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

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
• UHPLC-MS/MS
• bromophenols
• HBCDsTBBPA
• food analysis

Acknowledgments

This work was financed by the Belgian Federal Public Service (FPS) Health, Food Chain Safety and Environment (project RT 14/12 FLAREFOOD).

Disclosure statement

No potential conflict of interest was reported by the authors.

Additional information

Funding

This work was supported by the Belgian Federal Public Service (FPS) Health, Food Chain Safety and Environment [project RT 14/12 FLAREFOOD]