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Persistent Organic Pollutant Determination in Killer Whale Scat Samples: Optimization of a Gas Chromatography/Mass Spectrometry Method and Application to Field Samples

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Abstract

Biologic sample collection in wild cetacean populations is challenging. Most information on toxicant levels is obtained from blubber biopsy samples; however, sample collection is invasive and strictly regulated under permit, thus limiting sample numbers. Methods are needed to monitor toxicant levels that increase temporal and repeat sampling of individuals for population health and recovery models. The objective of this study was to optimize measuring trace levels (parts per billion) of persistent organic pollutants (POPs), namely polychlorinated-biphenyls (PCBs), polybrominated-diphenyl-ethers (PBDEs), dichlorodiphenyltrichloroethanes (DDTs), and hexachlorocyclobenzene, in killer whale scat (fecal) samples. Archival scat samples, initially collected, lyophilized, and extracted with 70 % ethanol for hormone analyses, were used to analyze POP concentrations. The residual pellet was extracted and analyzed using gas chromatography coupled with mass spectrometry. Method detection limits ranged from 11 to 125 ng/g dry weight. The described method is suitable for p,p′-DDE, PCBs-138, 153, 180, and 187, and PBDEs-47 and 100; other POPs were below the limit of detection. We applied this method to 126 scat samples collected from Southern Resident killer whales. Scat samples from 22 adult whales also had known POP concentrations in blubber and demonstrated significant correlations (p < 0.01) between matrices across target analytes. Overall, the scat toxicant measures matched previously reported patterns from blubber samples of decreased levels in reproductive-age females and a decreased p,p′-DDE/∑PCB ratio in J-pod. Measuring toxicants in scat samples provides an unprecedented opportunity to noninvasively evaluate contaminant levels in wild cetacean populations; these data have the prospect to provide meaningful information for vital management decisions.

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Acknowledgments

Research funding was provided by the Washington Sea Grant [pursuant to National Oceanic and Atmospheric Administration (NOAA), award no. NA10OAR417005], NOAA’s Northwest Fisheries Science Center (NWFSC), Canadian Consulate General, Center for Conservation Biology, and Northwest Science Association. This publication was developed under STAR Fellowship Assistance Agreement no. 91735201 awarded by the U.S. Environmental Protection Agency (EPA). It has not been formally reviewed by the EPA. The views expressed in this publication are solely those of Jessica Lundin, and the EPA does not endorse any products or commercial services mentioned in this publication. This project was made possible thanks to collaborations at NOAA NWFSC. Special thanks to Mike Ford at NOAA NWFSC for his continued support. Bernadita Anulacion, Daryle Boyd, Jennie Bolton, and Ronald Pearce at NOAA NWFSC conducted the pilot sample analyses on scat samples. The use of select internal standards was provided by the University of Washington Center for Ecogenetics and Environmental Health (P30ES007033). Liz Seely with Conservation Canines was the lead dog handler, and Deborah Giles and Kari Koski were the boat captains on the research vessel.

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Authors and Affiliations

  1. Department of Biology, Center for Conservation Biology, University of Washington, Box 351800, Seattle, WA, USA

    Jessica I. Lundin & Samuel K. Wasser

  2. Department of Environmental and Occupational Health Sciences, University of Washington, Seattle, WA, USA

    Russell L. Dills & Jacqui Ahmad

  3. Northwest Fisheries Science Center, National Marine Fisheries Service, National Oceanic and Atmospheric Administration, Seattle, WA, USA

    Gina M. Ylitalo, M. Bradley Hanson, Candice K. Emmons, Jennifer A. Hempelmann & Kim M. Parsons

  4. Cascadia Research Collective, Olympia, WA, USA

    Gregory S. Schorr

  5. National Marine Mammal Laboratory, Alaska Fisheries Science Center, National Marine Fisheries Service, National Oceanic and Atmospheric Administration, Seattle, WA, USA

    Kim M. Parsons

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  1. Jessica I. Lundin
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Correspondence to Jessica I. Lundin.

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Lundin, J.I., Dills, R.L., Ylitalo, G.M. et al. Persistent Organic Pollutant Determination in Killer Whale Scat Samples: Optimization of a Gas Chromatography/Mass Spectrometry Method and Application to Field Samples. Arch Environ Contam Toxicol 70, 9–19 (2016). https://doi.org/10.1007/s00244-015-0218-8

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