Rapid determination of PCDDs, PCDFs and DL-PCBs in foods, feeding stuffs and vegetable oils using new modified acid silica

Abstract

Polychlorinated dibenzo-p-dioxins, dibenzofurans and dioxin-like polychlorinated biphenyls are persistent organic pollutants (POPs), which in recent years received huge attention due to their extreme stability, high potential toxicity and bioaccumulation in food chains. The main source of human exposure to these compounds is discovered in foods of animal origin, especially foods rich in fat. The target of the present study was to set up an analytical method for the determination of PCDDs/PCDFs and DL-PCB in vegetable oils, sunflower meals, sunflower seeds, rapeseeds and milk powder. The first step consisted of a semi-automatic Soxhlet extraction for 3 hours, by using a mixture of Hexane: Acetone – 80:20, followed by acid digestion with 55% acid silica and filtration. After concentration, the extract is purified on a multilayer column (silica gel, silica-KOH, silica-H2SO4 anhydrous Na2SO4) followed by an alumina column separation in two fractions (first fraction containing PCDDs/PCDFs and second containing only PCBs). The purified extract was then analyzed by GC/MS/MS. The newly developed approach in our lab was capable to reduce the overall time of sample preparation to seven hours/ per sample. Since the method shows good mean recoveries for all labeled congeners spiked in the samples (for PCDDs/PCDFs – 80% - 110%, for DL-PCBs – 70% - 85%), we assumed the absence of overestimation or underestimation in the analyzed samples.