Abstract
Emerging brominated flame retardants (eBFRs) other than polybrominated diphenyl ethers (PBDEs), polybrominated biphenyls (PBBs) and their derivatives in foods have been in focus in recent years due to their increasing production volumes, indefinite information on toxicities and the lack of data on occurrence in environments, foods as well as humans. In this study, gas chromatography was coupled to an atmospheric pressure chemical ionization-tandem mass spectrometry (APGC-MS/MS) for the analysis of six eBFRs in pork, chicken, egg, milk and fish. A short section of unpacked capillary column coupled to the end of the analytical column was applied to improve the chromatographic behaviors of high boiling point compounds. The method was comprehensively validated with method limit of quantification (mLOQ) lower than 8 pg/g wet weight (w.w.). Samples from Chinese Total Diet study were quantified following the validated APGC-MS/MS method. 2,3,4,5-pentabromo-6-ethylbenzene (PBEB), hexabromobenzene (HBB), pentabromotoluene (PBT) and 1,2-bis(2,4,6-tribromophenoxy)ethane (BTBPE) were most frequently detected in samples. The highest concentration was found in fish with 351.9 pg/g w.w. of PBT. This is the first report on the presence of PBT in food samples with non-ignorable concentrations and detection rate.
Highlights
Gas chromatography coupled to mass spectrometry (GC-MS) using negative chemical ionization (NCI) source has been widely applied in the field of BFRs analysis to obtain higher sensitivity[6,11,16]
The use of APGC-MS/MS has been evaluated as an alternative approach for analyzing Emerging brominated flame retardants (eBFRs) in dietary samples with high sensitivities and low matrix effects
Owing to the soft ionization, the molecular ion was selected as the precursor ion and a multiple reaction monitoring (MRM) method was developed contributing to excellent selectivity and sensitivity
Summary
Gas chromatography coupled to mass spectrometry (GC-MS) using negative chemical ionization (NCI) source has been widely applied in the field of BFRs analysis to obtain higher sensitivity[6,11,16]. This technique has lower selectivity and specificity for eBFRs since only two isotopes of bromine atom (m/z 79 and 81) can be monitored. New attempts using liquid chromatography coupled to orbitrap mass spectrometry (LC-MS/MS) using atmospheric pressure photoionization (APPI) mode have been reported to detect some selected eBFRs (PBEB, HBB, BTBPE and DBHCTD) in fish with instrument limit of quantification (iLOQ) in the range of 0.5–59 pg on-column levels[19,20]. The Chinese Total Dietary Study (TDS) samples were collected for the monitoring occurrence of six selected eBFRs
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