ArticleThe journal of physical chemistry. B2014
DNP-enhanced MAS NMR of bovine serum albumin sediments and solutions.
Article in The journal of physical chemistry. B, 2014. The graph could read no effect estimate from its abstract, so it casts no vote on the map. Cited by 15 papers.
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Who cites it
15 citing papers in PubMed.
- DNP enhanced solid-state NMR of lattice-like microcrystalline protein assemblies facilitated by co-assembly with dinitroxide-tagged proteins.Journal of magnetic resonance (San Diego, Calif. : 1997) · 2026Article
- Sedimentation of large, soluble proteins up to 140 kDa forJournal of biomolecular NMR · 2024Article
- Characterization of dielectric properties and their impact on MAS-DNP NMR applications.Journal of magnetic resonance (San Diego, Calif. : 1997) · 2024Article
- Transient RNA Interactions Leave a Covalent Imprint on a Viral Capsid Protein.Journal of the American Chemical Society · 2022Article
- Targeted DNP for biomolecular solid-state NMR.Chemical science · 2021Review
- NMR Signal Quenching from Bound Biradical Affinity Reagents in DNP Samples.The journal of physical chemistry. B · 2017Article
- Protein-nucleotide contacts in motor proteins detected by DNP-enhanced solid-state NMR.Journal of biomolecular NMR · 2017Article
- In Situ Characterization of Pharmaceutical Formulations by Dynamic Nuclear Polarization Enhanced MAS NMR.The journal of physical chemistry. B · 2017Article
- New NMR tools for protein structure and function: Spin tags for dynamic nuclear polarization solid state NMR.Archives of biochemistry and biophysics · 2017Review
- Dynamic Nuclear Polarization Signal Enhancement with High-Affinity Biradical Tags.The journal of physical chemistry. B · 2017Article
- Frequency swept microwaves for hyperfine decoupling and time domain dynamic nuclear polarization.Solid state nuclear magnetic resonance · 2015Article
- Biosilica-Entrapped Enzymes Studied by Using Dynamic Nuclear-Polarization-Enhanced High-Field NMR Spectroscopy.Chemphyschem : a European journal of chemical physics and physical chemistry · 2015Article
- Facing and Overcoming Sensitivity Challenges in Biomolecular NMR Spectroscopy.Angewandte Chemie (International ed. in English) · 2015Review
- Dynamic nuclear polarization of (1)H, (13)C, and (59)Co in a tris(ethylenediamine)cobalt(III) crystalline lattice doped with Cr(III).Journal of the American Chemical Society · 2014Article
- Topical Developments in High-Field Dynamic Nuclear Polarization.Israel journal of chemistry · 2014Article
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Authors and funding
6 authors.
Funding
Abstract
Protein sedimentation sans cryoprotection is a new approach to magic angle spinning (MAS) and dynamic nuclear polarization (DNP) nuclear magnetic resonance (NMR) spectroscopy of proteins. It increases the sensitivity of the experiments by a factor of ∼4.5 in comparison to the conventional DNP sample preparation and circumvents intense background signals from the cryoprotectant. In this paper, we investigate sedimented samples and concentrated frozen solutions of natural abundance bovine serum albumin (BSA) in the absence of a glycerol-based cryoprotectant. We observe DNP signal enhancements of ε ∼ 66 at 140 GHz in a BSA pellet sedimented from an aqueous solution containing the biradical polarizing agent TOTAPOL and compare this with samples prepared using the conventional protocol (i.e., dissolution of BSA in a glycerol/water cryoprotecting mixture). The dependence of DNP parameters on the radical concentration points to the presence of an interaction between TOTAPOL and BSA, so much so that a frozen solution sans cryoprotectant still gives ε ∼ 50. We have studied the interaction of BSA with another biradical, SPIROPOL, that is more rigid than TOTAPOL and has been reported to give higher enhancements. SPIROPOL was also found to interact with BSA, and to give ε ∼ 26 close to its maximum achievable concentration. Under the same conditions, TOTAPOL gives ε ∼ 31, suggesting a lesser affinity of BSA for SPIROPOL with respect to TOTAPOL. Altogether, these results demonstrate that DNP is feasible in self-cryoprotecting samples.
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