Analysis of polychlorinated biphenyls in fatty biological matrixes by on-line supercritical fluid extraction and supercritical fluid cleanup.

We present a method that combines the extraction of polychlorinated biphenyls (PCBs) and their separation from relatively large quantities of fat in biological matrixes by combined supercritical fluid extraction and separation. Cyano-functionalized silica gel, silica gel, aluminum oxide, Florisil, 3-amino-propyl-functionalized silica gel, and octadecyl-functionalized silica gel were tested for suitability as chromatographic media for separation of PCBs from lipids. Silica gel, 3-aminopropyl-functionalized silica gel, and Florisil adequately separated PCBs from lipids when eluted with supercritical CO2. Florisil allowed both the extraction of PCBs and their separation from lipids in PCB-spiked chicken egg and fish. Two grams of sample containing PCBs at 0.125 microgram/g was sufficient for subsequent separations and the low-level analysis required for the more toxic PCB components.