PMID:18218189

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Citation

Loconto, PR, Isenga, D, O'Keefe, M and Knottnerus, M (2008) Isolation and recovery of selected polybrominated diphenyl ethers from human serum and sheep serum: coupling reversed-phase solid-phase disk extraction and liquid-liquid extraction techniques with a capillary gas chromatographic electron capture negative ion mass spectrometric determinative technique. J Chromatogr Sci 46:53-60

Abstract

Polybrominated diphenyl ethers (PBDEs) are isolated and recovered with acceptable percent recoveries from human serum via liquid-liquid extraction and column chromatographic cleanup and fractionation with quantitation using capillary gas chromatography-mass spectrometry with electron capture negative ion and selected ion monitoring. PBDEs are found in unspiked serum. An alternative sample preparation approach is developed using sheep serum that utilizes a formic acid pre-treatment followed by reversed-phase solid-phase disk extraction and normal-phase solid-phase cleanup using acidified silica gel that yields>50% recoveries. When these percent recoveries are combined with a minimized phase ratio for human serum and very low instrument detection limits, method detection limits below 500 parts-per-trillion are realized.

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Keywords

Animals; Chemical Fractionation/methods; Gas Chromatography-Mass Spectrometry; Humans; Phenyl Ethers/blood; Phenyl Ethers/isolation & purification; Polybrominated Biphenyls/blood; Polybrominated Biphenyls/isolation & purification; Reproducibility of Results; Sheep, Domestic; Solid Phase Extraction/methods

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