Systematic investigation of factors controlling supercritical fluid extraction (SFE) of spiked and aged PCBs from edible tissues of the blue crab (Callinectes sapidus).

Systematic investigation of factors controlling supercritical fluid extraction (SFE) of spiked and naturally incurred (aged) PCBs from edible tissues of the Blue Crab (Callinectes sapidus) was undertaken. Effects of extraction pressure, temperature and time, CO2 flow rate and total volume, and collection temperature were assessed. Temperature dramatically impacted extraction efficiency, especially at lower pressures. Surprisingly, extraction of both spiked and aged PCBs was flow rate dependent, counter to prevailing views regarding the relative ease of SFE of spiked versus aged contaminants from environmental matrices. PCBs were optimally trapped on a 1:1 mixture of C18-modified and porous silica at 0°C and eluted with <2 mL isooctane at 90°C. A combined 10 min static/30 min dynamic extraction at 35.5 MPa and 150°C with a CO2 flow rate of 3 mL min(-1) yielded maximum (quantitative) recoveries of spiked and aged PCBs. Resulting solvent extracts required no cleanup and could be analyzed directly by halogen-selective GC with MS confirmation.