Communication

Proton-Detected Solid-State NMR Spectroscopy of Natural-Abundance Peptide and Protein Pharmaceuticals†

  1. Donghua H. Zhou Dr.1,4,
  2. Gautam Shah1,
  3. Charles Mullen2,
  4. Dennis Sandoz3,
  5. Chad M. Rienstra Prof. Dr.1

Article first published online: 7 JAN 2009

DOI: 10.1002/anie.200801029

Issue

Angewandte Chemie International Edition

Angewandte Chemie International Edition

Volume 48, Issue 7, pages 1253–1256, February 2, 2009

Additional Information

How to Cite

Zhou, Donghua H., Shah, G., Mullen, C., Sandoz, D. and Rienstra, Chad M. (2009), Proton-Detected Solid-State NMR Spectroscopy of Natural-Abundance Peptide and Protein Pharmaceuticals. Angew. Chem. Int. Ed., 48: 1253–1256. doi: 10.1002/anie.200801029

Author Information

  1. 1

    Department of Chemistry, University of Illinois at Urbana-Champaign, Urbana, IL 61801 (USA), Fax: (+1) 217-244-4655 http://www.scs.uiuc.edu/∼rienstra

  2. 2

    Varian, Inc., Fort Collins, CO (USA)

  3. 3

    Varian, Inc., Palo Alto, CA (USA)

  4. 4

    Current address: Department of Physics, Oklahoma State University, OK 74078 (USA)

  1. †

    This research was supported by the National Institutes of Health (R01 GM-75937 to C.M.R). We thank John A. Stringer and Mircea Cormos (Varian, Inc.) for advice on probe performance.

Publication History

  1. Issue published online: 28 JAN 2009
  2. Article first published online: 7 JAN 2009
  3. Manuscript Revised: 25 SEP 2008
  4. Manuscript Received: 3 MAR 2008

Funded by

  • National Institutes of Health. Grant Number: R01 GM-75937

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Keywords:

  • insulin;
  • magic-angle spinning;
  • NMR spectroscopy;
  • proteins;
  • structure elucidation

Abstract

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The natural way: A sensitive NMR spectroscopic method is developed to obtain well-resolved two-dimensional spectra (15N–1H and 13C–1H) for natural-abundance (that is, without the need for isotopic enrichment) large-molecule samples, such as biopharmaceuticals. This method gives structural insights on two lyophilized aprotinin samples and three insulin samples in lyophilized, microcrystalline suspension formulation (red; see picture) and fibril (green) forms.

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