Simultaneous determination of polybrominated diphenyl ethers and polychlorinated biphenyls by gas chromatography–tandem mass spectrometry in human serum and plasma

Abstract

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 congeners. 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 3–145 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.

Association of Polybrominated Diphenyl Ethers (PBDEs) and Polychlorinated Biphenyls (PCBs) with Hyperthyroidism in Domestic Felines, Sentinels for Thyroid Hormone Disruption

“…The detailed description for sample preparation and GC-MS/MS parameters was reported elsewhere [29]. Calibration curves were weighted 1/x.…”

Association of serum concentrations of persistent organic pollutants (POPs) and risk of pre-eclampsia: a case–control study

“…The analytical procedure details for PBDEs and PCBs were described elsewhere [36]. Briefly, the samples were fortified with Hexachlorobenzene (internal standard) and then mixed with 0.5 ml of pure formic acid and ultrasonicated for 10 min.…”

Quantification of Polychlorinated Biphenyls and Polybrominated Diphenyl Ethers in Commercial Cows’ Milk from California by Gas Chromatography–Triple Quadruple Mass Spectrometry

“…Two μ L of extract were injected by pulsed splitless mode (split ratio of 50:1, 50 psi, 0.2 min) at 250°C. The individual PCB and PBDE analytes were quantified using the sum of two multiple reactions monitoring (MRM) transitions and characterized by their abundance ratios [45]. …”