title: Non-targeted screening for contaminants in paper and board food-contact materials using effect-directed analysis and accurate mass spectrometry.
abstract: Due to large knowledge gaps in chemical composition and toxicological data for substances involved, paper and board food-contact materials (P&B FCM) have been emerging as a FCM type of particular concern for consumer safety. This study describes the development of a step-by-step strategy, including extraction, high-performance liquid chromatography (HPLC) fractionation, tentative identification of relevant substances and in vitro testing of selected tentatively identified substances. As a case study, we used two fractions from a recycled pizza box sample which exhibited aryl hydrocarbon receptor (AhR) activity. These fractions were analysed by gas chromatography (GC) and ultra-HPLC (UHPLC) coupled to quadrupole time-of-flight mass spectrometers (QTOF MS) in order tentatively to identify substances. The elemental composition was determined for peaks above a threshold, and compared with entries in a commercial mass spectral library for GC-MS (GC-EI-QTOF MS) analysis and an in-house built library of accurate masses for substances known to be used in P&B packaging for UHPLC-QTOF analysis. Of 75 tentatively identified substances, 15 were initially selected for further testing in vitro; however, only seven were commercially available and subsequently tested in vitro and quantified. Of these seven, the identities of three pigments found in printing inks were confirmed by UHPLC tandem mass spectrometry (QqQ MS/MS). Two pigments had entries in the database, meaning that a material relevant accurate mass database can provide a fast tentative identification. Pure standards of the seven tentatively identified substances were tested in vitro but could not explain a significant proportion of the AhR-response in the extract. Targeted analyses of dioxins and PCBs, both well-known AhR agonists, was performed. However, the dioxins could explain approximately 3% of the activity observed in the pizza box extract indicating that some very AhR active substance(s) still remain to be identified in recycled low quality P&B.
authors.affiliation: a Division of Food Chemistry , National Food Institute, Technical University of Denmark , Søborg , Denmark.
authors.forename: Linda
authors.initials: L
authors.lastname: Bengtström
authors.affiliation: b Division of Diet, Disease Prevention, and Toxicology , National Food Institute, Technical University of Denmark , Søborg , Denmark.
authors.forename: Anna Kjerstine
authors.initials: AK
authors.lastname: Rosenmai
authors.affiliation: a Division of Food Chemistry , National Food Institute, Technical University of Denmark , Søborg , Denmark.
authors.forename: Xenia
authors.initials: X
authors.lastname: Trier
authors.affiliation: a Division of Food Chemistry , National Food Institute, Technical University of Denmark , Søborg , Denmark.
authors.forename: Lisbeth Krüger
authors.initials: LK
authors.lastname: Jensen
authors.affiliation: a Division of Food Chemistry , National Food Institute, Technical University of Denmark , Søborg , Denmark.
authors.forename: Kit
authors.initials: K
authors.lastname: Granby
authors.affiliation: b Division of Diet, Disease Prevention, and Toxicology , National Food Institute, Technical University of Denmark , Søborg , Denmark.
authors.forename: Anne Marie
authors.initials: AM
authors.lastname: Vinggaard
authors.affiliation: c Fera Science Ltd , National Agrifood Innovation Campus , York , UK.
authors.forename: Malcolm
authors.initials: M
authors.lastname: Driffield
authors.affiliation: a Division of Food Chemistry , National Food Institute, Technical University of Denmark , Søborg , Denmark.
authors.forename: Jens
authors.initials: J
authors.lastname: Højslev Petersen
mesh_terms: D002851:Chromatography, High Pressure Liquid / Q000379:methods; D004147:Dioxins / Q000032:analysis; D005506:Food Contamination / Q000032:analysis*; D018857:Food Packaging / Q000295:instrumentation*; D059022:Food Safety; D008401:Gas Chromatography-Mass Spectrometry; D007281:Ink; D013058:Mass Spectrometry / Q000379:methods*; D010209:Paper; D011078:Polychlorinated Biphenyls / Q000032:analysis; D018336:Receptors, Aryl Hydrocarbon / Q000032:analysis; D059027:Recycling; D021241:Spectrometry, Mass, Electrospray Ionization; D053719:Tandem Mass Spectrometry
chemical_list: D004147:Dioxins; D018336:Receptors, Aryl Hydrocarbon; D011078:Polychlorinated Biphenyls
keywords: Food packaging; aryl hydrocarbon receptor activity; effect-directed analysis; high-resolution mass spectrometry; non-target analysis; paper and board