Summary
Monodeuterated methylene positions exhibit substantially superior spectral characteristics in 1H−13C correlation experiments as compared to diprotio signals. A combination of 2H decoupling and multiplet editing of HMQC and HSQC experiments provides resolution enhancement for both stereoselective and random fractionally deuterated samples. For HMQC experiments with [2-2Hr, 2-13C]glycine-labeled E. coli thioredoxin (11.7 kDa), 3-fold increases in both 1H and 13C resolution result in a complementary 9-fold enhancement in sensitivity. Owing to a smaller improvement in 13C resolution, the corresponding enhancements for the HSQC experiment are 2-fold less.
References
Atkinson J. G., Csakvary J.J., Herbert G.T. and Stuart R.S. (1968) J. Am. Chem. Soc., 90, 498–499.
Bax A. and Freeman R. (1981) J. Magn. Reson., 44, 542–561.
Bax A., Ikura M., Kay L.E., Torchia D.A. and Tschudin R. (1990) J. Magn. Reson., 86, 304–318.
Browne D.T., Kenyon G.L., Packer E.L., Sternlicht H. and Wilson D.M. (1973) J. Am. Chem. Soc., 95, 1316–1323.
Cable, K.M., Herbert, R.B. and Mann, J. (1987) J. Chem. Soc. Perkin Trans. 1, 1593–1598.
Grzesiek S., Dobeli H., Gentz R., Garotta G., Labhardt A.M. and Bax A. (1992) Biochemistry, 31, 8180–8190.
Grzesiek S., Anglister J., Ren H. and Bax A. (1993) J. Am. Chem. Soc., 115, 4369–4370.
Hansen P.E. (1988) Prog. NMR Spectrosc., 20, 207–255.
Ikura M., Kay L.E. and Bax A. (1990) Biochemistry, 29, 4659–4667.
Jaffe E.K. and Markham G.D. (1988) Biochemistry, 27, 4475–4481.
Jaffe E.K., Markham G.D. and Rajagopalan J.S. (1990) Biochemistry, 29, 8345–8350.
Kalbitzer H.R., Leberman R. and Wittinghofer A. (1985) FEBS Lett., 180, 40–42.
Kessler H., Schmieder P. and Kurz M. (1989) J. Magn. Reson., 85, 400–405.
Kushlan, D.M. and LeMaster, D.M. (1993) J. Am. Chem. Soc., 115, in press.
LeMaster D.M. (1990) Q. Rev. Biophys., 23, 133–174.
LeMaster D.M. and Richards F.M. (1988) Biochemistry, 27, 142–150.
Majerski Z., Zuanic M., and Metelko B. (1985) J. Am Chem. Soc., 107, 1721–1726.
Malthouse J.P.G. and Finucane M.D. (1991) Biochem. J., 280, 649–657.
Norwood T.J., Boyd J. and Campbell I.D. (1988) FEBS Lett., 255, 369–371.
Norwood T.J., Boyd J., Heritage J.E., Soffe N. and Campbell I.D. (1990) J. Magn. Reson., 87, 488–501.
Powers R., Gronenborn A.M., Clore G.M. and Bax A. (1991) J. Magn. Reson., 94, 209–213.
Trimble L.A., Reese P.B. and Vederas J.C. (1985) J. Am. Chem. Soc., 107, 2175–2177.
Vuister G.W. and Bax A. (1992) J. Magn. Reson., 98, 428–435.
Wagner G. (1989) Methods Enzymol., 176, 93–113.
Author information
Authors and Affiliations
Rights and permissions
About this article
Cite this article
Kushlan, D.M., LeMaster, D.M. Resolution and sensitivity enhancement of heteronuclear correlation for methylene resonances via 2H enrichment and decoupling. J Biomol NMR 3, 701–708 (1993). https://doi.org/10.1007/BF00198372
Received:
Accepted:
Issue Date:
DOI: https://doi.org/10.1007/BF00198372