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.