Nanomole-scale Protein Solid-state NMR by Breaking Intrinsic 1HT1 Boundaries

Overview

Journal Nat Methods

Specialties Biomedical Engineering
Pathology

Date 2009 Feb 10

PMID 19198596

Citations 83

Authors

Nalinda P Wickramasinghe

Sudhakar Parthasarathy

Christopher R Jones

Chhavi Bhardwaj

Fei Long

Mrignayani Kotecha

Shahila Mehboob

Leslie W-M Fung

Jaan Past

Ago Samoson

Yoshitaka Ishii

Affiliations

Soon will be listed here.

Abstract

We present an approach that accelerates protein solid-state NMR 5-20-fold using paramagnetic doping to condense data-collection time (to approximately 0.2 s per scan), overcoming a long-standing limitation on slow recycling owing to intrinsic (1)H T(1) longitudinal spin relaxation. Using low-power schemes under magic-angle spinning at 40 kHz, we obtained two-dimensional (13)C-(13)C and (13)C-(15)N solid-state NMR spectra for several to tens of nanomoles of beta-amyloid fibrils and ubiquitin in 1-2 d.

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References

Buffy J, Hong T, Yamaguchi S, Waring A, Lehrer R, Hong M . Solid-state NMR investigation of the depth of insertion of protegrin-1 in lipid bilayers using paramagnetic Mn2+. Biophys J. 2003; 85(4):2363-73. PMC: 1303461. DOI: 10.1016/S0006-3495(03)74660-8. View

Hall D, Maus D, Gerfen G, Inati S, Becerra L, Dahlquist F . Polarization-enhanced NMR spectroscopy of biomolecules in frozen solution. Science. 1997; 276(5314):930-2. DOI: 10.1126/science.276.5314.930. View

Chimon S, Shaibat M, Jones C, Calero D, Aizezi B, Ishii Y . Evidence of fibril-like β-sheet structures in a neurotoxic amyloid intermediate of Alzheimer's β-amyloid. Nat Struct Mol Biol. 2007; 14(12):1157-64. DOI: 10.1038/nsmb1345. View

Lange A, Giller K, Hornig S, Martin-Eauclaire M, Pongs O, Becker S . Toxin-induced conformational changes in a potassium channel revealed by solid-state NMR. Nature. 2006; 440(7086):959-62. DOI: 10.1038/nature04649. View

Petkova A, Yau W, Tycko R . Experimental constraints on quaternary structure in Alzheimer's beta-amyloid fibrils. Biochemistry. 2006; 45(2):498-512. PMC: 1435828. DOI: 10.1021/bi051952q. View

Linser R, Chevelkov V, Diehl A, Reif B . Sensitivity enhancement using paramagnetic relaxation in MAS solid-state NMR of perdeuterated proteins. J Magn Reson. 2007; 189(2):209-16. DOI: 10.1016/j.jmr.2007.09.007. View

Igumenova T, McDermott A, Zilm K, Martin R, Paulson E, Wand A . Assignments of carbon NMR resonances for microcrystalline ubiquitin. J Am Chem Soc. 2004; 126(21):6720-7. DOI: 10.1021/ja030547o. View

Wickramasinghe N, Shaibat M, Jones C, Casabianca L, de Dios A, Harwood J . Progress in 13C and 1H solid-state nuclear magnetic resonance for paramagnetic systems under very fast magic angle spinning. J Chem Phys. 2008; 128(5):052210. DOI: 10.1063/1.2833574. View

Edison A, Long J . Spectroscopy: the magic of solenoids. Nature. 2007; 447(7145):646-7. DOI: 10.1038/447646a. View

10.

Wasmer C, Lange A, Van Melckebeke H, Siemer A, Riek R, Meier B . Amyloid fibrils of the HET-s(218-289) prion form a beta solenoid with a triangular hydrophobic core. Science. 2008; 319(5869):1523-6. DOI: 10.1126/science.1151839. View

11.

Ishii Y, Yesinowski J, Tycko R . Sensitivity enhancement in solid-state (13)C NMR of synthetic polymers and biopolymers by (1)H NMR detection with high-speed magic angle spinning. J Am Chem Soc. 2001; 123(12):2921-2. DOI: 10.1021/ja015505j. View

12.

Pintacuda G, Giraud N, Pierattelli R, Bockmann A, Bertini I, Emsley L . Solid-state NMR spectroscopy of a paramagnetic protein: assignment and study of human dimeric oxidized CuII-ZnII superoxide dismutase (SOD). Angew Chem Int Ed Engl. 2006; 46(7):1079-82. DOI: 10.1002/anie.200603093. View

13.

Weliky D, Bennett A, Zvi A, Anglister J, Steinbach P, Tycko R . Solid-state NMR evidence for an antibody-dependent conformation of the V3 loop of HIV-1 gp120. Nat Struct Biol. 1999; 6(2):141-5. DOI: 10.1038/5827. View

14.

Mani R, Cady S, Tang M, Waring A, Lehrer R, Hong M . Membrane-dependent oligomeric structure and pore formation of a beta-hairpin antimicrobial peptide in lipid bilayers from solid-state NMR. Proc Natl Acad Sci U S A. 2006; 103(44):16242-7. PMC: 1637567. DOI: 10.1073/pnas.0605079103. View