Use of 13C nuclear magnetic resonance distortionless enhancement by polarization transfer pulse sequence and multivariate analysis to discriminate olive oil cultivars |
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Authors: | Giovanna Vlahov Adrian D Shaw Douglas B Kell |
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Affiliation: | (1) Institute of Biological Sciences, University of Wales, Aberystwyth, Ceredigion, SY23 3DD Wales, United Kingdom;(2) Istituto Sperimentale per la Elaiotecnica, Contrada Fonte Umano, 65013 Città S. Angelo, Pescara, Italy |
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Abstract: | Distortionless enhancement by polarization transfer (DEPT) pulse sequence was used to set up a quantitative high-resolution
13C nuclear magnetic resonance (NMR) method to discriminate olive oils by cultivars and geographical origin. DEPT pulse sequence
enhances the intensity of NMR signals from nuclei of low magnetogyric ratio. The nuclear spin polarization is transferred
from spins with large Boltzmann population differences (usually protons) to nuclear species characterized by low Boltzmann
factors, e.g., 13C. The signal enhancement of 13C spectra ensures the accuracy of resonance integration, which is a major task when the resonance intensities of different
spectra must be compared. The resonances of triglyceride acyl chains C
n:0, C18:1, C18:2, and C18:3, were also assigned. Multivariate analysis was carried out on the 35 carbon signals obtained. By using variable reduction
techniques, coupled with standard statistical methods—partial least squares and principal components analysis—it was largely
possible to separate the samples according to their variety and region of origin. With one problem variety removed, 100% prediction
of the three remaining varieties was achieved. Similarly, by using the three regions with greatest representation in the data,
all but one of a test set of 34 samples were correctly predicted. Thus, the composition of olive oils from different cultivars
and of different geographical origin were compared and successfully studied by multivariate analysis. These considerations
in conjunction with the structural elucidations of triglyceride molecules demonstrated that 13C NMR is among the most powerful techniques yet described for analysis of olive oils. |
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Keywords: | Multivariate analysis 13C NMR DEPT olive oil |
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