Analysis of polychlorinated biphenyls in human serum by gas chromatography–mass selective detection operating at high ion source temperature

Abstract

Optimization of analytical instrumentation is essential when analyses of persistent organic pollutants in human serum are performed at ultra-trace levels. This research describes the analysis of polychlorinated biphenyls (PCBs) in serum using gas chromatography coupled with a mass selective detector (GC/MSD) in the selected ion monitoring (SIM) mode. We selected PCB-58 and PCB-186 as internal standards (ISs) for the method development, and newborn calf serum (NCS) was chosen as the matrix. The matrix was fortified with PCB congeners and extracted by an automated solid phase extraction system using C18 sorbent. The extracts were analyzed at two ion source temperatures, 230 and 300 °C. The use of high ion source temperature increased the abundances of high-mass ions, and the response factors in SIM mode for PCBs. An excellent linearity from 0.5 to 100 ng/ml at ion source temperature of 300 °C was demonstrated, with a calculated detection limit of 0.1 ng/g serum. Seven replicate fortifications of newborn calf serum, at three spiking levels of 1, 10, and 50 ng/g of serum, gave mean recoveries of 110%, 85%, and 98%, with average relative standard deviation (RSD) values of 5.4%, 7.3%, and 4.7%, respectively.