Simultaneous determination of polybrominated diphenyl ethers and polychlorinated biphenyls by gas...

Sensitive and reliable methods for simultaneous determination of polybrominated diphenyl ethers (PBDEs) and polychlorinated biphenyls (PCBs) in limited volumes of human serum or plasma need to be further documented especially when they accumulate at low levels that are still capable of disrupting endocrine and immune functions, and affecting neurodevelopment and reproduction. The objective of this study was to develop and validate a sensitive and quantitative method that simultaneously quantifies PBDEs and PCBs in 0.5 ml of human serum or plasma. We optimized a solid-phase extraction (SPE) method and used silica particle purification for the extraction of PBDEs and PCBs. Two multiple reactions monitoring (MRM) transitions were optimized for each congener. The sum of the transitions was used for quantification, and their abundance ratios were used for identification. The combined method optimization techniques resulted in limits of detection from 3 to 145 pg/ml for 10 PBDEs and 1-12 pg/ml for 15 PCBs. Method was solidly validated by analyzing serum fortified with a certified PBDE and PCB standard mixture from the National Institute of Standards and Technology (NIST). The accuracy was 88-118% and day-to-day precision was within 19%. The method was successfully applied to quantify native concentrations of PBDE and PCB in commercially available human serum. The sensitivity and selectivity of the GC/EI-MS/MS analysis enables it to be the method of choice for investigations of exposures to PBDE and PCB congeners, especially when sample volume is limited.