UPLC-MS/MS method for the quantification of HBCDDs and TBBPA with a focus on reliable detection of trace amounts in food

Abstract

Brominated flame retardants (BFR) are a broad class of substances with great economic importance. They can accumulate in the environment and become persistent organic pollutants (POPs). Two major substance classes are the 1,2,5,6,9,10-hexabromocyclododecanes (HBCDDs) and tetrabromobisphenol A (TBBPA). Because of their known toxicity and potential accumulation in the food chain, their detection in food is crucial. A sensitive method was developed and successfully validated to quantify the three most pertinent HBCDD isomers, α-, β- and γ-HBCDD and TBBPA in a wide variety of food matrices, including fish, meat, oil and insect powder. As an improvement to the methods described in the Guidance Document on the Determination of Organobromine Contaminants of the European Union Reference Laboratory (EURL) POPs our method is a time- and cost-saving alternative fulfilling all relevant parameters required for official food control by using commercially available laboratory equipment. The powdered sample is extracted without further clean-up on a sulfuric silica gel column and analysed via ultra-performance liquid chromatography (UPLC) coupled to tandem mass spectrometry (MS/MS). The method performance was demonstrated for the matrices insect flour, fish and olive oil with focus on the parameters linearity (0.1 to 10.0 ng mL⁻¹ for HBCDDs and 1 to 50 ng mL⁻¹ for TBBPA), trueness (89.7–118.6%), repeatability (1.59–9.46%), recovery of deuterated standard (63.8–105.6% for HBCDDs), limit of detection (≤ 0.005 µg/kg for HBCDDs and ≤ 0.046 µg/kg for TBBPA) and limit of quantification (≤ 0.016 µg/kg for HBCDDs and ≤ 0.147 µg/kg for TBBPA). The method was successfully applied in proficiency tests organised by the EURL POPs on the determination of HBCDDs and TBBPA in various food matrices.