The authentication of virgin olive oil samples requires usually the use of sophisticated and very expensive analytical techniques, so there is a need for fast and inexpensive analytical techniques for use in a quality control methodology. Virgin olive oils present an intense fluorescence spectra. Synchronous excitation-emission fluorescence spectroscopy (SEEFS) was assessed for origin determination of virgin olive oil samples from five French registered designation of origins (RDOs) (Nyons, Vallée des Baux, Aix-en-Provence, Haute-Provence, and Nice). The spectra present bands between 600 and 700 nm in emission due to chlorophylls a and b and pheophytins a and b. The bands between 275 and 400 nm in emission were attributed to alpha-, beta-, and gamma-tocopherols and to phenolic compounds, which characterize the virgin olive oils compared to other edible oils. The chemometric treatment (PLS1) of synchronous excitation-emission fluorescence spectra allows one to determine the origin of the oils from five French RDOs (Baux, Aix, Haute-Provence, Nice, and Nyons). Results were quite satisfactory, despite the similarity between two denominations of origin (Baux and Aix) that are composed by some common cultivars (Aglandau and Salonenque). The interpretation of the regression coefficients shows that RDOs are correlated to chlorophylls, pheophytins, tocopherols, and phenols compounds, which are different for each origin. SEEFS is part of a global analytic methodology that associates spectroscopic and chromatographic techniques. This approach can be used for traceability and vindicates the RDOs.
Chemometric treatment of near‐infrared (NIR) and mid‐infrared (MIR) combined spectra was used firstly to predict oil and water contents in fresh olive fruit samples (n = 223) and secondly to classify these samples into five principal French cultivar origins (Aglandau, Cailletier, Olivière, Salonenque, and Tanche). The study was carried out during four crop years (2005/2006 to 2008/2009) to take into account the seasonal variations. The comparison of the results obtained in the combined range (REP = 2.6% for the water content and 3.5% for the oil content) provides an obvious advantage compared to the NIR and MIR techniques used separately. Fresh olive fruit cultivars were satisfactorily classified with the partial least squares‐discriminant analysis (PLS‐DA) method in the combined range. After use of the K‐means clustering on the PLS‐DA scores, all the samples were well classified into their five groups of origin. The use of infrared combined spectra allows a considerable improvement in estimating olive fruit quality (oil and water contents, varietal origins).
International audienceThe search for the origin and the authentication of virgin olive oils (VOOs) is a problem of topical interest. VOOs with the protected designation of origin (PDO) label can be subject to fraudulent practices owing to high price commanded by these oils. This work evaluates the capability of confocal Raman spectroscopy combined with chemometric treatments for determining the fatty acid and triacylglycerol (TAG) compositions of VOOs and for authenticating the PDO labels of six French VOOs. Fatty acid and TAG compositions were determined by chemometric analysis of the Raman spectra using the partial least square (PLS) algorithms. Predictions have provided good results on the high percentage compounds, but for the fatty acids at very low percentages the predicted results were very poor. The PLS-discriminant analysis model on Raman spectra was able to correctly classify 92.3% of French PDOs and 100% of PDO samples made with only one principal cultivar. However, it was noticeable that the first regression coefficient (which explains the greatest amount of variation of the data) obtained for each PDO could be compared one by one with the first regression coefficient obtained for the quantitative analysis of fatty acids and TAGs. The first regression coefficients obtained for PDOs differed widely from each other. Their study allowed interpreting the PDOs according to their chemical composition. This work confirms that fatty acid and TAG percentages may be used to authenticate French VOOs into PDO
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