Magic-Angle 13C NMR Analysis of Hard Wheat Flour and Dough

  • Joel R. Garbow
  • Jacob Schaefer
Part of the Advances in Experimental Medicine and Biology book series (AEMB, volume 302)


Samples of hard wheat flour and dough are analyzed by magic-angle spinning 13C NMR spectroscopy. Cross-polarization magic-angle spinning (CPMAS) 13C NMR spectra of the dry flour allow its starch and protein content to be accurately measured. These two components are phase-separated. Spectra of hydrated hard wheat doughs are collected under both CPMAS and single-pulse carbon with low-power 1H decoupling conditions. The former report on the macromolecular components of the dough, while the latter reveal small molecules which are solubilized by the water. Results of the present study are interpreted as indicating that the protein is largely unaffected by the added water and remains phased-separated from the starch, while water causes significant changes in polymer dynamics of the starch component.


Nuclear Magnetic Resonance Nuclear Magnetic Resonance Spectroscopy Nuclear Magnetic Resonance Study Hard Wheat Starch Component 
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  1. 1.
    S.A. Matz, Modem baking technology, Scientific American November: 122 (1984).Google Scholar
  2. 2.
    D.L. Laidman and R.G. Wyn Jones, eds., “Recent Advances in the Biochemistry of Cereals,” Academic Press, New York (1979).Google Scholar
  3. 3.
    W.M. Shirley and R.G. Bryant, Proton-nuclear spin relaxation and molecular dynamics in the lysozyme-water system, J. Am. Chem. Soc. 104:2910 (1982).CrossRefGoogle Scholar
  4. 4.
    W.B. Wise and P.E. Pfeffer, Measurement of cross-relaxation effects in the proton NMR of water in fibrous collagen and insoluble elastin, Macromolecules 20:1550 (1987).CrossRefGoogle Scholar
  5. 5.
    R.A. Komoroski, ed., “High Resolution NMR Spectroscopy of Synthetic Polymers in Bulk,” VCH, Deerfield Beach (1986).Google Scholar
  6. 6.
    V.D. Fedotov and H. Schneider, “Structure and Dynamics of Bulk Polymers by NMR-Methods,” Springer-Verlag, Heidelberg (1989).CrossRefGoogle Scholar
  7. 7.
    J. Schaefer, E.O. Stejskal, R.A. McKay, and W.T. Dixon, Molecular motion in polycarbonates by dipolar rotational spin-echo 13C NMR, Macromolecules 17:1479 (1984).CrossRefGoogle Scholar
  8. 8.
    J. Schaefer and E.O. Stejskal, Carbon-13 nuclear magnetic resonance of polymers spinning at the magic angle, J. Am. Chem. Soc. 98:1031 (1976).CrossRefGoogle Scholar
  9. 9.
    R.H. Atalla, J.C. Gast, D.V. Sindorf, V.J. Bartuska, and G.E. Maciel, 13C NMR spectra of cellulose polymorphs, J. Am. Chem. Soc. 102:3249 (1980).CrossRefGoogle Scholar
  10. 10.
    W.L. Earl and D.L. VanderHart, High resolution magic angle sample spinning 13C NMR of solid cellulose I, J. Am. Chem. Soc. 102:3251 (1984).CrossRefGoogle Scholar
  11. 11.
    J. Schaefer, M.D. Sefcik, E.O. Stejskal, R.A. McKay, and P.L. Hall, Characterization of the catabolic transformation of lignin in culture using magic-angle carbon-13 nuclear magnetic resonance, Macromolecules 14:557 (1980).CrossRefGoogle Scholar
  12. 12.
