Analysis of polynuclear aromatic hydrocarbons in olive oil after solid-phase extraction using a dual-layer sorbent cartridge followed by high-performance liquid chromatography with fluorescence detection.

ABSTRACT

A simple and easy direct solid-phase extraction (SPE) method was developed for the analysis of polynuclear aromatic hydrocarbons (PAHs) in olive oil using a dual-layer cartridge containing activated Florisil and a mixture of octadecyl (C18)-bonded and zirconia-coated silicas. Undiluted olive oil was applied directly to the SPE cartridge, and the sample was eluted with acetonitrile solvent. Background in the extract was found to be low enough for either gas chromatography-mass spectrometry (GC-MS) or high-performance liquid chromatography with fluorescence detection (HPLC-FLD) analysis. Average recoveries for 16 different PAHs from spiked olive oil replicates were >75%, with intraday precisions of <20% relative standard deviation (% RSD). Detection limits ranged from 0.2 to 1.0 µg/kg and, specifically for the PAHs listed in EC Regulation 835/2011, benzo(a)anthracene, chrysene, benzo(b)fluoranthene, and benzo(a)pyrene, were from 0.3 to 0.7 µg/kg. The method was then applied to determine the PAH content present in commercial samples of refined versus extra-virgin olive oils.