Published:Journal of Chromatographic Science, ISSN 0021-9665 Volume 46, Number 1, January 2008, pp. 53-60

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

Paul R. Loconto, David Isenga, Michael O’Keefe, and Mark Knottnerus
Division of Chemistry and Toxicology, Bureau of Laboratories, Michigan Department of Community Health, 3350 North Martin Luther King Jr. Blvd. P.O. 30035 Lansing, MI 48909

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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