Levels of polychlorinated biphenyls (PCBs) and polybrominated diphenyl ethers (PBDEs) were measured in 53 human adipose tissue samples. The samples consisted of adipose tissue from 31 men and 22 women having a mean age of 53 years. No information about diet or occupational exposure was collected. Cleanup was performed using a glass column containing acidified silica, deactivated alumina, and anhydrous sodium sulphate. Subsequently, samples were analyzed by high-resolution gas chromatography/tandem mass spectrometry. PBDE concentrations (sum of BDEs 28, 47, 99, 100, 154, 153, and 183) ranged between 1.23 and 57.2 ng g(-1) lipid weight and were comparable with levels in samples from other European countries. The sum of seven International Council for the Exploration of the Sea (ICES) indicator PCB congeners (PCBs 28, 52, 101, 118, 138, 153, and 180) ranged from 126 to 2090 ng g(-1) lipid weight. No age dependency was found for PBDEs (Pearson correlation -0.023, p = 0.873), whereas PCBs showed higher correlation coefficients with age (Pearson correlation 0.613, p < 0.0005). There was no relationship between PBDE and PCB levels (Pearson correlation -0.010, p = 0.943).
A combined gas chromatographic mass spectrometric (GC/MS/MS) method for the determination of seven polybrominated diphenyl ethers (PBDEs) and seven marker polychlorinated biphenyls (PCBs) in adipose tissue has been developed. Adipose tissue was melted and filtered through anhydrous sodium sulphate to obtain pure fat. Clean-up was performed using a glass column containing acidified silica, deactivated alumina and anhydrous sodium sulphate. Polybrominated biphenyl (PBB) 155 and Mirex were added as internal standards for PBDEs and PCBs, respectively. Injection standards, PBB 103 and PCB 143, for PBDEs and PCBs, respectively, were added before analysis with GC/MS/MS. The developed GC/MS/MS method has the advantage of being more selective than single MS methods because matrix effects are largely eliminated. Validation of this method was conducted according to Commission Decision 2002/657/EC. Decision limits for PBDEs and PCBs ranged from 0.06-0.15 ng g(-1) and from 0.35-1.22 ng g(-1), respectively. Detection capabilities were all between 0.23-0.55 ng g(-1) for PBDEs and between 0.98-2.29 ng g(-1) for PCBs. Precision, recovery, bias and selectivity were tested, with satisfactory results.
A simplified clean-up procedure was developed in combination with gas chromatography-tandem mass spectrometry (GC-MS/MS) for the determination of polychlorinated biphenyls (PCBs) and polybrominated diphenyl ethers (PBDEs) in adipose tissue. Clean-up was performed by the successive application of a Mega Bond Elut silica column and a Bond Elut PCB column. Validation of the method was conducted according to European Union Commission Decision 2002/657/EC. In order to evaluate the applicability of the method, 44 horse fat samples were analysed. The total PCB concentration (sum of PCBs 28, 52, 101, 118, 138, 153 and 180) ranged from 5.35 to 140 ng g(-1) lipid weight. The total PBDE concentration (sum of BDEs 28, 47, 99, 100, 153, 154 and 183) ranged from below the decision limit to 6.34 ng g(-1) lipid weight.
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