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Fish exhibiting external lesions, incidences of intersex, and death have recently been observed in the Shenandoah and James River Basins. These basins are characterized by widespread agriculture (intensive in some areas), several major industrial discharges, numerous sewage treatment plant discharges, and urban, transportation, and residential growth that has increased rapidly in recent years. Nine locations in the Shenandoah River Basin, Virginia, and two in the James River Basin, Virginia, were selected for study in an attempt to identify chemicals that may have contributed to the declining fish health. Two passive sampling devices, semipermeable membrane devices (SPMDs) and polar organic chemical integrative samplers (POCIS), were deployed during the spring and early summer of 2007 to measure select organic contaminants to which fish may have been exposed. This study determined that concentrations of persistent hydrophobic contaminants, such as polycyclic aromatic hydrocarbons (<17,000 picograms per liter), legacy pesticides (<510 picograms per liter), and polychlorinated biphenyls (<1,600 picograms per liter) were generally low and indicative of a largely agricultural area. Chlorpyrifos, endosulfan, and lindane were the most commonly detected chlorinated pesticides. Atrazine, which was detected at concentrations much greater than other pesticides associated with agricultural use, ranged from <0.18 to 430 nanograms per liter during the deployment period. Few chemicals characteristic of wastewater treatment plant effluent or septic tank discharges were detected. The fragrance components, galaxolide, indole, and tonalide, were the predominant waste indicator chemicals detected. Caffeine, the caffeine metabolite 1,7-dimethylxanthine, the nicotine metabolite cotinine, and the prescription pharmaceuticals carbamazepine, venlafaxine, and trimethoprim were detected at several sites. Natural and synthetic hormones were detected at a few sites with 17α-ethynylestradiol concentrations estimated up to 8.1 nanograms per liter. Screening of the POCIS extracts for estrogenic chemicals by using the yeast estrogen screen revealed estrogenicity similar to levels reported for rural areas with minor effect from wastewater effluents. Introduction Anthropogenic pollution is recognized as a global problem contributing to degradation of ecosystem quality, loss of numerous plant and animal species, and potential adverse effects on human health. Sources of these environmental stressors include point and nonpoint inputs of a broad spectrum of agricultural, industrial, and residential related chemicals. Increasingly, environmental scientists are acknowledging that in addition to contaminants of historic concern, emerging contaminants, including pharmaceuticals, new generation pesticides, personal care products, and natural and synthetic hormones, are potential sources of adverse effects. Fish kills have been increasing in regularity in the Shenandoah River and Potomac River Basins in Virginia (Blazer and others, 2007). These observations were made primarily during the spring, and mostly in smallmouth bass (Micropterus dolomieu), red-breast sunfish (Lepomis auritus), and various species of suckers. The cause(s) of these phenomena are unknown; however, the input of anthropogenic organic chemicals into the basin may be a factor. A sampling approach that provides a time weighted average assessment is critical in understanding the consequences of exposure to these diverse mixtures of chemicals. The SPMD and the POCIS are two commonly used passive sampling technologies that provide a Reconnaissance of Persistent and Emerging Contaminants in the Shenandoah and James River Basins, Virginia, During Spring of 2007 By David Alvarez1, Walter Cranor1, Stephanie Perkins1, Vickie Schroeder2, Stephen Werner3, Edward Furlong3, Donald Kain4, and Robert Brent4 1 U.S. Geological Survey, Columbia Environmental Research Center, 4200 New Haven Road, Columbia, Missouri 65201. 2 Arctic Slope Regional Corporation (ASRC), 4200 New Haven Road, Columbia, Missouri 65201. 3 U.S. Geological Survey, National Water Quality Laboratory, Denver, Colorado 80225. 4 Virginia Department of Environmental Quality, Valley Regional Office, Harrisonburg, Virginia 22801. 