Single laboratory validation of an environmentally friendly single extraction and cleanup method for quantitative determination of four priority polycyclic aromatic hydrocarbons in edible oils and fats

Abstract

This paper reports a simple, rapid, reliable and environmentally friendly gas chromatography-mass spectrometry (GC-MS) method for analyzing polycyclic aromatic hydrocarbons (PAHs) in edible oils and fats. The fat sample was first dissolved in acetonitrile while oils were loaded directly onto a solid phase extraction cartridge. PAHs were eluted with acetonitrile. Owing to the background interference, GC-MS was found to be applicable for 4 European Union (EU) priority PAHs (benzo[a]pyrene, benz[a]anthracene, benzo[b]fluoranthene and chrysene) in various types of edible oils and fats, but not for 15+1 EU-priority PAHs. An adequate linear relationship was obtained in the studied concentration range (0.1–60.0 μg kg⁻¹) in samples; analytical limits of detection and quantification were 0.1 and 0.25 μg kg⁻¹, respectively. Due to the lack of a certified reference material, spiked recovery and a FAPAS quality control material were employed to assess the accuracy. The mean spiked recoveries for 4 PAHs, studied at concentration levels of 0.25 (method limit of quantification (MLOQ)), 1.0 and 2.0 μg kg⁻¹, ranged from 86 to 114%. Precision values, expressed as relative standard deviation, were below 10% at aforementioned spiking levels. Extraction and cleanup of a batch of 20 samples can be completed within an hour by one worker. The developed method was successfully applied for the PAH determination in real commercial samples, including lard, olive, corn, peanut, sunflower seed, rapeseed, sesame and vegetable oil.