Bullet-DNP Enables NMR Spectroscopy of Pyruvate and Amino Acids at Nanomolar to Low Micromolar Concentrations

Hyperpolarized pyruvate is a widely used marker to track metabolism in vivo and a benchmark molecule for hyperpolarization methods. Here, we show how a combination of improved bullet-DNP instrumentation, an optimized sample preparation and a further sensitivity increase via a <sup>13</sup>C-<sup>1</sup>H polarization transfer after dissolution enable the observation of pyruvate at a concentration of 250 nM immediately after dissolution. At this concentration, the experiment employs a total mass of pyruvate of only 20 ng or 180 pmol. If the concentration is increased to 45 μM, pyruvate may be detected 1 min after dissolution with a signal-to-noise ratio exceeding 50. The procedure can be extended to observe a mixture of amino acids at low micromolar concentrations.

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Publication Details

Journal
Analytical Chemistry
Published
2024-09-03
DOI
https://doi.org/10.1021/acs.analchem.4c00618
Citations
6
Primary Topic
Advanced NMR Techniques and Applications
Type
article
Field-Weighted Citation Impact
1.44

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article

Bullet-DNP Enables NMR Spectroscopy of Pyruvate and Amino Acids at Nanomolar to Low Micromolar Concentrations

Karel Kouřil, Pooja Narwal, Sami Jannin, Alvar D. Gossert et al.
6 citations
Analytical Chemistry
Advanced NMR Techniques and Applications
1.44
article

Bullet-DNP Enables NMR Spectroscopy of Pyruvate and Amino Acids at Nanomolar to Low Micromolar Concentrations

Karel Kouřil, Pooja Narwal, Sami Jannin, Alvar D. Gossert, Masoud Minaei, Benno Meier, Nils Lorz
article en
6 citations

Abstract

Hyperpolarized pyruvate is a widely used marker to track metabolism in vivo and a benchmark molecule for hyperpolarization methods. Here, we show how a combination of improved bullet-DNP instrumentation, an optimized sample preparation and a further sensitivity increase via a <sup>13</sup>C-<sup>1</sup>H polarization transfer after dissolution enable the observation of pyruvate at a concentration of 250 nM immediately after dissolution. At this concentration, the experiment employs a total mass of pyruvate of only 20 ng or 180 pmol. If the concentration is increased to 45 μM, pyruvate may be detected 1 min after dissolution with a signal-to-noise ratio exceeding 50. The procedure can be extended to observe a mixture of amino acids at low micromolar concentrations.

Analytical ChemistryVol. 96(37)
Université Claude Bernard Lyon 1 (FR), Karlsruhe Institute of Technology (DE), École Normale Supérieure de Lyon (FR), Centre National de la Recherche Scientifique (FR), ETH Zurich (CH), Centre de RMN à Très Hauts Champs de Lyon (FR)
Helmholtz-Gemeinschaft, Deutsche Forschungsgemeinschaft, H2020 European Research Council
Clean water and sanitation
Openalex Percentile: Top 20%
Advanced NMR Techniques and Applications
1.44
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