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Overhauser enhanced liquid state nuclear magnetic resonance spectroscopy in one and two dimensions

Author

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  • Marcel Levien

    (Max Planck Institute for Multidisciplinary Sciences
    Georg-August-University
    École Polytechnique Fédérale de Lausanne (EPFL))

  • Luming Yang

    (Max Planck Institute for Multidisciplinary Sciences)

  • Alex Ham

    (Max Planck Institute for Multidisciplinary Sciences)

  • Maik Reinhard

    (Max Planck Institute for Multidisciplinary Sciences
    Georg-August-University)

  • Michael John

    (Georg-August-University)

  • Armin Purea

    (Bruker Biospin GmbH)

  • Jürgen Ganz

    (Bruker Biospin GmbH)

  • Thorsten Marquardsen

    (Bruker Biospin GmbH)

  • Igor Tkach

    (Max Planck Institute for Multidisciplinary Sciences)

  • Tomas Orlando

    (Max Planck Institute for Multidisciplinary Sciences
    National High Magnetic Field Laboratory)

  • Marina Bennati

    (Max Planck Institute for Multidisciplinary Sciences
    Georg-August-University)

Abstract

Nuclear magnetic resonance (NMR) is fundamental in the natural sciences, from chemical analysis and structural biology, to medicine and physics. Despite its enormous achievements, one of its most severe limitations is the low sensitivity, which arises from the small population difference of nuclear spin states. Methods such as dissolution dynamic nuclear polarization and parahydrogen induced hyperpolarization can enhance the NMR signal by several orders of magnitude, however, their intrinsic limitations render multidimensional hyperpolarized liquid-state NMR a challenge. Here, we report an instrumental design for 9.4 Tesla liquid-state dynamic nuclear polarization that enabled enhanced high-resolution NMR spectra in one and two-dimensions for small molecules, including drugs and metabolites. Achieved enhancements of up to two orders of magnitude translate to signal acquisition gains up to a factor of 10,000. We show that hyperpolarization can be transferred between nuclei, allowing DNP-enhanced two-dimensional 13C–13C correlation experiments at 13C natural abundance. The enhanced sensitivity opens up perspectives for structural determination of natural products or characterization of drugs, available in small quantities. The results provide a starting point for a broader implementation of DNP in liquid-state NMR.

Suggested Citation

  • Marcel Levien & Luming Yang & Alex Ham & Maik Reinhard & Michael John & Armin Purea & Jürgen Ganz & Thorsten Marquardsen & Igor Tkach & Tomas Orlando & Marina Bennati, 2024. "Overhauser enhanced liquid state nuclear magnetic resonance spectroscopy in one and two dimensions," Nature Communications, Nature, vol. 15(1), pages 1-12, December.
    • Handle: RePEc:nat:natcom:v:15:y:2024:i:1:d:10.1038_s41467-024-50265-5
    DOI: 10.1038/s41467-024-50265-5
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    References listed on IDEAS

    as
    1. Danhua Dai & Xianwei Wang & Yiwei Liu & Xiao-Liang Yang & Clemens Glaubitz & Vasyl Denysenkov & Xiao He & Thomas Prisner & Jiafei Mao, 2021. "Room-temperature dynamic nuclear polarization enhanced NMR spectroscopy of small biological molecules in water," Nature Communications, Nature, vol. 12(1), pages 1-15, December.
    2. Michael A. Hope & Bernardine L. D. Rinkel & Anna B. Gunnarsdóttir & Katharina Märker & Svetlana Menkin & Subhradip Paul & Ivan V. Sergeyev & Clare P. Grey, 2020. "Selective NMR observation of the SEI–metal interface by dynamic nuclear polarisation from lithium metal," Nature Communications, Nature, vol. 11(1), pages 1-8, December.
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