Simultaneous Method for Selected PBDEs and HBCDDs in Foodstuffs Using Gas Chromatography-Tandem Mass Spectrometry and Liquid Chromatography-Tandem Mass Spectrometry.

Content Provider	Europe PMC
Author	Lipičar, Eva Fras, Danijela Javernik, Nino Prosen, Helena
Editor	Fernandes, Virgínia Cruz
Copyright Year	2022
Abstract	Flame retardants are added to consumer products to retard the ignition of combustible materials. Technical mixtures of polybrominated diphenyl ethers (PBDEs) and hexabromocyclododecane (HBCDD) were massively used for several decades. They are bioaccumulative, persistent, and have adverse effects on organisms. Recognised as persistent organic pollutants, they are banned almost worldwide. Food is the principal source of human exposure. Yet, no maximum residue limits for food have been established in the EU. Nevertheless, monitoring of specific congeners is recommended. Simultaneous analysis of HBCDDs and PBDEs is rarely encountered, especially including BDE-209, as this thermally unstable congener is particularly challenging for analysis. We have developed a method for the simultaneous determination of all relevant PBDEs and HBCDDs recommended for monitoring by the EU. In the method, single sample preparation is used for different types of foodstuffs, applying ultrasound-assisted extraction, clean-up by gel permeation, and adsorption chromatography. Analyses were performed on the same extract, first by GC-MS/MS(EI) method for PBDEs and followed by LC-MS/MS(ESI) method for HBCDDs. The analytical method was validated on a blank sample of milk formula at 2–3 fortification levels, including recommended LOQ level of 0.01 µg/kg wet weight. Satisfactory accuracy with recoveries 85–119%, intra-day precision (1.5–11.3%), and inter-day precision (4.3–18.4%) was obtained. The method ensures LOQs that are compliant with the EU recommendations for all PBDEs and HBCDDs, including BDE-209. Method applicability was further confirmed on proficiency testing samples of baby food, fish, and citrus.
Journal	Toxics
Volume Number	11
PubMed Central reference number	PMC9862769
Issue Number	1
PubMed reference number	36668741
e-ISSN	23056304
DOI	10.3390/toxics11010015
Language	English
Publisher	MDPI
Publisher Date	2022-12-24
Access Restriction	Open
Rights License	Licensee MDPI, Basel, Switzerland. This article is an open access article distributed under the terms and conditions of the Creative Commons Attribution (CC BY) license (https://creativecommons.org/licenses/by/4.0/). © 2022 by the authors.
Subject Keyword	brominated flame retardants hexabromocyclododecane—HBCDD polybrominated diphenyl ethers—PBDE POPs GC-MS/MS LC-MS/MS ultrasound-assisted extraction clean-up validation
Content Type	Text
Resource Type	Article
Subject	Chemical Health and Safety Health, Toxicology and Mutagenesis Toxicology