Low microwave-amplitude ESR spectroscopy: Measuring spin-relaxation interactions of moderately immobilized spin labels in proteins

Journal of Biochemical and Biophysical Methods

Volumn 60, Issue 2, 2004, Pages 117-138

  Hedin, Eva M K ^a   Hult, Karl ^a   Mouritsen, Ole G ^b   Høyrup, Pernille ^c  

^a ALBANOVA UNIVERSITY CENTER   (Sweden)

^b UNIVERSITY OF SOUTHERN DENMARK   (Denmark)

^c TECHNICAL UNIVERSITY OF DENMARK   (Denmark)

Author keywords

chromium(III) oxalate; continuous wave; Crox; CW; DL dithiothreitol; DTT; EDTA; Electron spin resonance; electron spin resonance; electrospray mass spectroscopy; Electrospray MS; ESR; ethylenediamine tetraacetic acid; HEPES; Lipase; Microwave saturation; MTSL

Indexed keywords

1 OXYL 2,2,5,5 TETRAMETHYL DELTA 3 PYRROLINE 3 METHYLMETHANETHIOSULFONATE; CHROMIUM DERIVATIVE; FUNGAL ENZYME; MUTANT PROTEIN; OXALIC ACID; SULFONIC ACID DERIVATIVE; TRIACYLGLYCEROL LIPASE; UNCLASSIFIED DRUG; WATER;

ARTICLE; CORRELATION ANALYSIS; ELECTRON SPIN RESONANCE; EQUIPMENT; FUNGUS; MAGNETISM; MICROWAVE RADIATION; MOLECULAR DYNAMICS; MOLECULAR INTERACTION; PRIORITY JOURNAL; PROTEIN IMMOBILIZATION; PROTEIN STRUCTURE; QUANTITATIVE ANALYSIS; ROTATION; SOLUBILITY; SPIN LABELING; STANDARD; THEORY; TIME;

ASCOMYCOTA; BIOPHYSICS; CYCLIC N-OXIDES; CYSTEINE; DOSE-RESPONSE RELATIONSHIP, DRUG; ELECTRON SPIN RESONANCE SPECTROSCOPY; LIPASE; MAGNETIC RESONANCE SPECTROSCOPY; MESYLATES; MICROWAVES; MUTAGENESIS, SITE-DIRECTED; MUTATION; PEPTIDES; PROTEINS; RECOMBINANT PROTEINS; SPIN LABELS; TIME FACTORS; WATER;

THERMOMYCES; THERMOMYCES LANUGINOSUS;

EID: 3242710304     PISSN: 0165022X     EISSN: None     Source Type: Journal    
DOI: 10.1016/j.jbbm.2004.05.002     Document Type: Article

References (48)

