Sample cleanup by solid-phase extraction for the ultratrace determination of polychlorinated dibenzo-p-dioxins and...

A sample cleanup method for the isolation of polychlorinated dibenzo-p-dioxins (PCDDs) and dibenzofurans (PCDFs) by solid-phase extraction is described. A C18 bonded silica cartridge is used for the initial extraction and enrichment of the analytes. Subsequent cleanup is achieved with a dual-cartridge arrangement consisting of a bonded benzenesulfonic acid cartridge in series with a silica cartridge. A Florisil cartridge is employed for the final cleanup step. Sample preparation procedures used for blood plasma and animal tissues are described. The precision and accuracy of the method is validated by determining recoveries of 2,3,7,8-substituted PCDD and PCDF congeners spiked at various levels in blood plasma and in animal tissues. The effectiveness of the cleanup method is shown by the analysis of wild bird eggs which are highly contaminated with a variety of pesticides and polychlorinated biphenyls. The application of this cleanup method to human plasma containing PCDDs/PCDFs at parts-per-quadrillion levels and results of analyses by high-resolution mass spectrometry and low-resolution mass spectrometry are presented. The validity of this method is demonstrated by the comparable results obtained from this method and from other established methods.