Assessment of comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry based methods for investigating 206 dioxin-like micropollutants in animal-derived food matrices

•GC × GC-TOF/MS enabled 206 dioxin-related micropollutants in solvent to be separated.•A sample preparation protocol was set up for the analysis of complex food matrices.•A powerful food spiking method was proposed.•The LODs ranged between 50 and 227 pg/g.

This paper evaluates different multiresidue methods based on comprehensive two-dimensional gas chromatography coupled to time-of-flight mass spectrometry (GC × GC-TOF/MS) to analyze dioxin-related micropollutants in complex food matrices. In a first step, the column sets Rtx-PCB/BPX-50 and Rtx-Dioxin2/BPX-50 were compared in terms of peak shape (width and symmetry) and resolution for the separation of polychlorinated biphenyls (PCBs) and polychlorinated dibenzo-p-dioxins/dibenzofurans (PCDD/Fs) in solvent. A satisfactory separation of 206 dioxin-related micropollutants including the 17 toxic PCDD/Fs was achieved in 75 min with the column set Rtx-Dioxin2/BPX-50. In a second time, the GC × GC-TOF/MS method was spread to the analysis of dioxin-related micropollutants in complex food matrices. An extraction procedure including accelerated solvent extraction (ASE), centrifugal evaporation and gel permeation chromatography (GPC) was optimized. Starting with meat as a model matrix, a micropollutant spiking method was then set up by comparing seven methods in terms of recoveries and reproducibility. The method combining immersion of the meat in a large volume of solvent containing micropollutants followed by homogenization by blender induced recoveries in the acceptable range of 70–130% and satisfactory standard deviations (≤10%) for most of the compounds studied. Limits of detection of the GC × GC-TOF/MS method ranged between 50 and 100 pg/g of spiked fresh meat for PCBs and between 65 and 227 pg/g for PCDD/Fs. Potential applications of this method are discussed.