Non-targeted screening for contaminants in paper and board food-contact materials using effect-directed analysis and accurate mass spectrometry

Linda Bengtström, Anna Kjerstine Rosenmai, Xenia Trier, Lisbeth Krüger Jensen, Kit Granby, Anne Marie Vinggaard, Malcolm Driffield, Jens Højslev Petersen

Research output: Contribution to journalJournal articleResearchpeer-review

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.
Original languageEnglish
JournalFood Additives & Contaminants: Part A - Chemistry, Analysis, Control, Exposure & Risk Assessment
Volume33
Issue number6
Pages (from-to)1080-1093
Number of pages14
ISSN1944-0049
DOIs
Publication statusPublished - 2016

Keywords

  • Food Science
  • Health, Toxicology and Mutagenesis
  • Public Health, Environmental and Occupational Health
  • Toxicology
  • Chemistry (all)
  • aryl hydrocarbon receptor activity
  • effect-directed analysis
  • Food packaging
  • high-resolution mass spectrometry
  • non-target analysis
  • paper and board

Cite this

@article{c3bb1ecefede445d8657bad1bbdcb591,
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.",
keywords = "Food Science, Health, Toxicology and Mutagenesis, Public Health, Environmental and Occupational Health, Toxicology, Chemistry (all), aryl hydrocarbon receptor activity, effect-directed analysis, Food packaging, high-resolution mass spectrometry, non-target analysis, paper and board",
author = "Linda Bengtstr{\"o}m and Rosenmai, {Anna Kjerstine} and Xenia Trier and Jensen, {Lisbeth Kr{\"u}ger} and Kit Granby and Vinggaard, {Anne Marie} and Malcolm Driffield and Petersen, {Jens H{\o}jslev}",
year = "2016",
doi = "10.1080/19440049.2016.1184941",
language = "English",
volume = "33",
pages = "1080--1093",
journal = "Food Additives & Contaminants: Part A - Chemistry, Analysis, Control, Exposure & Risk Assessment",
issn = "1944-0049",
publisher = "Taylor & Francis Online",
number = "6",

}

TY - JOUR

T1 - Non-targeted screening for contaminants in paper and board food-contact materials using effect-directed analysis and accurate mass spectrometry

AU - Bengtström, Linda

AU - Rosenmai, Anna Kjerstine

AU - Trier, Xenia

AU - Jensen, Lisbeth Krüger

AU - Granby, Kit

AU - Vinggaard, Anne Marie

AU - Driffield, Malcolm

AU - Petersen, Jens Højslev

PY - 2016

Y1 - 2016

N2 - 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.

AB - 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.

KW - Food Science

KW - Health, Toxicology and Mutagenesis

KW - Public Health, Environmental and Occupational Health

KW - Toxicology

KW - Chemistry (all)

KW - aryl hydrocarbon receptor activity

KW - effect-directed analysis

KW - Food packaging

KW - high-resolution mass spectrometry

KW - non-target analysis

KW - paper and board

U2 - 10.1080/19440049.2016.1184941

DO - 10.1080/19440049.2016.1184941

M3 - Journal article

C2 - 27146477

VL - 33

SP - 1080

EP - 1093

JO - Food Additives & Contaminants: Part A - Chemistry, Analysis, Control, Exposure & Risk Assessment

JF - Food Additives & Contaminants: Part A - Chemistry, Analysis, Control, Exposure & Risk Assessment

SN - 1944-0049

IS - 6

ER -