Efficient 18.8 T MAS-DNP NMR reveals hidden side chains in amyloid fibrils

Akbey Ü, Linden AH, Oschkinat H (2012) High-temperature dynamic nuclear polarization enhanced magic-angle-spinning NMR. Appl Magn Reson 43:81–90

Article  Google Scholar 

Bahri S et al (2022) H detection and dynamic nuclear polarization—enhanced NMR of Aβ 1–42 fibrils.

Bajaj VS, Mak-Jurkauskas ML, Belenky M, Herzfeld J, Griffin RG (2010) DNP enhanced frequency-selective TEDOR experiments in bacteriorhodopsin. J Magn Reson 202:9–13

Article  ADS  Google Scholar 

Barnes AB et al (2009) Cryogenic sample exchange NMR probe for magic angle spinning dynamic nuclear polarization. J Magn Reson 198:261–270

Article  ADS  Google Scholar 

Barnes AB et al (2010) Resolution and polarization distribution in cryogenic DNP/MAS experiments. Phys Chem Chem Phys 12:5861

Article  Google Scholar 

Bauer T et al (2017) Line-broadening in low-temperature solid-State NMR spectra of fibrils. J Biomol NMR 67:51–61

Bayro MJ et al (2011) Intermolecular structure determination of amyloid fibrils with magic-angle spinning and dynamic nuclear polarization NMR. J Am Chem Soc 133:13967–13974

Article  Google Scholar 

Berruyer P (2020) Dynamic nuclear polarization enhancement of 200 at 21.15 T enabled by 65 kHz magic angle spinning. J Phys Chem Lett 11:8386–8391.

Biedenbänder T, Aladin V, Saeidpour S, Corzilius B (2022) Dynamic nuclear polarization for sensitivity enhancement in NMR. Chem Rev.

Article  Google Scholar 

Björklund S, Nowacka A, Bouwstra JA, Sparr E, Topgaard D (2013) Characterization of stratum corneum molecular dynamics by natural-abundance 13C solid-state NMR. PLoS ONE.

Blank M, Borchard P, Cauffman S, Felch K, Rosay M (2016) Development of high-frequency cw gyrotrons for DNP/NMR applications. Terahertz Sci Technol 9:177–186

Google Scholar 

Cai X et al (2021) Highly efficient trityl-nitroxide biradicals for biomolecular high-field dynamic nuclear polarization. Chemisty A 27:12758–12762

Google Scholar 

Chapman MR et al (2002) Role of Escherichia coli curli operons in directing amyloid fiber formation. Science (80-) 295:851–855

Article  ADS  Google Scholar 

Colvin MT et al (2015) High resolution structural characterization of Aβ42 amyloid fibrils by magic angle spinning NMR. J Am Chem Soc 137:7509–7518

Article  Google Scholar 

Colvin MT et al (2016) Atomic resolution structure of monomorphic Aβ 42 amyloid fibrils. J Am Chem Soc 138:9663–9674

Article  Google Scholar 

Conroy DW et al (2022) Probing Watson-Crick and Hoogsteen base pairing in duplex DNA using dynamic nuclear polarization solid-state NMR spectroscopy. Proc Natl Acad Sci USA

Corzilius B, Andreas LB, Smith AA, Ni QZ, Griffin RG (2014) Paramagnet induced signal quenching in MAS-DNP experiments in frozen homogeneous solutions. J Magn Reson 240:113–123

Article  ADS  Google Scholar 

Daskalov A et al (2015) Signal transduction by a fungal NOD-like receptor based on propagation of a prion amyloid fold. PLoS Biol 13:1–26

Article  Google Scholar 

Daskalov A et al (2020) Structural and molecular basis of cross-seeding barriers in amyloids. Proc Natl Acad Sci USA 118:1–8

Google Scholar 

Daskalov A et al (2021) Structures of pathological and functional amyloids and prions, a solid-state NMR perspective. Front Mol Neurosci 14:1–18

Article  Google Scholar 

David G et al (2018) Structural studies of self-assembled subviral particles: combining cell-free expression with 110 kHz MAS NMR spectroscopy. Angew Chem Int Ed 57:4787–4791

