Background The emissions of brominated flame retardants have been proved to be the major source of polybrominated dibenzo-p-dioxin/furans (PBDD/Fs). With the extensive use of brominated flame retardants in recent decades, the concentrations of PBDD/Fs in the environment increase gradually.
Objective This study aims to establish a rapid and accurate method for the determination of 13 PBDD/F congeners in human milk by gas chromatography-high resolution mass spectrometry (GC-HRMS).
Methods Lyophilized human milk was subject to accelerated solvent extraction, dispersive solid phase extraction (SPE) defatting, and tandem SPE purification successively, and consequently detected by GC-HRMS with isotopic dilution method.
Results This method showed low limits of detection (LOD, 0.002-0.012 ng/g, in 50 g milk sample), good linearity (correlation coefficients, R2 > 0.99), satisfactory accuracy (the recovery rates of lowconcentration spiked standard were 71.8%-101.8%, and the recovery rates of high-concentration spiked standard were 80.5%-97.8%), and high precision (relative standard deviations, RSD < 10%). Forty breast milk samples collected in Shanghai were determined by the method. PBDDs were not detected, and three PBDF congeners including 2, 3, 7, 8-tetrabromodibenzofuran (2, 3, 7, 8-TetraBDF), 1, 2, 3, 4, 6, 7, 8-heptabromodibenzofuran (1, 2, 3, 4, 6, 7, 8-HpBDF), and octabromodibenzofuran (OBDF) were positive, with detection rates of 72.5%, 100%, and 67.5%, respectively.
Conclusion This method has exhibited rapidness, accuracy, efficiency, and reliability for the determination of PBDD/Fs in human milk samples. It provides methodological support for PBDD/Fs exposure risk assessment and toxicological research.
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