Article pubs.acs.org/JAFC
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 Katherine K. Stenerson,* Olga Shimelis, Michael R. Halpenny, Ken Espenschied, and Maochun M. Ye Sigma-Aldrich, 595 North Harrison Road, Bellefonte, Pennsylvania 16823, United States 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 0.98 for 11 of the 15 target compounds. The highest deviations in measured versus spiked values were E
DOI: 10.1021/jf506299f J. Agric. Food Chem. XXXX, XXX, XXX−XXX
Article
Journal of Agricultural and Food Chemistry
Table 4. PAH Levels in Commercially Purchased Olive Oil Samples, Measured in μg/kg, with Each at an Average of Three Replicate Samples extra-virgin, first cold press
typea
extra-light
extra-light
origina
Spain, Turkey, and Morocco
Italy, Spain, Greece, and Tunisia
naphthalene acenaphthene fluorene phenanthrene anthracene fluoranthene pyrene benzo(a)anthracene chrysene benzo(b)fluoranthene benzo(k)fluoranthene benzo(a)pyrene dibenzo(a,h)anthracene benzo(g,h,i)perylene indeno(1,2,3-cd)pyrene
μg/kg
% RSD (%)b
μg/kg
5.20 0.3 NDd 3.3
