Boosting <sup>1</sup> H and <sup>13</sup> C NMR signals by orders of magnitude on a bench

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., 80-MHz <sup>1</sup>H frequency), with rapidly increasing access to NMR through benchtop systems, but also sometimes for higher-field NMR systems from 300 MHz to 1.2 GHz. Hyperpolarization by dissolution dynamic nuclear polarization (dDNP) can address this sensitivity limitation. However, dDNP implies massive and complex cryogenic and high-field instrumentation, which cannot be installed on the bench. We introduce here a compact helium-free 1-T tabletop polarizer as a simple and low-cost alternative. After freezing and polarizing the frozen analyte solutions at 77 K, we demonstrate <sup>1</sup>H signal enhancement factors of 100, with rapid 1-s buildup times. The high polarization is subsequently transferred by <sup>1</sup>H→<sup>13</sup>C cross polarization (CP) to <sup>13</sup>C spins. Such a simple benchtop polarizer, in combination with hyperpolarizing solid matrices (HYPSOs), may open the way to replenishable hyperpolarization throughout multiple liquid-state NMR experiments.

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Publication Details

Journal
Science Advances
Published
2024-12-04
DOI
https://doi.org/10.1126/sciadv.adq3780
Citations
8
Primary Topic
Advanced NMR Techniques and Applications
Type
article
Field-Weighted Citation Impact
1.93

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article

Boosting 1 H and 13 C NMR signals by orders of magnitude on a bench

Roberto Melzi, Armin Purea, Daniel Banks, Sami Jannin et al.
8 citations
Science Advances
Advanced NMR Techniques and Applications
1.93
article

Boosting 1 H and 13 C NMR signals by orders of magnitude on a bench

Roberto Melzi, Armin Purea, Daniel Banks, Sami Jannin, Quentin Stern, Ewoud Vaneeckhaute, James Kempf, Chloé Thieuleux, Charlotte Bocquelet, Laurent Veyre, Nathan Rougier, Huu-Nghia Le
article en
8 citations

Abstract

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., 80-MHz <sup>1</sup>H frequency), with rapidly increasing access to NMR through benchtop systems, but also sometimes for higher-field NMR systems from 300 MHz to 1.2 GHz. Hyperpolarization by dissolution dynamic nuclear polarization (dDNP) can address this sensitivity limitation. However, dDNP implies massive and complex cryogenic and high-field instrumentation, which cannot be installed on the bench. We introduce here a compact helium-free 1-T tabletop polarizer as a simple and low-cost alternative. After freezing and polarizing the frozen analyte solutions at 77 K, we demonstrate <sup>1</sup>H signal enhancement factors of 100, with rapid 1-s buildup times. The high polarization is subsequently transferred by <sup>1</sup>H→<sup>13</sup>C cross polarization (CP) to <sup>13</sup>C spins. Such a simple benchtop polarizer, in combination with hyperpolarizing solid matrices (HYPSOs), may open the way to replenishable hyperpolarization throughout multiple liquid-state NMR experiments.

Science AdvancesVol. 10(49)
Université Claude Bernard Lyon 1 (FR), Centre National de la Recherche Scientifique (FR), Bruker (United States) (US), École d'Ingénieurs en Chimie et Sciences du Numérique (FR)
Université Claude Bernard Lyon 1
Affordable and clean energy
Openalex Percentile: Top 14%
Advanced NMR Techniques and Applications
1.93
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