Miniaturised selective pressurised liquid extraction of polychlorinated biphenyls from foodstuffs

The feasibility of miniaturised pressurised liquid extraction (PLE) with in-cell purification and subsequent gas chromatography with micro-electron capture detection (GC–micro-ECD) for the determination of prioritary and toxic polychlorinated biphenyls (PCBs) in a variety of foodstuffs (fat contents in the range 22–49%, w/w, on a freeze-dried basis) has been investigated. After optimisation of the several experimental parameters affecting the efficiency of the selective PLE process, the developed method provided quantitative recoveries of the endogenous PCBs studied and complete fat elimination in a single step using n-hexane as extraction solvent. A total solvent volume of 3.5 mL was used for the two consecutive 7 min static PLEs of 100-mg samples. Detection limits using GC–micro-ECD were below 0.2 ng/g freeze dried sample for all 22 PCBs investigated in real-life foodstuffs, and the repeatability of the complete PLE plus GC–micro-ECD method as calculated for the analysis of the endogenous PCBs in general was better than 14%. Comparison of the miniaturised PLE method developed with either conventional Soxhlet extraction or matrix solid phase dispersion with subsequent (off-line) clean-up for the analysis of non-spiked samples showed that the efficiency of PLE was similar to or better (recoveries in the range 83–133%, as calculated for the endogenous analytes) than for the other two extraction methods assayed.