1. Berliner L.J. Spin labeling: Theory and applications I. 1976;Academic Press, New York
2. Berliner L.J. Spin labeling: Theory and applications II. 1979;Academic Press, New York
3. Millhauser G.L. Selective placement of electron spin resonance spin labels: new structural methods for peptides and proteins. Trends Biochem. Sci. 17:1992;448-452
4. Hubbell W.L., Cafiso D.S., Altenbach C. Identifying conformational changes with site-directed spin labeling. Nat. Struct. Biol. 7:2000;735-739
5. Lakshmi K.V., Brudvig G.W. Pulsed electron paramagnetic resonance methods for macromolecular structure determination. Curr. Opin. Struct. Biol. 11:2001;523-531
6. Schreier S., Polnaszek C.F., Smith I.C.P. Spin labels in membranes. Problems in practice. Biochim. Biophys. Acta. 515:1978;375-436
7. Marsh D. Experimental methods in spin-label spectral analysis. Berliner L.J., Reuben J. Spin labeling: Theory and applications. 1989;255-303 Plenum Press, New York
8. Alber T., Sun D.P., Nye J.A., Muchmore D.C., Matthews B.W. Temperature-sensitive mutations of bacteriophage-T4 lysozyme occur at sites with low mobility and low solvent accessibility in the folded protein. Biochemistry. 26:1987;3754-3758
9. Mchaourab H.S., Lietzow M.A., Hideg K., Hubbell W.L. Motion of spin-labeled side chains in T4 lysozyme. Correlation with protein structure and dynamics. Biochemistry. 35:1996;7692-7704
10. Todd A.P., Cong J.P., Levinthal F., Levinthal C., Hubbell W.L. Site-directed mutagenesis of Colicin E1 provides specific attachment sites for spin labels whose spectra are sensitive to local conformation. Proteins Struct., Funct., Genet. 6:1989;294-305
11. Hubbell W.L., Gross A., Langen R., Lietzow M.A. Recent advances in site-directed spin labeling of proteins. Curr. Opin. Struct. Biol. 8:1998;649-656
12. Robinson B.H., Haas D.A., Mailer C. Molecular dynamics in liquids: Spin-lattice relaxation of nitroxide spin labels. Science. 263:1994;490-493
13. Altenbach C., Marti T., Khorana H.G., Hubbell W.L. Transmembrane protein structure: Spin labeling of bacteriorhodopsin mutants. Science. 248:1990;1088-1092
14. Altenbach C., Yang K., Farrens D.L., Farahbakhsh Z.T., Khorana H.G., Hubbell W.L. Structural features and light-dependent changes in the cytoplasmic interhelical E-F loop region of rhodopsin: A site-directed spin-labeling study. Biochemistry. 35:1996;12470-12478
15. Klug C.S., Su W.Y., Feix J.B. Mapping of the residues involved in a proposed β-strand located in the ferric enterobactin receptor FepA using site-directed spin-labeling. Biochemistry. 36:1997;13027-13033
16. Fanucci G.E., Cadieux N., Piedmont C.A., Kadner R.J., Cafiso D.S. Structure and dynamics of the β-barrel of the membrane transporter BtuB by site-directed spin labeling. Biochemistry. 41:2002;11543-11551
17. Pake G.E., Tuttle T.R. Jr. Anomalous loss of resolution of paramagnetic resonance hyperfine structure in liquids. Phys. Rev. 3:1959;423-425
18. Poole C.P. Jr. Electron spin resonance: a comprehensive treatise on experimental techniques. 1967;Interscience Publishers, New York
19. Altenbach C., Flitsch S.L., Khorana H.G., Hubbell W.L. Structural studies on transmembrane proteins: II. Spin labeling of bacteriorhodopsin mutants at unique cysteines. Biochemistry. 28:1989;7806-7812
20. 2 on membranes using electrostatic potential-modulated spin-relaxation magnetic resonance. Science. 279:1998;1925-1929
21. Froncisz W., Hyde J.S. The loop-gap resonator - a new microwave lumped circuit electron spin resonance sample structure. J. Magn. Reson. 47:1982;515-521
22. Mailer C., Haas D.A., Hustedt E.J., Gladden J.G., Robinson B.H. Low-power electron paramagnetic resonance spin-echo spectroscopy. J. Magn. Reson. 91:1991;475-496
23. 1e from continuous wave electron paramagnetic resonance spectra at all rotational rates. Biophys. J. 64:1993;594-604
24. Berg S.P., Nesbitt D.M. Chromium oxalate - new spin label broadening agent for use with thylakoids. Biochim. Biophys. Acta. 548:1979;608-615
25. Lawson D.M., Brzozowski A.M., Dodson G.G., Hubbard R.E., Huge-Jensen B., Boel E., Derewenda Z.S. Wolley P., Petersen S.B. Lipases: Their structure, biochemistry and application. 1994;77-94 Cambridge Univ. Press, Cambridge
