Gas-chromatographic determination of polychlorinated biphenyls in water after headspace solid-phase microextraction

Headspace-analytical techniques are usually applied to the determination of easily volatile substances in water, whereas semivolatiles are generally isolated by liquid-liquid or solid-phase extraction. In the present paper, a method is presented for isolating high boiling polychlorinated biphenyls (PCB) using headspace solid-phase microextraction at elevated temperature. In spite of their low vapor pressure, the analytes are adsorbed very efficiently on a polydimethylsiloxane-coated fiber. Thus, in combination with GC/ECD, a very simple and sensitive solventless determination of PCB is accomplished. Using the simplest possible standard conditions, limits of determination in the lowest nanogram-per-liter range are achieved. Further increased sensitivity down to the ppq (parts per quadrillion) range is possible by stirring and increasing the sample volume and adsorption time. Moderate matrix effects have been observed in some surface and groundwaters.