Determination of polybrominated diphenyl ethers and polychlorinated biphenyls in human adipose tissue by large-volume injection-narrow-bore capillary gas chromatography/electron impact low-resolution mass spectrometry.
A new analytical method has been developed for the quantification of polybrominated diphenyl ethers (PBDEs) in human adipose tissue samples. After Soxhlet extraction and a cleanup procedure using two successive solid-phase extraction cartridges containing acid silica and acid silica: neutral silica:deactivated basic alumina (from top to bottom), detection can been achieved by narrow-bore (0.10-mm i.d.) capillary gas chromatography/electron impact low-resolution mass spectrometry using a large-volume injection technique. Using narrow-bore capillaries, it is possible to analyze complex mixtures in a short time (up to 10 min), saving 50% or more of the analysis time of conventional columns while maintaining a similar resolution power. The method allows the determination of five major PBDE congeners (BDE 28, 47, 99, 100, and 153) at concentrations below 1 ng/g lipid weight. Detection limits in the selected ion mode varied between 0.05 and 0.30 ng/g lipid weight, depending on the degree of bromination. The sensitivity of this method can compete with low-resolution mass spectrometry with electron capture ionization, while a much better selectivity is obtained. Levels of PBDEs in 20 Belgian human adipose tissue samples ranged between 2.18 and 11.70 ng/g lipid weight and were similar to previously reported values from Europe.
Covaci
Adrian
A
Toxicological Center, University of Antwerp, Wilnijk, Belgium. covaci@uia.ua.ac.be
de
Boer Jacob
BJ
Ryan
John Jake
JJ
Voorspoels
Stefan
S
Schepens
Paul
P
D000273:Adipose Tissue / Q000737:chemistry*; D001713:Biphenyl Compounds / Q000737:chemistry*; D004987:Ethers / Q000737:chemistry*; D008401:Gas Chromatography-Mass Spectrometry; D006801:Humans; D011078:Polychlorinated Biphenyls / Q000032:analysis*; D011786:Quality Control
D001713:Biphenyl Compounds; D004987:Ethers; D011078:Polychlorinated Biphenyls