    G.E. Maciel, J.F. Haw, D.H. Smith, B.C. Gabrielson, and G.R. Hatfield, Carbon-13 nuclear magnetic resonance of herbaceous plants and their components, using cross polarization and magic-angle spinning, J. Agric. Food Chem. 33:185 (1985).CrossRefGoogle Scholar
  13. 13.
    N.G. Lewis, J. Newman, G. Just, and J. Ripmeister, Determination of bonding patterns of 13C specifically enriched dehydrogenatively polymerized lignin in solution and solid state, Macromolecules 20:1752 (1987).CrossRefGoogle Scholar
  14. 14.
    R. Botto, Synthesis and characterization of [13C] lignins. Macromolecules 21:1246 (1988).CrossRefGoogle Scholar
  15. 15.
    T. Zlotnik-Mazori and R.E. Stark, Nuclear magnetic resonance studies of cutin, an insoluble plant polyester, Macromolecules 21:2412 (1988).CrossRefGoogle Scholar
  16. 16.
    R.E. Stark, T. Zlotnik-Mazori, D.M. Ferrantello, and J.R. Garbow, Molecular structure and dynamics of intact plant polyesters: solid-state NMR studies, in: “Plant Cell Wall Polymers, Biogenesis and Biodegradation,” N.G. Lewis and M.G. Paice, eds., ACS, Washington, DC (1989).Google Scholar
  17. 17.
    J.R. Garbow, L.M. Ferrantello, and R.E. Stark, 13C nuclear magnetic resonance study of suberized potato cell wall, Plant Physiology 90:783 (1989).CrossRefGoogle Scholar
  18. 18.
    E.O. Stejskal, J. Schaefer, and T.R. Steger, High-resolution 13C nuclear magnetic resonance in solids, Faraday Disc. Chem. Soc. 13:56 (1979).Google Scholar
  19. 19.
    E.O. Stejskal, J. Schaefer, M.D. Sefcik, and R.A. McKay, Magic-angle carbon-13 nuclear magnetic resonance study of the compatibility of solid polymeric blends, Macromolecules 14:275 (1981).CrossRefGoogle Scholar
  20. 20.
    J. Schaefer, J.R. Garbow, E.O. Stejskal, and J. Lefalar, Plasticization of butvar resins, Macromolecules 20:1271 (1987).CrossRefGoogle Scholar
  21. 21.
    A. Pines, M.G. Gibby, and J.S. Waugh, Proton-enhanced NMR of dilute spins in solids, J. Chem. Phys. 59:569 (1973).CrossRefGoogle Scholar
  22. 22.
    E.R. Andrew, A. Bradbury, and R.G. Eades, Nuclear magnetic resonance spectra from a crystal rotated at high speed, Nature 182:1659 (1958).CrossRefGoogle Scholar
  23. 23.
    I.J. Lowe, Free induction decays of rotating solids, Phvs. Rev. Lett. 2:285 (1959).CrossRefGoogle Scholar
  24. 24.
    J.R. Havens and D.L. VanderHart, Morphology of poly(ethylene terephthalate) fibers as studied by multiple-pulse 1H NMR, Macromolecules 18:1663 (1985).CrossRefGoogle Scholar
  25. 25.
    W. Rothwell and J. Waugh, Transverse relaxation of dipolar coupled spin systems under r.f. irradiation: detecting motions in solids, J. Chem. Phvs. 74:2721 (1981).CrossRefGoogle Scholar
  26. 26.
    J.R. Garbow, J. Schaefer, E.O. Stejskal, and G.S. Jacob, Protein dynamics from chemical shift and dipolar rotational spin-echo 15N NMR, Biochemistry 28:1362 (1989).CrossRefGoogle Scholar
  27. 27.
    J.R. Garbow and J. Schaefer, J. Agric. Food Chem.. in press.Google Scholar

Copyright information

© Springer Science+Business Media New York 1991

Authors and Affiliations

  • Joel R. Garbow
    • 1
  • Jacob Schaefer
    • 2
  1. 1.Physical Sciences Center, Monsanto Corporate ResearchMonsanto CompanySt. LouisUSA
  2. 2.Department of ChemistryWashington UniversitySt. LouisUSA

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