Chapter 2 Recent Advances in Solvent Suppression for Solution NMR: A Practical Reference

doi:10.1016/S0066-4103(08)00402-X

Annual Reports on NMR Spectroscopy

Volume 66, 2009, Pages 33-76

https://doi.org/10.1016/S0066-4103(08)00402-X Get rights and content

Abstract

Recent advances in solvent suppression for liquids based NMR spectroscopy are explored. An emphasis on techniques developed over the past 10 years is provided including recommendations on sample preparation and spectrometer optimization. In addition, biologically relevant samples were used to demonstrate and compare the relative strengths/weaknesses of described techniques. This publication attempts to provide practical background and general knowledge for both novice and experienced users seeking to select and optimize the most appropriate tools for their NMR challenges.

Section snippets

Objectives

There are a fantastic number of exploratory manuscripts and reviews thoroughly covering aspects of biomolecular NMR and the relationship with solvent suppression over the last 30 years. Biochemically^a focused NMR spectroscopy has been developing for well over a half century.¹ Originally we had planned to cover all aspects of solvent suppression but were quickly forced to re-evaluate

Practicalities

The following sections attempt to quickly express some general NMR ‘rules of thumb’ that we have adopted. They are not meant to imply hard and fast rules or requirements to be imposed on all samples and spectroscopists (though some are certainly required at our facility), but instead simply methods we have found to effectively acquire consistent data in the most reasonable amount of time. As the saying goes, ‘Your mileage may vary’.

Suppression Pulse Sequences

The order of review was intended to be alphabetical with the exception of presaturation and water-eliminated Fourier transform (WEFT)/NOESY due to the importance of these sequences and comparisons to subsequent developments. Presaturation and WEFT (commonly referred to as 1D-NOESY) remain, for many groups, the ‘gold standard’ to which all other forms of suppression are compared. Suppression techniques prior to or during acquisition are considered. Suppression in the solid state⁶⁷ and

Comparisons, Conclusions, and Advice

All the suppression techniques worked well in reducing solvent by many orders of magnitude. Solvent suppression has become so effective that improvements on the order of only a few percent can be the deciding factor when trying to determine the ‘best’ method during comparisons.

We selected two samples for the sequence comparisons. The first sample was a 1 mM ubiquitin protein dissolved in 90% H₂O with 10% D₂O with 1 mM DSS as an internal reference. The sample was deliberatively shortened to 550

Acknowledgments

I would like to thank Kent Dixon for critical reading, Trent Bjorndahl (D. Wishart research group, Univ. of Alberta) for assistance and access to a cryogenically cooled probe on an 11.74T spectrometer to confirm the demagnetization field effects, John C. Lindon and David Neuhaus for correspondence over the years regarding solvent suppression developments, Frank Delaglio for discussions and patience on so many NMR techniques, George Gray for assistance with Varian's BioPack pulse sequences,

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For instance, exchanging H2O with D2O is known to stabilize compact conformations of both globular [1] and tubular proteins [2,3] and protect them against aggregation. For these reasons, solvent signal suppression becomes necessary under many circumstances [e.g., 4–12]. WATERGATE [13,14] sequences provide robust solvent signal suppression in NMR experiments, achieved by application of a pulsed field gradient pair, where all coherences not affected by a selective inversion pulse are rephased, while affected coherences are dephased and removed.
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Chapter 2 Recent Advances in Solvent Suppression for Solution NMR: A Practical Reference

Abstract

Section snippets

Objectives

Practicalities

Suppression Pulse Sequences

Comparisons, Conclusions, and Advice

Acknowledgments

Methods Enzymol.

J. Magn. Reson.

Progress in NMR Spectroscopy

Annual Reports on NMR Spectroscopy

J. Pharm. Biomed. Anal.

Progress in NMR Spectroscopy

Biochim. Biophys. Acta

FEBS Lett.

Biochem. Biophys. Res. Commun.

Journal of Magnetic Resonance

J. Magn. Reson.

J. Magn. Reson.

Progress in NMR Spectroscopy

Chemical Physics

J. Magn. Reson.

Progress in NMR Spectroscopy

Annual Reports on NMR Spectroscopy

Journal of Magnetic Resonance

Journal of Magnetic Resonance

J. Magn. Reson.

Curr. Opin. Struct. Biol.

J. Magn. Reson.

Progress in NMR Spectroscopy

Journal of Magnetic Resonance

Journal of Magnetic Resonance

J. Magn. Reson.

Journal of Magnetic Resonance

J. Magn. Reson. B

J. Magn. Reson.

Journal of Magnetic Resonance

Journal of Magnetic Resonance

Journal of Magnetic Resonance

Journal of Magnetic Resonance

J. Magn. Reson.

Journal of Magnetic Resonance

J. Magn. Reson.

J. Magn. Reson.

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Journal of Magnetic Resonance

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Journal of Magnetic Resonance

Journal of Magnetic Resonance

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Journal of Magnetic Resonance

J. Magn. Reson.