Article  Google Scholar 

De Paëpe G et al (2011) Heteronuclear proton assisted recoupling. J Chem Phys 134:1–18

Article  Google Scholar 

Debelouchina GT et al (2013) Higher order amyloid fibril structure by MAS NMR and DNP spectroscopy. J Am Chem Soc 135:19237–19247

Article  Google Scholar 

Delage-Laurin L et al (2021) Overhauser dynamic nuclear polarization with selectively deuterated BDPA radicals. J Am Chem Soc 143:20281–20290

Article  Google Scholar 

Deo T, Cheng Q, Paul S, Qiang W, Potapov A (2021) Application of DNP-enhanced solid-state NMR to studies of amyloid-β peptide interaction with lipid membranes. Chem Phys Lipids 236:105071

Article  Google Scholar 

Dobson CM, Knowles TPJ, Vendruscolo M (2020) The amyloid phenomenon and its significance in biology and medicine. Cold Spring Harb Perspect Biol 12

Donovan KJ, Jain SK, Silvers R, Linse S, Griffin RG (2017a) Proton-assisted recoupling (PAR) in peptides and proteins. J Phys Chem B 121:10804–10817

Article  Google Scholar 

Donovan KJ, Silvers R, Linse S, Griffin RG (2017b) 3D MAS NMR experiment utilizing through-space 15 N– 15 N correlations. J Am Chem Soc 139:6518–6521

Article  Google Scholar 

Felch K et al (2013) First tests of a 527 GHz gyrotron for dynamic nuclear polarization. In 2013 IEEE 14th international vacuum electronics conference (IVEC) 1–2 (IEEE, 2013).

Fitzpatrick AWP et al (2013) Atomic structure and hierarchical assembly of a cross-β amyloid fibril. Proc Natl Acad Sci USA 110:5468–5473

Article  ADS  Google Scholar 

Fitzpatrick AW, Saibil HR (2019) Cryo-EM of amyloid fibrils and cellular aggregates. Curr Opin Struct Biol 58:34–42

Article  Google Scholar 

Frederick KK et al (2017) Combining DNP NMR with segmental and specific labeling to study a yeast prion protein strain that is not parallel in-register. Proc Natl Acad Sci USA 114:3642–3647

Article  ADS  Google Scholar 

Fricke P, Demers JP, Becker S, Lange A (2014) Studies on the MxiH protein in T3SS needles using DNP-enhanced ssNMR spectroscopy. ChemPhysChem 15:57–60

Article  Google Scholar 

Fricke P et al (2016) High resolution observed in 800 MHz DNP spectra of extremely rigid type III secretion needles. J Biomol NMR 65:121–126

Article  Google Scholar 

Gath J et al (2014) Yet another polymorph of α-synuclein: solid-state sequential assignments. Biomol NMR Assign 8:395–404

Article  Google Scholar 

Gauto DF et al (2019) Aromatic ring dynamics, thermal activation, and transient conformations of a 468 kDa enzyme by specific 1H–13C labeling and fast magic-angle spinning NMR. J Am Chem Soc 141:11183–11195

Article  Google Scholar 

Gauto D, Dakhlaoui O, Marin-Montesinos I, Hediger S, De Paëpe G (2021) Targeted DNP for biomolecular solid-state NMR. Chem Sci 12:6223–6237

Article  Google Scholar 

Halbritter T, Harrabi R, Paul S, Tol JV, Lee D, Sigurdsson ST, Mentink-Vigier F, De Paëpe G (2022) PyrroTriPol: a Semi-rigid trityl-nitroxide for high field dynamic nuclear polarization. Chem. Sci.

Article  Google Scholar 

Heise H et al (2008) Solid-state NMR reveals structural differences between fibrils of wild-type and disease-related A53T mutant α-synuclein. J Mol Biol 380:444–450

Article  Google Scholar 

Henstra A, Dirksen P, Schmidt J, Wenckebach WT (1988) Nuclear spin orientation via electron spin locking (NOVEL). J Magn Reson 77:389–393

ADS  Google Scholar 

Jaroniec CP (2019) Two decades of progress in structural and dynamic studies of amyloids by solid-state NMR. J Magn Reson 306:42–47

Article  ADS  Google Scholar 

Jaudzems K et al (2018) Dynamic nuclear polarization-enhanced biomolecular NMR spectroscopy at high magnetic field with fast magic-angle spinning. Angew Chem Int Ed 7458–7462.

