Semiautomated high-throughput extraction and cleanup method for the measurement of polybrominated diphenyl ethers, polybrominated biphenyls, and polychlorinated biphenyls in human serum.
A semiautomated extraction and cleanup method has been developed for the measurement of eight polybrominated diphenyl ethers (PBDEs), 2,2',4,4',5,5'-hexabromobiphenyl (BB-153) and 2,2',4,4',5,5'-hexachlorobiphenyl (CB-153). The method employs automated addition of internal standards ((13)C-labeled), addition of formic acid (denaturation agent), and dilution with water prior to automated overnight extraction using a modular solid-phase extraction (SPE) system. Removal of coextracted biogenic materials was performed on a two-layered 3-mL disposable cartridge containing activated silica gel and a mixture of silica gel and sulfuric acid. Sample cleanup was automated using the same modular SPE system. Reproducibility and precision of the liquid handler used for internal standard additions were shown to be 2 and 4%, respectively. Overall reproducibility during processing of eight batches of samples (N = 30/batch, including methods blanks) was below 10% for most analytes. Mean recoveries of the (13)C-labeled internal standards ranged from 69 to 95% for the seven monitored PBDEs; 76 and 98% were recovered for BB-153 and CB-153, respectively.
Sjödin
Andreas
A
Organic Analytical Toxicology, Division of Laboratory Sciences, National Center for Environmental Health, Centers for Disease Control and Prevention, 4770 Buford Highway N.E., Mail Stop F-17, Atlanta, GA 30341, USA. asjodin@cdc.gov
Jones
Richard S
RS
Lapeza
Chester R
CR
Focant
Jean-François
JF
McGahee
Ernest E
EE
Patterson
Donald G
DG
D001331:Automation; D004785:Environmental Pollutants / Q000097:blood*; D055768:Halogenated Diphenyl Ethers; D006801:Humans; D006842:Hydrocarbons, Brominated / Q000097:blood*; D013058:Mass Spectrometry / Q000379:methods*; D010647:Phenyl Ethers / Q000097:blood*; D011075:Polybrominated Biphenyls / Q000097:blood*; D011078:Polychlorinated Biphenyls / Q000097:blood*; D011786:Quality Control; D012822:Silicon Dioxide / Q000494:pharmacology; D013464:Sulfuric Acids / Q000494:pharmacology
D004785:Environmental Pollutants; D055768:Halogenated Diphenyl Ethers; D006842:Hydrocarbons, Brominated; D010647:Phenyl Ethers; D011075:Polybrominated Biphenyls; D013464:Sulfuric Acids; D012822:Silicon Dioxide; C086401:pentabromodiphenyl ether; D011078:Polychlorinated Biphenyls