26. Lawson D.M., Brzozowski A.M., Rety S., Verma C., Dodson G.G. Probing the nature of substrate-binding in Humicola lanuginosa lipase through X-ray crystallography and intuitive modeling. Protein Eng. 7:1994;543-550
27. Brzozowski A.M., Savage H., Verma C.S., Turkenburg J.P., Lawson D.M., Svendsen A., et al. Structural origins of the interfacial activation in Thermomyces (Humicola) lanuginosa lipase. Biochemistry. 39:2000;15071-15082
28. Bailar J.C., Jones E.M. Trioxalato salts. Inorg. Synth. 1:1939;35-38
29. Svendsen A., Clausen I.G., Patkar S.A., Borch K., Thellersen M. Protein engineering of microbial lipases of industrial interest. Methods Enzymol. 284:1997;317-340
30. Hedin E.M.K., Patkar S.A., Vind J., Svendsen A., Hult K., Berglund P. Selective reduction and chemical modification of oxidized lipase cysteine mutants. Can. J. Chem. 80:2002;529-539
31. Briggs R.G., Fee J.A. Sulfhydryl reactivity of human erytrocyte superoxide dismutase. On the origin of the unusual spectral properties of the protein when prepared by a procedure utilizing chloroform and ethanol for the precipitation of hemoglobin. Biochim. Biophys. Acta. 537:1978;100-109
32. Pantoliano M.W., Whitlow M., Wood J.F., Dodd S.W., Hardman K.D., Rollence M.L., et al. Large increases in general stability for Subtilisin BPN' through incremental changes in the free-energy of unfolding. Biochemistry. 28:1989;7205-7213
33. Pace C.N., Vajdos F., Fee L., Grimsley G., Gray T. How to measure and predict the molar absorption-coefficient of a protein. Protein Sci. 4:1995;2411-2423
34. Merianos H.J., Cadieux N., Lin C.H., Kadner R.J., Cafiso D.S. Substrate-induced exposure of an energy-coupling motif of a membrane transporter. Nat. Struct. Biol. 7:2000;205-209
35. Hung S.C., Wang W., Chan S.I., Chen H.M. Membrane lysis by the antibacterial peptides cecropins B1 and B3: A spin-label electron spin resonance study on phospholipid bilayers. Biophys. J. 77:1999;3120-3133
36. Devaux P., Scandella C.J., McConnell H.M. Spin-spin interactions between spin-labeled phospholipids incorporated into membranes. J. Magn. Reson. 9:1973;474-485
37. 1 method. Biochim. Biophys. Acta. 643:1981;283-291
38. Livshits V.A., Pali T., Marsh D. Relaxation time determinations by progressive saturation EPR: effects of molecular motion and Zeeman modulation for spin labels. J. Magn. Reson. 133:1998;79-91
39. Robinson B.H., Mailer C., Reese A.W. Linewidth analysis of spin labels in liquids: I. Theory and data analysis. J. Magn. Reson. 138:1999;199-209
40. Robinson B.H., Mailer C., Reese A.W. Linewidth analysis of spin labels in liquids: II. Experimental. J. Magn. Reson. 138:1999;210-219
41. Kostrzewa A., Páli T., Froncisz W., Marsh D. Membrane location of spin-labeled cytochrome c determined by paramagnetic relaxation agents. Biochemistry. 39:2000;6066-6074
42. Altenbach C., Froncisz W., Hyde J.S., Hubbell W.L. Conformation of spin-labeled melittin at membrane surfaces investigated by pulse saturation recovery and continuous wave power saturation electron paramagnetic resonance. Biophys. J. 56:1989;1183-1191
43. Farahbakhsh Z.T., Altenbach C., Hubbell W.L. Spin labeled cysteines as sensors for protein lipid interaction and conformation in rhodopsin. Photochem. Photobiol. 56:1992;1019-1033
44. Altenbach C., Hubbell W.L. The aggregation state of spin-labeled melittin in solution and bound to phospholipid-membranes: Evidence that membrane-bound melittin is monomeric. Proteins Struct., Funct., Genet. 3:1988;230-242
45. Isas J.M., Langen R., Haigler H.T., Hubbell W.L. Structure and dynamics of a helical hairpin and loop region in annexin 12: a site-directed spin labeling study. Biochemistry. 41:2002;1464-1473
46. Marsh D., Páli T., Horváth L.I. Progressive saturation and saturation transfer EPR for measuring exchange processes and proximity relations in membranes. Berliner L.J. Spin labeling: the next millennium. Biological magnetic resonance. 14:1998;23-82 Plenum Press, New York
47. Hedin E.M.K., Høyrup P., Patkar S.A., Vind J., Svendsen A., Fransson L., et al. Interfacial orientation of Thermomyces lanuginosa lipase on phospholipid vesicles investigated by electron spin resonance relaxation spectroscopy. Biochemistry. 41:2002;14185-14196
48. Cajal Y., Svendsen A., Girona V., Patkar S.A., Alsina M.A. Interfacial control of lid opening in Thermomyces lanuginosa lipase. Biochemistry. 39:2000;413-423