One-Dimensional and Two-Dimensional 1H- and 13C-Nuclear Magnetic Resonance (NMR) Analysis of Vitamin E Raw Materials or Analytical Reference Standards |
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Authors: | Baker John K Myers Chris W |
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Institution: | (1) Department of Medicinal Chemistry, School of Pharmacy, University of Mississippi, University, Mississippi, 38677 |
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Abstract: | Two-dimensional spectral analysis (COSY, HETCOR) was utilized to make the complete 13C- and 1H-NMR assignments for -, -, - -, and -tocopherol as well as for the acetate and succinate esters of -tocopherol. 13C-NMR was found to be especially useful in distinguishing between the various tocopherols and distinguishing between the d-isomer and the d,l-racemic mixture. HETCOR spectra were also found to be useful for the qualitative identification of mixtures of the tocopherols and sesame oil. Using a procedure designed to minimize errors arising from spin relaxation and nuclear Overhauser effects, 13C-NMR peak integrals were used to quantitate -tocopherol and -tocopherol in the presence of sesame oil using benzoic acid as the standard for calibration of the quantitation. The NMR results were compared to a capillary column gas chromatographic analysis of the individual -tocopherol and -tocopherol reference materials.Chris W. Myers: Recipient of the Analysis and Pharmaceutical Quality Section Undergraduate Award in Pharmaceutical Analysis from the APQ Section of the American Association of Pharmaceutical Scientists. |
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Keywords: | -tocopherol determination" target="_blank">gif" alt="agr" align="BASELINE" BORDER="0">-tocopherol determination nuclear Overhauser effect spin lattice relaxation heteronuclear gated decoupling capillary gas chromatographic analysis primary standards vegetable oil sesame oil stereoisomers |
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