RESUMO
There is a need for cost-efficient alternatives to gas chromatography (GC)-high-resolution mass spectrometry (HRMS) for the analysis of polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDD/Fs) and dioxin-like polychlorinated biphenyls (PCBs) in food and feed. Comprehensive two-dimensional GC-micro electron capture detection (GC x GC-microECD) was tested and all relevant (according to the World Health Organisation, WHO) PCDD/Fs and PCBs could be separated when using a DB-XLB/LC-50 column combination. Validation tests by two laboratories showed that detectability, repeatability, reproducibility and accuracy of GC x GC-microECD are all statistically consistent with GC-HRMS results. A limit of detection of 0.5 pg WHO PCDD/F tetrachlorodibenzo-p-dioxin equivalency concentration per gram of fish oil was established. The reproducibility was less than 10%, which is below the recommended EU value for reference methods (less than 15%). Injections of vegetable oil extracts spiked with PCBs, polychlorinated naphthalenes and diphenyl ethers at concentrations of 200 ng/g showed no significant impact on the dioxin results, confirming in that way the robustness of the method. The use of GC x GC-microECD as a routine method for food and feed analysis is therefore recommended. However, the data evaluation of low dioxin concentrations is still laborious owing to the need for manual integration. This makes the overall analysis costs higher than those of GC-HRMS. Further developments of software are needed (and expected) to reduce the data evaluation time. Combination of the current method with pressurised liquid extraction with in-cell cleanup will result in further reduction of analysis costs.