title: Validation of a gas chromatography-triple quadrupole mass spectrometry method for confirmatory analysis of dioxins and dioxin-like polychlorobiphenyls in feed following new EU Regulation 709/2014.
abstract: The European Regulations laying down methods of sampling and analysis for the EU official control of levels of polychlorodibenzo-p-dioxins (PCDDs), polychloro-dibenzofurans (PCDFs), dioxin-like (DL) and non dioxin-like (NDL) PCBs in food and feed have been recently amended by EU Regulation Nos. 589/2014 and 709/2014. A major update is the recognition of gas chromatography (GC) triple quadrupole mass spectrometry (GC-QQQMS/MS) as a confirmatory tool for checking compliance with maximum levels (ML). These revisions have been initiated since this technology now exhibits similar performances to GC (magnetic sector) high resolution mass spectrometry (GC-HRMS). In this paper, we show a fully validated method for PCDD/Fs and DL-PCBs analysis in feed material of plant origin (vegetable oil) using GC-QQQMS/MS following the dedicated EU Regulation 709/2014. We show that individual analytical criteria (selectivity, linearity, quant/qual MRM transitions, accuracy around ML of 1.50ng WHO2005TEQ/kg, within-lab reproducibility, robustness, and background subtraction) meet the strict requirements set by the EU Regulation. We also propose a clear interpretation of instrumental limit of quantitation (iLOQ) as a 'performance-LOQ', defined in a specific way for GC-QQQMS/MS, and method limit of quantitation (mLOQ) as 'real-LOQ' that is used to report bound results. Eventually, the evaluation of measurement uncertainty, following a top-down approach and data produced with our method, demonstrates similar results than with GC-HRMS, thus offering a reliable alternative to the standard method for vegetable oil.
authors.affiliation: CART, Organic and Biological Analytical Chemistry Group, Chemistry Department, University of Liège, Allée de la Chimie 3, B6c Sart-Tilman, B-4000 Liège, Belgium. Electronic address: Benjamin.lhomme@ulg.ac.be.
authors.forename: B
authors.initials: B
authors.lastname: L'Homme
authors.affiliation: CART, Organic and Biological Analytical Chemistry Group, Chemistry Department, University of Liège, Allée de la Chimie 3, B6c Sart-Tilman, B-4000 Liège, Belgium.
authors.forename: G
authors.initials: G
authors.lastname: Scholl
authors.affiliation: CART, Organic and Biological Analytical Chemistry Group, Chemistry Department, University of Liège, Allée de la Chimie 3, B6c Sart-Tilman, B-4000 Liège, Belgium.
authors.forename: G
authors.initials: G
authors.lastname: Eppe
authors.affiliation: CART, Organic and Biological Analytical Chemistry Group, Chemistry Department, University of Liège, Allée de la Chimie 3, B6c Sart-Tilman, B-4000 Liège, Belgium.
authors.forename: J-F
authors.initials: JF
authors.lastname: Focant
mesh_terms: D004147:Dioxins / Q000032:analysis*; D005062:European Union; D005504:Food Analysis / Q000379:methods*; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods; D013058:Mass Spectrometry; D010938:Plant Oils / Q000737:chemistry*; D011078:Polychlorinated Biphenyls / Q000032:analysis*; D000072317:Polychlorinated Dibenzodioxins / Q000031:analogs & derivatives* / Q000032:analysis; D015203:Reproducibility of Results
chemical_list: D004147:Dioxins; D010938:Plant Oils; D000072317:Polychlorinated Dibenzodioxins; D011078:Polychlorinated Biphenyls
keywords: Dioxins; EU Regulation 709/2014; Gas chromatography coupled to tandem-in-space triple quadrupole mass spectrometry (GC–QQQMS/MS); Validation; Vegetable oil