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research article

Characterization of different water pools in solid-state NMR protein samples

Boeckmann, Anja
•
Gardiennet, Carole
•
Verel, Rene
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2009
JOURNAL OF BIOMOLECULAR NMR

We observed and characterized two distinct signals originating from different pools of water protons in solid-state NMR protein samples, namely from crystal water which exchanges polarization with the protein (on the NMR timescale) and is located in the protein-rich fraction at the periphery of the magic-angle spinning (MAS) sample container, and supernatant water located close to the axis of the sample container. The polarization transfer between the water and the protein can be probed by two-dimensional exchange spectroscopy, and we show that the supernatant water does not interact with protein on the timescale of the experiments. The two water pools have different spectroscopic properties, including resonance frequency, longitudinal, transverse and rotating frame relaxation times. The supernatant water can be removed almost completely physically or can be frozen selectively. Both measures lead to an enhancement of the quality factor of the probe circuit, accompanied by an improvement of the experimental signal/noise, and greatly simplify solvent-suppression by substantially reducing the water signal. We also present a tool, which allows filling solid-state NMR sample containers in a more efficient manner, greatly reducing the amount of supernatant water and maximizing signal/noise.

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Type
research article
DOI
10.1007/s10858-009-9374-3
Web of Science ID

WOS:000270871600009

Author(s)
Boeckmann, Anja
Gardiennet, Carole
Verel, Rene
Hunkeler, Andreas
Loquet, Antoine
Pintacuda, Guido
Emsley, Lyndon  
Meier, Beat H.
Lesage, Anne
Date Issued

2009

Publisher

SPRINGER

Published in
JOURNAL OF BIOMOLECULAR NMR
Volume

45

Issue

3

Start page

319

End page

327

Subjects

Solid-state NMR

•

Water-protein polarization transfer

•

Microcrystalline protein

•

Chemical exchange

Editorial or Peer reviewed

REVIEWED

Written at

OTHER

EPFL units
LRM  
Available on Infoscience
January 8, 2015
Use this identifier to reference this record
https://infoscience.epfl.ch/handle/20.500.14299/110031
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