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1H HR/MAS NMR in the suspended state: Molecular recognition processes in liquid chromatography between steroids and a silica hydride-based cholesterol phase
Journal of Separation Science (2009)
  • V. Freibolin, University of Tuebingen
  • M. P. Bayer, University of Tuebingen
  • Maria T. Matyska-Pesek, San Jose State University
  • J. J. Pesek, San Jose State University
  • K. Albert
Abstract

A mixture of eight steroids was separated by HPLC on a silica hydride-based stationary phase modified with a moiety of cholesteryl 10-undecanoate. Within the steroid mixture progesterone showed the longest retention time suggesting the strongest interaction with the stationary phase material. To obtain more detailed information upon the effective separation process, interaction studies were performed by high resolution/magic angle spinning (HR/MAS) NMR spectroscopy recorded in the suspended state. 1H saturation transfer difference (STD) NMR experiments with T1ρ suppression showed significant hydrophobic binding affinities of progesterone toward the cholesterol column material. These NMR results can be correlated directly to the chromatographic data obtained by HPLC.

Disciplines
Publication Date
2009
Publisher Statement
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Citation Information
V. Freibolin, M. P. Bayer, Maria T. Matyska-Pesek, J. J. Pesek, et al.. "1H HR/MAS NMR in the suspended state: Molecular recognition processes in liquid chromatography between steroids and a silica hydride-based cholesterol phase" Journal of Separation Science Vol. 32 Iss. 10 (2009)
Available at: http://works.bepress.com/maria_matyska-pesek/24/