Jaudzems K, Polenova T, Pintacuda G, Oschkinat H, Lesage A (2019) DNP NMR of biomolecular assemblies. J Struct Biol 206:90–98

Article  Google Scholar 

Jirasko V et al (2021) Dimer organization of membrane-associated NS5A of hepatitis C virus as determined by highly sensitive 1H-detected solid-state NMR. Angew Chem Int Ed 60:5339–5347

Article  Google Scholar 

Ke PC et al (2020) Half a century of amyloids: past, present and future. Chem Soc Rev 49:5473–5509

Article  Google Scholar 

Kubicki DJ et al (2014) Amplifying dynamic nuclear polarization of frozen solutions by incorporating dielectric particles. J Am Chem Soc 136:15711–15718

Article  Google Scholar 

Lewandowski JR, De Paëpe G, Griffin RG (2007) Proton assisted insensitive nuclei cross polarization. J Am Chem Soc 129:728–729

Article  Google Scholar 

Li Y et al (2021) Solid-state MAS NMR at ultra low temperature of hydrated alanine doped with DNP radicals. J Magn Reson 333:107090

Article  Google Scholar 

Lopez del Amo J-M, Schneider D, Loquet A, Lange A, Reif B (2013) Cryogenic solid state NMR studies of fibrils of the Alzheimer’s disease amyloid-β peptide: perspectives for DNP. J Biomol NMR 56:359–363

Article  Google Scholar 

Loquet A, Saupe SJ (2017) Diversity of amyloid motifs in NLR signaling in fungi. Biomolecules 7:1–10

Article  Google Scholar 

Loquet A et al (2012) Atomic model of the type III secretion system needle. Nature 486:276–279

Article  ADS  Google Scholar 

Loquet A, Saupe SJ, Romero D (2018a) Functional amyloids in health and disease. J Mol Biol 430:3629–3630

Article  Google Scholar 

Loquet A et al (2018b) 3D structure determination of amyloid fibrils using solid-state NMR spectroscopy. Methods.

Article  Google Scholar 

Lund A et al (2020) TinyPols: a family of water-soluble binitroxides tailored for dynamic nuclear polarization enhanced NMR spectroscopy at 18.8 and 21.1 T. Chem Sci 68:42–61.

Maciejko J et al (2015) Visualizing specific cross-protomer interactions in the homo-oligomeric membrane protein proteorhodopsin by dynamic-nuclear-polarization-enhanced solid-state NMR. J Am Chem Soc 137:9032–9043

Article  Google Scholar 

Maji SK et al (2009) Functional amyloids as natural storage of peptide hormones in pituitary secretory granules. Science (80-) 325:328–332

Article  ADS  Google Scholar 

Marin-Montesinos I et al (2019) Selective high-resolution DNP-enhanced NMR of biomolecular binding sites. Chem Sci 10:3366–3374

Article  Google Scholar 

Mathies G et al (2015) Efficient dynamic nuclear polarization at 800 MHz/527 GHz with trityl-nitroxide biradicals. Angew Chemie - Int Ed 54:11770–11774

Article  Google Scholar 

Matsuki Y, Idehara T, Fukazawa J, Fujiwara T (2016) Advanced instrumentation for DNP-enhanced MAS NMR for higher magnetic fields and lower temperatures. J Magn Reson 264:107–115

Article  ADS  Google Scholar 

Maus DC et al (1996) A solid-state NMR study of tungsten methyl group dynamics in [W(η 5-C 5Me 5)Me 4][PF 6]. J Am Chem Soc 118:5665–5671

Article  Google Scholar 

Meier BH, Böckmann A (2015) The structure of fibrils from ‘misfolded’ proteins. Curr Opin Struct Biol 30:43–49

Article 

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