Abstract.
We report results of applying a commercial implementation of the dissolution dynamic nuclear polarization (DNP) methodology developed by K. G. Golman et al. to a range of molecular species in the mass range of 100–400 Da. The molecules are typical of those that might be encountered in natural product chemistry or pharmaceutical analysis. Using an experimental protocol previously reported, in combination with the ERETIC method for generating a reference signal for estimation of concentrations, we determine the signal enhancement and high-field, liquid-state T 1 values for many of the carbon atoms in the six species studied. The results presented in this work suggest that the measured variation in nuclear magnetic resonance enhancements within a given molecule, arising from the dissolution DNP method, is accounted for principally by relaxation of 13C atoms towards thermal polarization values in the liquid state. We conclude that dissolution DNP will be able to be employed for a wide range of chemical species, provided that the total time taken for dissolution and transfer of solutions is comparable to, or shorter than, the high-field, liquid-state T 1 values in the species being studied.
References
Wolber, J., Ellner, F., Fridlund, B., Gram, A., Johannesson, H., Hansson, G., Hansson, L.H., Lerche, M.H., Mansson, S., Servin, R., Thaning, M., Golman, K., Ardenkjaer-Larsen, J.H.: Nucl. Instrum. Methods Phys. Res. A 526, 173–181 (2004)
Ardenkjaer-Larsen, J.H., Fridlund, B., Gram, A., Hansson, G., Hansson, G., Lerche, M.H., Servin, R., Thaning, M., Golman, K.: Proc. Natl. Acad. Sci. USA 100, 10158–10163 (2003)
Eldridge, G.R., Vervoort, H.C., Lee, C.M., Cremin, P.A., Williams, C.T., Hart, S.M., Goering, M.G., O'Neil-Johnson, M., Zeng, L.: Anal. Chem. 74, 3963–3971 (2002)
Branch, S.K.: J. Pharm. Biomed. Anal. 38, 798–805 (2005)
Ardenkjaer-Larsen, J.H., Laursen, I., Leunbach, I., Ehnholm, G., Wistrand, L.G., Petersson, J.S., Golman, K.: J. Magn. Reson. 133, 1–12 (1998)
Day, I.J., Mitchell, J.C., Snowden, M.J., Davis, A.L.: J Magn Reson. 187, 216–224 (2007)
Day, I.J., Mitchell, J.C., Snowden, M.J., Davis, A.L.: Magn. Reson. Chem. 45, 1018–1021 (2007)
Akoka, S., Barantin, L., Trierweiler, M.: Anal. Chem. 71, 2554–2557 (1999)
Cavanagh, J., Fairbrother, W.J., Palmer, A.G. III, Skelton, N.J.: Protein NMR Spectroscopy: Principles and Practice. Academic Press, New York (1996)
Höfer, P., Parigi, G., Luchinat, C., Carl, P., Guthausen, G., Reese, M., Carlomagno, T., Griesinger, C., Bennati, M.: J. Am. Chem. Soc. 130, 3254–3255 (2008)
Piotto, M., Bourdonneau, M., Elbayed, K., Wieruszeksi, J.-M., Lippens, G.: Magn. Reson. Chem. 44, 943–947 (2006)
Vasos, P.R., Hall, J.B., Kummerle, R., Fushman, D.: J. Biomol. NMR 36, 27–36 (2006)
Frydman, L., Blazina, D.: Nat. Phys. 3, 415–419 (2007)
Galiana, G., Branca, R.T., Warren, W.S.. J. Am. Chem. Soc. 127, 17574–17575 (2005)
Fukushi, E.: Biosci. Biotechnol. Biochem. 70, 1803–1812 (2006)
Bax, A., Mehlkopf, A.F., Smidt, J., Freeman, R.: J. Magn. Reson. 41, 502–506 (1980)
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Authors' address: Adrian L. Davis, Pfizer Global Research and Development, Sandwich Laboratories, Ramsgate Road, Sandwich CT13 9NJ, United Kingdom
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Day, I., Mitchell, J., Snowden, M. et al. Investigation of the Potential of the Dissolution Dynamic Nuclear Polarization Method for General Sensitivity Enhancement in Small-Molecule NMR Spectroscopy. Appl Magn Reson 34, 453–460 (2008). https://doi.org/10.1007/s00723-008-0122-8
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DOI: https://doi.org/10.1007/s00723-008-0122-8