Microwave-assisted extraction followed by headspace solid-phase microextraction and gas chromatography with mass spectrometry detection (MAE-HSSPME-GC-MS/MS) for determination of polybrominated compounds in aquaculture samples

摘要

This paper describes the first validated method for the extraction, purification and determination of trace levels of a number of pollutants of growing concern, including polybrominated biphenyls (PBBs) and polybrominated diphenyl ethers (PBDEs), in aquaculture feeds and products. The new procedure comprises microwave-assisted extraction (MAE; optimized, using a central composite experimental design, to 15 min at 85 °C in 14 mL of 1:1 hexane/dichloromethane), and concentration by headspace solid-phase microextraction (HSSPME), and separation/quantification by gas chromatography with mass spectrometry detection (GC-MS/MS). The method was validated on the reference materials IAEA-406 and WMF-01. Limits of detection for fourteen of the fifteen analytes considered range from 10 to 600 pg g?1, and limits of quantification from 50 pg g?1 to 1.9 ng g?1. Linear ranges, accuracies and precisions are reported.