Skip to main content
SpringerLink
Log in

13C Saturation-Transfer Difference (STD)-NMR Experiments Using INEPT Polarization Transfer

  • Original Paper
  • Published:
Applied Magnetic Resonance Aims and scope Submit manuscript

Abstract

Saturation-transfer difference (STD)-NMR spectroscopy has been widely used to screen potential ligands for binding to large receptor molecules. The STD-NMR experiment is typically based on a proton NMR spectrum, which can suffer from spectral overlap, leading to missing information in STD-based epitope mapping. Two-dimensional STD-NMR experiments can alleviate spectral overlap, but are time consuming. Here, we examine the feasibility of saturating protons in a receptor molecule and observing the STD effect on nearby carbon nuclei after transferring polarization from protons to carbons using the insensitive nuclei enhanced by polarization transfer (INEPT) pulse sequence. We show that under favorable conditions, a 1H→13C STD-INEPT experiment can give information similar to that obtained from a two-dimensional heteronuclear experiment, but in significantly less time. The STD-INEPT experiment could be especially useful when studying mixtures of ligands in which the peak positions in the proton and HSQC spectrum change significantly, and in particular, when using high-throughput, automated methods to analyze the data.

This is a preview of subscription content, log in via an institution to check access.

Access this article

Log in via an institution

Price excludes VAT (USA)
Tax calculation will be finalised during checkout.

Instant access to the full article PDF.

Institutional subscriptions

Fig. 1
Fig. 2
Fig. 3
Fig. 4
Fig. 5

Similar content being viewed by others

References

  1. J.L. Wagstaff, S.L. Taylor, M.J. Howard, Mol. BioSyst. 9, 571–577 (2013)

    Article  Google Scholar 

  2. M. Mayer, B. Meyer, B. Angew, Chem. Int. Ed. 38, 1784–1788 (1999)

    Article  Google Scholar 

  3. M. Mayer, B. Meyer, J. Am. Chem. Soc. 123, 6108–6117 (2001)

    Article  Google Scholar 

  4. J. Angulo, P.M. Enríquez-Navas, P.M. Nieto, Chem. Eur. J. 16, 7803–7812 (2010)

    Article  Google Scholar 

  5. Y. Zhang, H. Xu, A.M. Parsons, L.B. Casabianca, J. Phys. Chem. C 121, 24678–24686 (2017)

    Article  Google Scholar 

  6. Y. Zhang, H. Xu, L.B. Casabianca, Magn. Reson. Chem. 56, 1054–1060 (2018)

    Article  Google Scholar 

  7. Y. Zhang, L.B. Casabianca, J. Phys. Chem. Lett. 9, 6921–6925 (2018)

    Article  Google Scholar 

  8. A. Bax, D.G. Davis, J. Magn. Reson. 65, 355–360 (1985)

    ADS  Google Scholar 

  9. A.G. Palmer III, J. Cavanagh, P.E. Wright, M. Rance, J. Magn. Reson. 93, 151–170 (1991)

    ADS  Google Scholar 

  10. L.E. Kay, P. Keifer, T. Saarinen, J. Am. Chem. Soc. 114, 10663–10665 (1992)

    Article  Google Scholar 

  11. J. Schleucher, M. Schwendinger, M. Sattler, P. Schmidt, O. Schedletzky, S.J. Glaser, O.W. Sorensen, C. Griesinger, J. Biomol. NMR 4, 301–306 (1994)

    Article  Google Scholar 

  12. C. Räuber, S. Berger, Magn. Reson. Chem. 48, 91–93 (2010)

    Google Scholar 

  13. T. Diercks, J.P. Ribeiro, F.J. Cañada, S. André, J. Jiménez-Barbero, H.-J. Gabius, Chem. Eur. J. 15, 5666–5668 (2010)

    Article  Google Scholar 

  14. H. Min, G. Sekar, C. Hilty, ChemMedChem. 10, 1559–1563 (2015)

    Article  Google Scholar 

Download references

Acknowledgements

This work was supported by the National Science Foundation (grants CHE-1751529 and CHE-1725919). DL was supported by the Clemson Chemistry Research Experiences for Undergraduates grant from the NSF (CHE-1560300).

Author information

Author notes

  1. Danielle Lustig

    Present address: Department of Chemistry, University of Puget Sound, 1500 N. Warner Street, Tacoma, WA, 98416, USA

Authors and Affiliations

  1. Department of Chemistry, Clemson University, Clemson, SC, USA

    Hui Xu, Danielle Lustig & Leah B. Casabianca

Authors
  1. Hui Xu
    View author publications

    You can also search for this author in PubMed Google Scholar

  2. Danielle Lustig
    View author publications

    You can also search for this author in PubMed Google Scholar

  3. Leah B. Casabianca
    View author publications

    You can also search for this author in PubMed Google Scholar

Contributions

All authors designed experiments, HX and DL performed experiments, all authors analyzed data, LBC wrote the manuscript, all authors commented on the manuscript and approved the final version of the manuscript.

Corresponding author

Correspondence to Leah B. Casabianca.

Additional information

Publisher's Note

Springer Nature remains neutral with regard to jurisdictional claims in published maps and institutional affiliations.

Rights and permissions

Reprints and permissions

About this article

Check for updates. Verify currency and authenticity via CrossMark

Cite this article

Xu, H., Lustig, D. & Casabianca, L.B. 13C Saturation-Transfer Difference (STD)-NMR Experiments Using INEPT Polarization Transfer. Appl Magn Reson 51, 277–286 (2020). https://doi.org/10.1007/s00723-019-01182-0

Download citation

  • Received:

  • Revised:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s00723-019-01182-0

Search

Navigation