Metabolic fingerprinting strategy: Investigation of markers for the detection of extra virgin olive oil adulteration with soft-deodorized olive oils

Abstract

As extra virgin olive oil (EVOO) is a high value commodity, it might be subject of various fraudulent practices. This study is focused on a challenging authentication issue, addition of lower grade, soft-deodorized olive oil to EVOO. In the first step, sample sets of authentic EVOOs, soft-deodorized oils and their admixtures were extracted by aqueous methanol; obtained polar fractions were then analysed by ultra-high performance liquid chromatography coupled to hybrid quadrupole time-of-flight high-resolution tandem mass spectrometry (UHPLC-QTOF-HRMS/MS). Subsequent chemometric evaluation of metabolic fingerprints enabled suggestion of several ions that might be characteristic for deodorized oils; most of tentatively identified compounds were oxidized fatty acid derivatives. In the second phase, the ‘marker' ions were employed for target analysis by ultra-high performance liquid chromatography coupled to triple quadrupole tandem mass spectrometry (UHPLC-QqQ-MS/MS) what enabled achieving lower the detection limits. Two compounds were selected as the best markers for detection of soft-deodorized olive oil addition, tentatively identified as methyl ester of hydroxy octadecenoic acid and ester derivative of oleic acid. • Addition of soft-deodorized olive oil into extra virgin olive oil was studied. • Untargeted approach revealed new markers emerging in soft-deodorization process. • Markers were successfully tested by target approach to be used in routine practice. • Best markers were tentatively identified as fatty acid esters.