Optimization and Validation of a Method Based on QuEChERS Extraction and Gas Chromatographic-Mass Spectrometric Analysis for the Determination of Polycyclic Aromatic Hydrocarbons and Polychlorinated Biphenyls in Olive Fruits Irrigated with Treated Wastewaters

Abstract

The wastewater reuse is an important measure to face water shortage, thus improving the resilience of agricultural production chains. However, treated wastewater can contain residual organic micropollutants residues that may result in crop contamination. Among edible crops, olive is the most important agricultural product in the Mediterranean region. Methods to assess the contamination of organic micropollutants such as polycyclic aromatic hydrocarbons (PAHs) and polychlorinated biphenyls (PCBs) in olives are poorly investigated. Given the complexity of olives, this study focused on the development and validation of a method for the simultaneous extraction of PAHs and PCBs from olives, and subsequent analysis by gas chromatography coupled with mass spectrometry detection. Extraction was optimized through a QuEChERS protocol, studying the effect of the extraction solvent (CH2Cl2, cyclohexane, CH3CN) and of the dispersive-solid phase extraction (d-SPE) sorbent (octadecyl silica, Florisil, primary secondary amine, Z-Sep) on the recovery of micropollutants. The best recoveries (94–122%, relative standard deviations below 5%) were obtained using CH3CN/H2O and a double purification step with Z-Sep and Florisil. The method developed for PAHs and PCBs, which showed good intra-day (<2.7%) and inter-day (<2.9%) precision and low matrix effect (|ME| < 14%), was applied to the analysis of olives grown by irrigation with reclaimed wastewaters.