RAPID METHOD FOR SIMULTANEOUS DETERMINATION OF PCBS, PBDES AND PAHS IN FISH SAMPLES

摘要

Analytical methods for determination of various organic contaminants such as polychlorinated biphenyls (PCBs), polybrominated diphenyl ethers (PBDEs) and polyaromatic hydrocarbons (PAHs) in environmental and food matrices are typically based on multistep procedures that include Soxhlet extraction with a subsequent clean up and fractionation steps prior to relatively slow gas chromatography (GC) runs using either an electron capture (ECD) or a mass spectrometric (MS) detection in case of halogenated analytes, PAHs are commonly analysed separately using a liquid chromatography coupled to a fluorescence detector (LC-FLD), but for several non-flurescence PAHs including in the EFSA opinion, a GC-MS analysis is needed. In this study, the fast extraction and clean-up procedure of all mentioned pollutants from a fish fillet by a pressurised liquid extraction (PLE) has been tested. The main goal was to optimize an appropriate extraction/clean up procedure and to demonstrate the separation power of comprehensive two-dimensional gas chromatography (GC×GC) coupled with a time-of-flight detector (TOF) for analysis of PCBs, PBDEs and PAHs in a single run. Repeatability of this simplified sample preparation procedure for all target analytes, expressed as relative standard deviation (RSD, n=6) ranged from 3 to 19% and recovery on the level 1 μg/kg ranged from 71 to 121%.