ArticleJournal of magnetic resonance (San Diego, Calif. : 1997)2014
Paramagnet induced signal quenching in MAS-DNP experiments in frozen homogeneous solutions.
Article in Journal of magnetic resonance (San Diego, Calif. : 1997), 2014. The graph could read no effect estimate from its abstract, so it casts no vote on the map. Cited by 49 papers.
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Who cites it
49 citing papers in PubMed.
- Characterization of strongly hyperfine-split protons by DNP.Physical chemistry chemical physics : PCCP · 2026Article
- Targeted NMR signal enhancement of RNA by site-directed bis-nitroxide labeling.Proceedings of the National Academy of Sciences of the United States of America · 2026Article
- Systematic Evaluation of Polarizing Agents for Dynamic Nuclear Polarization Enhanced NMR.Angewandte Chemie (International ed. in English) · 2025Article
- Position-Specific Substitution in Cellulose Ethers Studied by DNP Enhanced Solid-State NMR Spectroscopy.Magnetic resonance in chemistry : MRC · 2025Article
- A DNP-Supported Solid-State NMR Approach to Study Nucleic Acids In Situ Reveals Berberine-Stabilized Hoogsteen Structures in Mitochondria.Angewandte Chemie (International ed. in English) · 2025Article
- Frequency-Chirped Magic Angle Spinning Dynamic Nuclear Polarization Combined with Electron Decoupling.The journal of physical chemistry letters · 2024Article
- Resolution in cryogenic solid state NMR: Challenges and solutions.Protein science : a publication of the Protein Society · 2024Review
- Dynamic Nuclear Polarization Using Electron Spin Cluster.The journal of physical chemistry letters · 2024Article
- AsymPol-TEKs as efficient polarizing agents for MAS-DNP in glass matrices of non-aqueous solvents.Physical chemistry chemical physics : PCCP · 2024Article
- A high-field cellular DNP-supported solid-state NMR approach to study proteins with sub-cellular specificity.Chemical science · 2023Article
- Large cross-effect dynamic nuclear polarisation enhancements with kilowatt inverting chirped pulses at 94 GHz.Communications chemistry · 2023Article
- Optically Enhanced Solid-StateJournal of the American Chemical Society · 2023Article
- Polarizing agents for efficient high field DNP solid-state NMR spectroscopy under magic-angle spinning: from design principles to formulation strategies.Chemical science · 2023Review
- Spin Hyperpolarization in Modern Magnetic Resonance.Chemical reviews · 2023Review
- Highly Efficient Polarizing Agents for MAS-DNP of Proton-Dense Molecular Solids.Angewandte Chemie (International ed. in English) · 2022Article
- A novel strategy for site selective spin-labeling to investigate bioactive entities by DNP and EPR spectroscopy.Scientific reports · 2021Article
- Targeted DNP for biomolecular solid-state NMR.Chemical science · 2021Review
- Characterizing proteins in a native bacterial environment using solid-state NMR spectroscopy.Nature protocols · 2021Article
- Biomolecular Perturbations in In-Cell Dynamic Nuclear Polarization Experiments.Frontiers in molecular biosciences · 2021Article
- Site-specific dynamic nuclear polarization in a Gd(III)-labeled protein.Physical chemistry chemical physics : PCCP · 2020Article
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5 authors.
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Abstract
The effects of nuclear signal quenching induced by the presence of a paramagnetic polarizing agent are documented for conditions used in magic angle spinning (MAS)-dynamic nuclear polarization (DNP) experiments on homogeneous solutions. In particular, we present a detailed analysis of three time constants: (1) the longitudinal build-up time constant TB for (1)H; (2) the rotating frame relaxation time constant T1ρ for (1)H and (13)C and (3) T2 of (13)C, the transverse relaxation time constant in the laboratory frame. These relaxation times were measured during microwave irradiation at a magnetic field of 5 T (140 GHz) as a function of the concentration of four polarizing agents: TOTAPOL, 4-amino-TEMPO, trityl (OX063), and Gd-DOTA and are compared to those obtained for a sample lacking paramagnetic doping. We also report the EPR relaxation time constants T1S and T2S, the DNP enhancements, ε, and the parameter E, defined below, which measures the sensitivity enhancement for the four polarizing agents as a function of the electron concentration. We observe substantial intensity losses (paramagnetic quenching) with all of the polarizing agents due to broadening mechanisms and cross relaxation during MAS. In particular, the monoradical trityl and biradical TOTAPOL induce ∼40% and 50% loss of signal intensity. In contrast there is little suppression of signal intensity in static samples containing these paramagnetic species. Despite the losses due to quenching, we find that all of the polarizing agents provide substantial gains in signal intensity with DNP, and in particular that the net enhancement is optimal for biradicals that operate with the cross effect. We discuss the possibility that much of this polarization loss can be regained with the development of instrumentation and methods to perform electron decoupling.
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