High-throughput analytical methods for persistent organic pollutants in high-lipid matrices.
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Robinson, Eleanor Marian.
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Persistent organic pollutant (POP) trends and profiles reconstructed from environmental matrices, such as mammal tissues, have provided a wealth of information regarding contaminant behavior and environmental fate. These POP trends and profiles are unique and often irreplaceable due to difficulties in obtaining marine mammal samples. Historically, sample preparation methods for lipid-rich marine mammal matrices require an extraction followed by multiple cleanup and concentration steps. Due to the volatility of select POPs, during sample preparation steps (traditional packed column and GPC cleanup steps followed by a concentration step via nitrogen) there are possibilities for analyte loss and contamination. The goal of sample preparation methods for POPs should seek to reduce the overall number of steps. Selective pressurized liquid extractions (SPLE; an analytical technique that combines PLE with sorbent cleanup) has reduced and/or eliminated the number of cleanup steps associated with organic pollutants extraction and cleanup. SPLE methods for lipid-rich matrices were developed and improved for the trace analysis of multiple classes of organic pollutants (organochlorine pesticides, polychlorinated biphenyls, and polybrominated diphenyl ethers). Analytical methods for lipid-rich matrices, such as marine mammal blubber (Weddell seal Leptonychotes weddelli and bowhead whale blubber Balaena mysticetus) and whale earwax (blue whale Balaenoptera musculus), were developed and emphasized improvements on sample preparation for the analysis of organic pollutants. Marine mammal blubber methods utilizing SPLE followed by GPC were developed (Chapter II; Weddell seal blubber tissue), and improved to eliminate all post-extraction (i.e. GPC) cleanup steps (Chapter III; bowhead whale blubber tissue). An SPLE method for whale earwax with no post-extraction cleanup was also developed (Chapter IV). These methods were applied to environmental samples and utilized to generate irreplaceable data including the first identification of PBDEs in Antarctica’s Weddell seals (Chapter II) as well as in Arctic bowhead whales (Chapter III), and the first identification (Chapter IV) and reconstruction (Chapter V) of contaminant profiles in whale earplugs.