Quantitative analysis of polybrominated diphenyl ethers in adipose tissue, human serum and foodstuff samples by gas chromatography with ion trap tandem mass spectrometry and isotope dilution

Abstract

A method based on gas chromatography (GC) separation followed by ion trap tandem mass spectrometry detection in EI mode (ITD-MS/MS), using isotope dilution, was developed for the determination of ten native polybrominated diphenyl ethers (PBDEs) and four (13)C(12)-labeled congeners in biological (fat tissue and human serum) and food samples. The highest-mass fragment ions were used as precursor ions for those congeners with molecular ions with m/z values higher than the maximum of the instrument. In these cases (hepta-BDEs and (13)C(12)-hexa-BDEs) no fragmentation was achieved under the experimental conditions employed. Repeatability (lower than 9%) and reproducibility (lower than 13%), expressed as relative standard deviation (RSD, n = 3 and 4, respectively), were satisfactory. Similarly, the coefficient of variation (n = 4) of the isotopic ratio between the two most abundant product ions was lower than 10 and 6% for native and labeled congeners, respectively. To evaluate the feasibility of the method, the optimized isotope dilution GC/ITD-MS/MS method was used for the quantitation of selected PBDE congeners in different samples including adipose tissue, human serum and foodstuff samples, from three inter-laboratory comparative exercises, covering a wide range of concentrations. A solid-phase extraction procedure, previously developed for PCB determination in small-size bird serum samples, was successfully applied to quantification of PBDEs in 1 mL samples of human serum.

PBDE exposure from food in Ireland: optimising data exploitation in probabilistic exposure modelling

“…To put the Irish dose estimates into perspective, they are compared with doses presented in other studies (Table 5) (Bocio et al, 2003;Harrad et al, 2004;Gomara et al, 2006;UKFSA, 2006b;Voorspoels et al, 2007;Akutsu et al, 2008a;Bakker et al, 2008;Sioen et al, 2008;Schecter et al, 2010). We also present external doses (i.e., before uptake into the body) to make our estimates better comparable with other studies (for detailed results see Supplementary Table S11 and Table S12).…”

Simultaneous determination of polybrominated diphenyl ethers and polychlorinated biphenyls by gas chromatography–tandem mass spectrometry in human serum and plasma

“…When comparing our LODs to methods using ion trap mass spectrometry for analysis of human serum or tissues, for PBDEs and PCBs, our LODs conducted by triple quadruple tandem mass spectrometry were up to 10 times lower than previously reported LODs values ranging from 0.07–1.3 ng/ml for PBDEs [67], and 0.05–0.13 ng/ml for PCBs [68, 69]. …”

Analysis of polybrominated diphenyl ethers in sewage sludge by matrix solid‐phase dispersion and isotope dilution GC–MS

“…PBDEs are chemically and toxicologically similar to another banned family of chemicals known as polychlorinated biphenyls (PCBs). Given their lipophilicity, low vapour pressures, and high octanol -water partition coefficients [3], PBDEs bind well to particles with high organic carbon content of sewage sludge and have a tendency to accumulate [4,5]. Sewage treatment plant effluents are probably a major source of contamination for PBDEs, especially in the receiving water bodies of local aquatic environments surrounding the location of these discharges.…”