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Enhanced signal dispersion in saturation transfer difference experiments by conversion to a 1D-STD-homodecoupled spectrum

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Abstract

The saturation transfer difference (STD) experiment is a rich source of information on topological aspects of ligand binding to a receptor. The epitope mapping is based on a magnetization transfer after signal saturation from the receptor to the ligand, where interproton distances permit this process. Signal overlap in the STD spectrum can cause difficulties to correctly assign and/or quantitate the measured enhancements. To address this issue we report here a modified version of the routine experiment and a processing scheme that provides a 1D-STD homodecoupled spectrum (i.e. an experiment in which all STD signals appear as singlets) with line widths similar to those in original STD spectrum. These refinements contribute to alleviate problems of signal overlap. The experiment is based on 2D-J-resolved spectroscopy, one of the fastest 2D experiments under conventional data sampling in the indirect dimension, and provides excellent sensitivity, a key factor for the difference experiments.

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Abbreviations

J-resolved:

J-resolved spectroscopy

STD:

saturation transfer difference

wg:

watergate

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Acknowledgements

The generous support by an EC Marie Curie Research Training Network grant (contract No. HRTN-CT-2005-019561) is gratefully acknowledged. Dr. Juan Carlos Cobas (Mestrelab research) is acknowledged for helping discussions regarding the processing of the STD-homodecoupled spectra.

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Authors and Affiliations

  1. Laboratorio Integral de Dinámica e Estructura de Biomoléculas José R. Carracido, Unidade de Resonancia Magnética, Edificio CACTUS, RIAIDT, Universidade de Santiago de Compostela, 15706, Santiago de Compostela, Spain

    Manuel Martín-Pastor & Marino Vega-Vázquez

  2. Dipartimento di Scienze Ambientali, Seconda Universitá degli Studi di Napoli, via Vivaldi 43, 81100, Caserta, Italy

    Antonia De Capua

  3. Departamento de Estructura y función de proteínas, Centro de Investigaciones Biológicas, CSIC, Ramiro de Maeztu 9, 28040, Madrid, Spain

    Angeles Canales & Jesús Jiménez-Barbero

  4. Institut für Physiologische Chemie, Tierärztliche Fakultät, Ludwig-Maximilians-Universität, Veterinärstr. 13, 80539, München, Germany

    Sabine André & Hans-Joachim Gabius

Authors
  1. Manuel Martín-Pastor
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  2. Marino Vega-Vázquez
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  3. Antonia De Capua
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  4. Angeles Canales
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  5. Sabine André
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  6. Hans-Joachim Gabius
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  7. Jesús Jiménez-Barbero
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Correspondence to Jesús Jiménez-Barbero.

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Martín-Pastor, M., Vega-Vázquez, M., De Capua, A. et al. Enhanced signal dispersion in saturation transfer difference experiments by conversion to a 1D-STD-homodecoupled spectrum. J Biomol NMR 36, 103–109 (2006). https://doi.org/10.1007/s10858-006-9055-4

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