by a Grant MCB0843141 from the National Science Foundation . A grant from the NIH 5G12 RR03060 is acknowledged for partial support of the core facilities at CCNY. FF, SB, DC and RG are members of the New York Structural Biology Center, a STAR center supported by the New York State Office for Science, Technology and Academic Research. ",

year = "2010",

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doi = "10.1016/j.jmr.2010.09.014",

language = "English (US)",

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pages = "294--303",

journal = "Journal of Magnetic Resonance",

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AU - Ferrage, Fabien

AU - Reichel, Amy

AU - Battacharya, Shibani

AU - Cowburn, David

AU - Ghose, Ranajeet

N1 - Funding Information: We thank Geoffrey Bodenhausen for his careful reading of and critical comments on this manuscript. This work has been partially supported by a Grant MCB0843141 from the National Science Foundation . A grant from the NIH 5G12 RR03060 is acknowledged for partial support of the core facilities at CCNY. FF, SB, DC and RG are members of the New York Structural Biology Center, a STAR center supported by the New York State Office for Science, Technology and Academic Research.

PY - 2010/12

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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.

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KW - Protein dynamics

KW - Radiation damping

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