TP7 Persistent Organic Pollutants
Tuesday, 15 November 2005: 8:00 AM - 6:30 PM in Exhibit Hall

(SAM-1117-816401) Analysis of Hydroxylated Metabolites of PCBs and PBDEs in Fish using GC/MS and LC/MS.

Samara, F¹, Aga, D¹, ¹ The State University of New York- University at Buffalo, Buffalo, NY, USA

ABSTRACT- Persistent organic pollutants (POPs)are chemical substances that have long half-lives in the environment, bioaccumulate through the food web, and could cause adverse health effects to human and wildlife. Some POPs such as polychlorinated biphenyls (PCBs) and polybrominated diphenyl ethers (PBDEs) are also considered to be endocrine disruptors, which, by altering the hormonal system, can damage the reproductive and immune systems of exposed individuals as well as their offspring. PCBs and PBDEs are ubiquitous in lake and river sediments such that concentrations as high as 1450 ng/g total PCBs and 80.1 ng/g total PBDEs have been reported in fish. Measuring both the parent and the metabolites, which also accumulate in the body, can assess the bioaccumulation of these POPs. This work will focus on the analysis of hydroxylated PCB and PBDE metabolites, which have been detected in fish and marine mammals. These metabolites were extracted using accelerated solvent extraction followed by a clean up step consisting on liquid/liquid extraction with concentrated sulfuric acid and hexane. The hexane layer was further cleaned-up on basic silica (33% KOH) and florisil. Analysis was performed by comparing gas chromatography/ mass spectrometry (GC/MS) after derivatization with trifluoroacetic acid anhydride (TFAA), and ion-trap liquid chromatography/ mass spectrometry (LC/MS) using electrospray ionization under negative ion mode. Both methods achieved comparable instrumental limits of detection of around 0.1 ppb for the hydroxylated metabolites of PCBs and PBDEs in fish. Losses during sample preparation and derivatization were compensated using labeled internal standards of PCBs and deuterated pyrene. The advantage of using LC/MS over GC/MS is that the first one does not require a derivatization step prior to injection.

Key words: Persistent Organic Pollutants, Hydroxylated PCBs, Hydroxylated PBDEs, Fish