Simplified micro perchlorination method for polychlorinated biphenyls in biological samples.

Simplified methodology is presented for the micro determination of polychlorinated biphenyls (PCBs) in biological samples, by conversion to the decachlorobiphenyl (DCB) derivative. Beef adipose tissue and human milk extracts were fortified with PCB standards at 0.1--5.0 ppm, and perchlorinated with antimony pentachloride (SbCl5). Several Aroclors representing various degrees of chlorine content were investigated to assess the efficiency of conversion to DCB. Samples were cleaned up on a Florisil mini column and the PCBs were quantitated by electron capture GLC. Several chlorinated pesticides which were subjected to the perchlorination procedure did not interfere. As little as 0.1 ppm PCBs in 500 mg tissue extract can be recovered at 79-99%. The background DCB content of several brands of SbCl5 was determined. The levels of PCBs in human milk obtained by the perchlorination technique are compared with data acquired by electron capture gas-liquid chromatography in which the individual chlorobiphenyls in the sample are measured.