In dissolution-dynamic nuclear polarization, nuclear spins are hyperpolarized at cryogenic temperatures using radicals and microwave irradiation. The hyperpolarized solid is dissolved with hot solvent and the solution is transferred to a secondary magnet where strongly enhanced magnetic resonance signals are observed. Here we present a method for transferring the hyperpolarized solid. A bullet containing the frozen, hyperpolarized sample is ejected using pressurized helium gas, and shot into a receiving structure in the secondary magnet, where the bullet is retained and the polarized solid is dissolved rapidly. The transfer takes approximately 70 ms. A solenoid, wound along the entire transfer path ensures adiabatic transfer and limits radical-induced low-field relaxation. The method is fast and scalable towards small volumes suitable for high-resolution nuclear magnetic resonance spectroscopy while maintaining high concentrations of the target molecule. Polarization levels of approximately 30% have been observed for 1-C-labelled pyruvic acid in solution.
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http://dx.doi.org/10.1038/s41467-019-09726-5 | DOI Listing |
Anal Chem
January 2025
Institute for Bioengineering of Catalonia (IBEC), Barcelona Institute of Science and Technology (BIST), 08028 Barcelona, Spain.
Nuclear magnetic resonance (NMR) spectroscopy is a valuable diagnostic tool limited by low sensitivity due to low nuclear spin polarization. Hyperpolarization techniques, such as dissolution dynamic nuclear polarization, significantly enhance sensitivity, enabling real-time tracking of cellular metabolism. However, traditional high-field NMR systems and bioreactor platforms pose challenges, including the need for specialized equipment and fixed sample volumes.
View Article and Find Full Text PDFJ Am Chem Soc
January 2025
Nantes Université, CNRS, CEISAM, UMR 6230, F-44000 Nantes, France.
NMR is a central tool in the field of metabolomics, thanks to its ability to provide valuable structural and quantitative information with high precision. Most NMR-based metabolomics studies rely on 1D H detection, which is heavily limited by strong peak overlap. C NMR benefits from a wider spectral dispersion and narrower signal line width but is barely used in metabolomics due to its low sensitivity.
View Article and Find Full Text PDFProg Nucl Magn Reson Spectrosc
December 2024
Laboratoire de Chimie et Biochimie Pharmacologiques et Toxicologiques Université Paris Cité, 45 rue des Saints Pères, 75006 Paris, France. Electronic address:
In recent years, there has been remarkable progress in the field of dissolution dynamic nuclear polarization (D-DNP). This method has shown significant potential for enhancing nuclear polarization by over 10,000 times, resulting in a substantial increase in sensitivity. The unprecedented signal enhancements achieved with D-DNP have opened new possibilities for in vitro analysis.
View Article and Find Full Text PDFJ Am Chem Soc
December 2024
Laboratoire des biomolécules, LBM, Département de chimie, Ecole normale supérieure, CNRS, PSL University, Sorbonne Université, Paris 75005, France.
The hyperpolarization of biological samples using dissolution dynamic nuclear polarization (dDNP) has become an attractive method for the monitoring of fast chemical and enzymatic reactions using NMR by taking advantage of a large signal increase. This approach is actively developing but still needs key methodological breakthroughs to be used as an analytical method for the monitoring of complex networks of simultaneous metabolic pathways. In this article, we use the deceptively simple example of glucose-6-phosphate (G6P) oxidation reaction by the enzyme G6P dehydrogenase (G6PDH) to discuss some important methodological aspects of dDNP kinetic experiments, such as its robustness and its ability to provide repeatable results as well as the capacity of this time-resolved methodology to test kinetic models and hypotheses and to provide reliable parameter estimates.
View Article and Find Full Text PDFSci Adv
December 2024
Universite Claude Bernard Lyon 1, CNRS, ENS Lyon, CRMN UMR 5082, 69100 Villeurbanne, France.
Sensitivity is often the Achilles' heel of liquid-state nuclear magnetic resonance (NMR) experiments. This problem is perhaps most pressing at the lowest fields (e.g.
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