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

Marcel Levien, Luming Yang, Alex Ham, Maik Reinhard, Michael John, Armin Purea, Jürgen Ganz, Thorsten Marquardsen, Igor Tkach, Tomas Orlando and Marina Bennati ()
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Marcel Levien: Max Planck Institute for Multidisciplinary Sciences
Luming Yang: Max Planck Institute for Multidisciplinary Sciences
Alex Ham: Max Planck Institute for Multidisciplinary Sciences
Maik Reinhard: Max Planck Institute for Multidisciplinary Sciences
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
Marina Bennati: Max Planck Institute for Multidisciplinary Sciences

Nature Communications, 2024, vol. 15, issue 1, 1-12

Abstract: 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.

Date: 2024
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DOI: 10.1038/s41467-024-50265-5

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