title: 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.
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.
authors.affiliation: 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, USA. locontop@michigan.gov
authors.forename: Paul R
authors.initials: PR
authors.lastname: Loconto
authors.forename: David
authors.initials: D
authors.lastname: Isenga
authors.forename: Michael
authors.initials: M
authors.lastname: O'Keefe
authors.forename: Mark
authors.initials: M
authors.lastname: Knottnerus
mesh_terms: D000818:Animals; D005591:Chemical Fractionation / Q000379:methods*; D008401:Gas Chromatography-Mass Spectrometry; D006801:Humans; D010647:Phenyl Ethers / Q000097:blood* / Q000302:isolation & purification*; D011075:Polybrominated Biphenyls / Q000097:blood* / Q000302:isolation & purification*; D015203:Reproducibility of Results; D034561:Sheep, Domestic; D052616:Solid Phase Extraction / Q000379:methods*
chemical_list: D010647:Phenyl Ethers; D011075:Polybrominated Biphenyls; C031538:phenyl ether