ArticleJournal of magnetic resonance (San Diego, Calif. : 1997)2013
Dynamic nuclear polarization-enhanced 13C NMR spectroscopy of static biological solids.
Article in Journal of magnetic resonance (San Diego, Calif. : 1997), 2013. The graph could read no effect estimate from its abstract, so it casts no vote on the map. Cited by 12 papers.
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Who cites it
12 citing papers in PubMed, 26 citations in OpenAlex.
- Application of DNP-enhanced solid-state NMR to studies of amyloid-β peptide interaction with lipid membranes.Chemistry and physics of lipids · 2021Article
- Advances in studying protein disorder with solid-state NMR.Solid state nuclear magnetic resonance · 2020Review
- Succinyl-DOTOPA: An effective triradical dopant for low-temperature dynamic nuclear polarization with high solubility in aqueous solvent mixtures at neutral pH.Journal of magnetic resonance (San Diego, Calif. : 1997) · 2020Article
- Verdazyl-ribose: A new radical for solid-state dynamic nuclear polarization at high magnetic field.Journal of magnetic resonance (San Diego, Calif. : 1997) · 2018Article
- Low-temperature dynamic nuclear polarization with helium-cooled samples and nitrogen-driven magic-angle spinning.Journal of magnetic resonance (San Diego, Calif. : 1997) · 2016Article
- Rational design of dinitroxide biradicals for efficient cross-effect dynamic nuclear polarization.Chemical science · 2016Article
- Design and characterization of a W-band system for modulated DNP experiments.Journal of magnetic resonance (San Diego, Calif. : 1997) · 2015Article
- Cellular solid-state NMR investigation of a membrane protein using dynamic nuclear polarization.Biochimica et biophysica acta · 2015Article
- Amplifying dynamic nuclear polarization of frozen solutions by incorporating dielectric particles.Journal of the American Chemical Society · 2014Article
- Topical Developments in High-Field Dynamic Nuclear Polarization.Israel journal of chemistry · 2014Article
- Dynamic nuclear polarization of 17O: direct polarization.The journal of physical chemistry. B · 2013Article
- Shortening spin-lattice relaxation using a copper-chelated lipid at low-temperatures - A magic angle spinning solid-state NMR study on a membrane-bound protein.Journal of magnetic resonance (San Diego, Calif. : 1997) · 2013Article
Corrections and comments
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Authors and funding
3 authors at 2 institutions in 1 country.
Funding
Abstract
We explore the possibility of using dynamic nuclear polarization (DNP) to enhance signals in structural studies of biological solids by solid state NMR without sample spinning. Specifically, we use 2D (13)C-(13)C exchange spectroscopy to probe the peptide backbone torsion angles (φ, ψ) in a series of selectively (13)C-labeled 40-residue β-amyloid (Aβ(1-40)) samples, in both fibrillar and non-fibrillar states. Experiments are carried out at 9.39 T and 8 K, using a static double-resonance NMR probe and low-power microwave irradiation at 264 GHz. In frozen solutions of Aβ(1-40) fibrils doped with DOTOPA-TEMPO, we observe DNP signal enhancement factors of 16-21. We show that the orientation- and frequency-dependent spin polarization exchange between sequential backbone carbonyl (13)C labels can be simulated accurately using a simple expression for the exchange rate, after experimentally determined homogeneous (13)C lineshapes are incorporated in the simulations. The experimental 2D (13)C-(13)C exchange spectra place constraints on the φ and ψ angles between the two carbonyl labels. Although the data are not sufficient to determine φ and ψ uniquely, the data do provide non-trivial constraints that could be included in structure calculations. With DNP at low temperatures, 2D (13)C-(13)C exchange spectra can be obtained from a 3.5 mg sample of Aβ(1-40) fibrils in 4 h or less, despite the broad (13)C chemical shift anisotropy line shapes that are observed in static samples.
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Registered trials
Read under generation 80e0d062 · epoch 390. Bibliography from PubMed, PubMed Central and OpenAlex; grants from NIH RePORTER; trial links from ClinicalTrials.gov; estimates, votes and beliefs from the OpenQuestion graph.