Gradient-purged isotope filter experiments for the detection of bound water in proteins

Yasmin Karimi-Nejad; Frank Löhr; Dick Schipper; Heinz Rüterjans; Rolf Boelens

doi:10.1016/S0009-2614(98)01421-3

Gradient-purged isotope filter experiments for the detection of bound water in proteins

Yasmin Karimi-Nejad, Frank Löhr, Dick Schipper, Heinz Rüterjans, Rolf Boelens

Biomolecular Mass Spectrometry and Proteomics, Bijvoet Center for Biomolecular Research and Utrecht Institute for Pharmaceutical Sciences, Utrecht University , Padualaan 8, 3584 CH Utrecht, The Netherlands.
Institut für Biophysikalische Chemie, Johann-Wolfgang-Goethe Universität Frankfurt, Biozentrum N230, Marie-Curie-Str. 9, D-60439 Frankfurt, Germany
Gist Brocades B.V., Research and Development, P.O. Box 1, NL-2600 MA Delft, The Netherlands

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

Abstract

A combination of gradient-purged isotope-filtered NMR experiments is presented, which allows for the detection of long-lived bound water molecules in proteins. The discrimination of direct water-protein exchange from NOE effects between bound water and protein protons is achieved by NOE/ROE cancellation during the mixing time in one of the otherwise identical experiments. The method was applied successfully to 13C/ 15N-labelled serine protease PB92, and allowed for the identification of 22 protein-water NOEs in this 269-residue enzyme.

Original language	English
Pages (from-to)	706-712
Journal	Chemical Physics Letters
Volume	300
Issue number	5
DOIs	https://doi.org/10.1016/S0009-2614(98)01421-3
Publication status	Published - 1 Feb 1999

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10.1016/S0009-2614(98)01421-3

http://adsabs.harvard.edu/abs/1999CPL...300..706K

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abstract = "A combination of gradient-purged isotope-filtered NMR experiments is presented, which allows for the detection of long-lived bound water molecules in proteins. The discrimination of direct water-protein exchange from NOE effects between bound water and protein protons is achieved by NOE/ROE cancellation during the mixing time in one of the otherwise identical experiments. The method was applied successfully to 13C/ 15N-labelled serine protease PB92, and allowed for the identification of 22 protein-water NOEs in this 269-residue enzyme.",

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AU - Karimi-Nejad, Yasmin

AU - Löhr, Frank

AU - Schipper, Dick

AU - Rüterjans, Heinz

AU - Boelens, Rolf

PY - 1999/2/1

Y1 - 1999/2/1

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AB - A combination of gradient-purged isotope-filtered NMR experiments is presented, which allows for the detection of long-lived bound water molecules in proteins. The discrimination of direct water-protein exchange from NOE effects between bound water and protein protons is achieved by NOE/ROE cancellation during the mixing time in one of the otherwise identical experiments. The method was applied successfully to 13C/ 15N-labelled serine protease PB92, and allowed for the identification of 22 protein-water NOEs in this 269-residue enzyme.

U2 - 10.1016/S0009-2614(98)01421-3

DO - 10.1016/S0009-2614(98)01421-3

M3 - Article

SN - 0009-2614

VL - 300

SP - 706

EP - 712

JO - Chemical Physics Letters

JF - Chemical Physics Letters

IS - 5

ER -

Gradient-purged isotope filter experiments for the detection of bound water in proteins

Abstract

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