Targeted analysis for detection the adulteration in extra virgin olive oil’s using LC-DAD/ESI–MS/MS and combined with chemometrics tools


The hand-held LC-DAD/ESI–MS/MS approach was employed, for the first time, for the quantification of extra virgin olive oil (EVOO) adulteration with refined pomace olive oil (RPOO). The total polyphenols (TP) and sterols were quantified according to their chemical methods, with more reliable methods required in this field to avoid undue dependence on chlorophylls, carotenoids contents and antioxidant activity (DPPH assays), which were evaluated by spectrophotometric methods. Some differences concerning the antioxidant activity and the TP content were observed. Actually, Chemlali EVOO activity was the most pronounced (13.84 ± 0.21%) and it contained the highest TP content (284.54 ± 4.27 mg/kg). Indeed, a correlation between antioxidant activity, TP and oxidative stability was established herewith. The metabolomics data were elaborated with the help of chemometric tools i.e. principal component analysis (PCA) and hierarchical cluster analysis (HCA). This approach allowed the estimation of the best discrimination markers for EVOO authenticity evaluation (i.e. Hydroxytyrosol quinone, oxidized hydroxytyrosol, 3,4-DHPEA-EA, p-HPEA (tyrosol), p-coumaric acid, luteolin, decarboxymethyl 10-hydroxyoleuropein aglycon, β-sitosterol apparently; campesterol, stigmasterol, ∆-7-stigmastenol and ∆-7-avenasterol).

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Extra virgin olive oil


Refined pomace olive oil


Total Polyphenols


Principal component analysis


Hierarchical cluster analysis


International olive Council


Flame ionization detector


Fatty acid ethyl ester

DPPH radical:

Free radical 2,2-diphenyl-1- picrylhydrazyl


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The authors would like to thank the "Ministère de l’Enseingement Supérieur et de la Recherche Scientifique, Tunisia LR14ES08" and the National Funds through Ministry of Higher Education-Tunisia for financing MedOOmics Project—“Mediterranean Extra Virgin Olive Oil Omics: profiling and fingerprinting”—“Arimnet2/0001/2015”, They are also thankful to Mme. Mariem DRIRA for proofreading and polishing the language of the manuscript.

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Correspondence to Mohamed Bouaziz.

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Drira, M., Kelebek, H., Guclu, G. et al. Targeted analysis for detection the adulteration in extra virgin olive oil’s using LC-DAD/ESI–MS/MS and combined with chemometrics tools. Eur Food Res Technol 246, 1661–1677 (2020).

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  • Extra virgin olive oil adulteration
  • Refined pomace olive oil
  • Correlation analysis
  • Phenolic compounds
  • Chemometrics