Development and validation of a quantitative UHPLC-MS/MS method for selected brominated flame retardants in food

Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2018 Feb;35(2):292-304. doi: 10.1080/19440049.2017.1393110. Epub 2017 Oct 31.

Abstract

An ultra-high performance liquid chromatography - tandem mass spectrometry (UHPLC-MS/MS) method was developed and validated (in-house) for the quantification of selected brominated flame retardants (BFRs), including tetrabromobisphenol A (TBBPA), hexabromocyclododecanes (HBCDs), tetrabromobisphenol S (TBBPS) and bromophenols (BPs), in various food matrices. The sample preparation consisted of extraction of TBBPS with acidified acetonitrile followed by a fast dispersive solid-phase extraction (dSPE) clean-up and extraction of the other BFRs with a mixture of hexane and dichloromethane (1:1, v/v) with subsequent clean-up using acidified silica (44%, w/w). The limits of quantification of the method varied widely for the types of food matrices and the different classes of BFRs from 4 pg g-1 wet weight (ww) to 8 ng g-1 ww. For most of the analytes the apparent recovery was in the range 70-120%, and the method precision (under repeatability conditions) was below 20%. The method was successfully applied in proficiency testing exercises as well as for analysis of various food items. Only 25% of the collected food samples contained BFRs, with 4-bromophenol and α-HBCD as the only detected compounds. The contaminated foodstuffs were fish and eggs with concentrations in the range from 48 to 305 pg g-1 ww.

Keywords: Brominated flame retardants; HBCDsTBBPA; UHPLC-MS/MS; bromophenols; food analysis.

Publication types

  • Validation Study

MeSH terms

  • Chromatography, High Pressure Liquid
  • Flame Retardants / analysis*
  • Food Analysis / methods*
  • Food Analysis / standards*
  • Food Contamination / analysis*
  • Halogenation
  • Hydrocarbons, Brominated / analysis*
  • Polybrominated Biphenyls / analysis*
  • Solid Phase Extraction
  • Tandem Mass Spectrometry

Substances

  • Flame Retardants
  • Hydrocarbons, Brominated
  • Polybrominated Biphenyls
  • hexabromocyclododecane
  • tetrabromobisphenol A