Study of molecular interactions with 13C DNP-NMR

Lerche, Mathilde Hauge; Meier, Sebastián; Jensen, Pernille Rose; Baumann, Herbert; Petersen, Bent O.; Karlsson, Magnus; Duus, Jens Øllgaard; Ardenkjær-Larsen, Jan Henrik

doi:10.1016/j.jmr.2009.11.020

Cited by 61 publications

(65 citation statements)

References 35 publications

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“…In a proof-of-principle study, a HP ligand solution containing salicylate and ascorbate was mixed with human serum albumin. 38 In the presence of the receptor, resonances corresponding to salicylate were not seen, while the ascorbate resonances are clearly visible (Fig. 14A).…”

Section: Observing Fast Chemistry By Dnp-nmrmentioning

confidence: 99%

“…For example, the binding of salicylic acid and ascorbic acid to albumin was studied via polarization of the natural abundance small-molecules, while the effect of hydrophobic binding on T 1 was analyzed by polarization of natural abundance benzoic acid and mixing with varying concentrations of β-cyclodextrin. 38,54 …”

Section: Considerations For Dnp Probe Developmentmentioning

confidence: 99%

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Chemistry and biochemistry of¹³C hyperpolarized magnetic resonance using dynamic nuclear polarization

2014

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The study of transient chemical phenomena by conventional NMR has proved elusive, particularly for non-1H nuclei. For 13C, hyperpolarization using the dynamic nuclear polarization (DNP) technique has emerged as a powerful means to improve SNR. The recent development of rapid dissolution DNP methods has facilitated previously impossible in vitro and in vivo study of small molecules. This review presents the basics of the DNP technique, identification of appropriate DNP substrates, and approaches to increase hyperpolarized signal lifetimes. Also addressed are the biochemical events to which DNP-NMR has been applied, with descriptions of several probes that have met with in vivo success.

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Section: Observing Fast Chemistry By Dnp-nmrmentioning

confidence: 99%

Section: Considerations For Dnp Probe Developmentmentioning

confidence: 99%

Chemistry and biochemistry of¹³C hyperpolarized magnetic resonance using dynamic nuclear polarization

2014

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“…Furthermore, Lerche et al [80] applied hyperpolarised 13 C NMR screening as a competitive assay to characterise the binding of salicylate and ascorbate to human serum albumin. Signal enhancements were achieved using dynamic nuclear polarisation (DNP) 13 C NMR spectroscopy.…”

Section: Ligand-protein Interactionsmentioning

confidence: 99%

NMR Spectroscopy for Studying Interactions of Bioactive Molecules

Novak¹,

Jednačak²

2012

Physico-Chemical Methods in Drug Discovery and Development

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“…Cryogenically cooled detection systems should further improve the limits of detection and quantification by 13 C DNP-NMR by roughly four-fold. Even in the absence of high-field hyperpolarization and cryogenically cooled detection, dissolution DNP-NMR in the current set-up yields a sensitivity gain on the order of approximately 1000 relative to the state of high-field NMR spectrometers equipped with cryogenically cooled probes (27). Despite these vast sensitivity improvements relative to conventional NMR technology, quantitative in vitro DNP-NMR in this set-up has a limit of detection that is at least one order of magnitude poorer than for LC-MS set-ups, such as that used for validation in this study.…”

Section: Analytical Considerationsmentioning

confidence: 95%

Quantitative dynamic nuclear polarization‐NMR on blood plasma for assays of drug metabolism

Lerche¹,

Meier

Jensen³

et al. 2010

NMR in Biomedicine

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Analytical platforms for the fast detection, identification and quantification of circulating drugs with a narrow therapeutic range are vital in clinical pharmacology. As a result of low drug concentrations, analytical tools need to provide high sensitivity and specificity. Dynamic nuclear polarization-NMR (DNP-NMR) in the form of the hyperpolarization-dissolution method should afford the sensitivity and spectral resolution for the direct detection and quantification of numerous isotopically labeled circulating drugs and their metabolites in single liquid-state NMR transients. This study explores the capability of quantitative in vitro DNP-NMR to assay drug metabolites in blood plasma. The lower limit of detection for the anti-epileptic drug (13)C-carbamazepine and its pharmacologically active metabolite (13)C-carbamazepine-10,11-epoxide is 0.08 µg/mL in rabbit blood plasma analyzed by single-scan (13)C DNP-NMR. An internal standard is used for the accurate quantification of drug and metabolite. Comparison of quantitative DNP-NMR data with an established analytical method (liquid chromatography-mass spectrometry) yields a Pearson correlation coefficient r of 0.99. Notably, all DNP-NMR determinations were performed without analyte derivatization or sample purification other than plasma protein precipitation. Quantitative DNP-NMR is an emerging methodology which requires little sample preparation and yields quantitative data with high sensitivity for therapeutic drug monitoring.

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Study of molecular interactions with 13C DNP-NMR

Cited by 61 publications

References 35 publications

Chemistry and biochemistry of¹³C hyperpolarized magnetic resonance using dynamic nuclear polarization

Chemistry and biochemistry of¹³C hyperpolarized magnetic resonance using dynamic nuclear polarization

NMR Spectroscopy for Studying Interactions of Bioactive Molecules

Quantitative dynamic nuclear polarization‐NMR on blood plasma for assays of drug metabolism

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Study of molecular interactions with 13C DNP-NMR

Cited by 61 publications

References 35 publications

Chemistry and biochemistry of13C hyperpolarized magnetic resonance using dynamic nuclear polarization

Chemistry and biochemistry of13C hyperpolarized magnetic resonance using dynamic nuclear polarization

NMR Spectroscopy for Studying Interactions of Bioactive Molecules

Quantitative dynamic nuclear polarization‐NMR on blood plasma for assays of drug metabolism

Contact Info

Product

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About

Chemistry and biochemistry of¹³C hyperpolarized magnetic resonance using dynamic nuclear polarization

Chemistry and biochemistry of¹³C hyperpolarized magnetic resonance using dynamic nuclear polarization