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Practical considerations over spectral quality in solid state NMR spectroscopy of soluble proteins

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Abstract

Great theoretical and methodological advances are pushing the limits of resolution and sensitivity in solid state NMR (SSNMR). However, sample preparation remains a critical issue for the success of an experiment. The factors affecting spectral quality in SSNMR samples are discussed, examining cases encountered in the literature and presenting new experimental data. A discussion on resolution and sensitivity in sedimented solutes is framed in this context.

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Notes

  1. This value is calculated by comparing the Direct Polarization signal intensity of the present sample to the same spectrum of a sample comprising of 6 mg of lyophilized ubiquitin, rehydrated to 400 mg/ml with a glycerol/water mixture. A concentration value of 833 mg/ml can be calculated under the assumption that conc = (ρsol − ρsolv)/(1 − ρsolv/ρprot) (Chatelier and Minton 1987).

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Acknowledgments

Discussions with Lyndon Emsley, Moreno Lelli, Guido Pintacuda and Robert G. Griffin on resolution in SSNMR and with Vito Calderone on crystallization conditions are acknowledged. This work has been supported by Ente Cassa di Risparmio di Firenze, the European Commission (contract Bio-NMR no. 261863), and Instruct, part of the European Strategy Forum on Research Infrastructures (ESFRI) and supported by national member subscriptions. Specifically, we thank the EU ESFRI Instruct Core Centre CERM, Italy.

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Authors and Affiliations

  1. Center for Magnetic Resonance (CERM), University of Florence, Via L. Sacconi 6, 50019, Sesto Fiorentino, FI, Italy

    Marco Fragai, Claudio Luchinat, Giacomo Parigi & Enrico Ravera

  2. Department of Chemistry, University of Florence, Via della Lastruccia 3, 50019, Sesto Fiorentino, FI, Italy

    Marco Fragai, Claudio Luchinat, Giacomo Parigi & Enrico Ravera

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  1. Marco Fragai
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  2. Claudio Luchinat
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  3. Giacomo Parigi
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  4. Enrico Ravera
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Corresponding author

Correspondence to Claudio Luchinat.

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Fragai, M., Luchinat, C., Parigi, G. et al. Practical considerations over spectral quality in solid state NMR spectroscopy of soluble proteins. J Biomol NMR 57, 155–166 (2013). https://doi.org/10.1007/s10858-013-9776-0

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  • DOI: https://doi.org/10.1007/s10858-013-9776-0

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