2 Persistent and Emerging Contaminants in the Shenandoah and James River Basins, Virginia, Spring of 2007 means of integratively sampling a wide array of bioavailable waterborne nonpolar and polar organic contaminants. Passive samplers are deployed for weeks to months, extract chemicals continuously from the water, and sample only dissolved chemicals, excluding chemicals associated with particulate, suspended sediment, or colloidal matter. During a typical one-month exposure, a passive sampler potentially can sample tens to hundreds of liters (L) of water, allowing for the detection of chemicals at low concentrations, or those that are present episodically. This time integration of contaminants is not readily achievable using standard sampling methods that collect discrete 1or 2-L water samples. The SPMD consists of a layflat low-density polyethylene membrane tube containing a neutral lipid (triolein). The SPMD is designed to mimic key aspects of the bioconcentration process that results in elevated contaminant concentrations in organism tissues after exposure to trace hydrophobic organic contaminants in aquatic environments (Huckins and others, 2006). Sampling of compounds with moderate to high (greater than 3) octanol to water partition coefficients (Kows) is integrative, meaning extracted residues are constantly accumulated without significant losses back into the environment. As such, chemcial concentrations are reported as time weighted average values. Like SPMDs, the POCIS is designed to mimic key aspects of the bioconcentration process and exposure of an organism to hydrophilic organic contaminants. The POCIS consists of a solid phase sorbent or mixture of sorbents contained between two sheets of a microporous polyethersulfone membrane (Alvarez and others, 2004, 2007). Sampling of compounds with low to moderate (less than 3) Kows is integrative and chemical concentrations are reported as time weighted average values. The U.S. Geological Survey (USGS) in cooperation with the Virginia Department of Environmental Quality (VADEQ), conducted this study to identify anthropogenic organic chemicals and assess the estrogenicity of the complex mixtures of chemicals by using an in vitro assay. Passive samplers were used to detect potentially endocrine disrupting compounds and other chemicals at 10 locations on various rivers and streams within the Shenandoah and James River Basins. SPMDs and POCIS were deployed between March and May 2007 to address the potential effect of agricultural and municipal inputs into the basin during the months when fish kills have been most prevalent. A suite of anthropogenic organic contaminants was selected for study, including polycyclic aromatic hydrocarbons (PAHs), legacy organochlorine pesticides (OCs), polychlorinated biphenyls (total PCBs), select natural and synthetic hormones, current-use agricultural pesticides, pharmaceuticals, and waste indicator contaminants. Methodology Passive Sampler Construction The passive samplers used in this study were purchased from Environmental Sampling Technologies (EST Labs, St. Joseph, Missouri). For each site, six POCIS and three SPMDs were used. The POCIS used in this study contained Oasis HLB as the chemical sequestration medium enclosed between two polyethersulfone membranes. Oasis HLB is a functionalized polystyrene-divinylbenzene polymer with blended hydrophilic-lipophilic properties, commonly used in environmental monitoring studies for a range of organic contaminants (Kolpin and others, 2002; Cahill and others, 2004; Tran and others, 2007). Each POCIS unit had an effective sampling surface area of 41 square centimeters and a membrane surface area to sorbent mass ratio of 180 square centimeters per gram conforming to the specification of a standard POCIS (Alvarez and others, 2004). Each SPMD consisted of a 97 centimeter (cm) long (86 cm between the lipid-containment seals) by 2.5 cm wide layflat low-density polyethylene tubing containing 1.0 milliliter (mL) of purified triolein (Lebo and others, 2004). The membrane surface area to total SPMD volume ratio of SPMDs used in this study was 86 square centimeters per mL (cm2/mL), and triolein represented 20 percent of the mass of the SPMDs conforming to a “standard SPMD” as defined by Huckins and others (2006). Two of the three SPMDs used at each site were fortified with about 21 to 24 nanograms (ng) of each of the three PCB congeners 14, 29, and 50 which were selected as performance reference compounds (PRCs). A description of the PRC approach is given in the Estimation of Ambient Water Concentrations section. In addition to the field deployed SPMDs, two freshly prepared SPMDs were fortified with the PRC mixture and were used as a measure of the initial concentration for the PRC modeling. Sampling Sites and Field Deployment Eleven sites were selected by members of VADEQ. These sites included eight fish kill sites in the Shenandoah River Basin, one “control” site in the Shenandoah River Basin, and two “control” sites in the James River Basin. The control sites were streams with similar characteristics, including fish communities, which had not experienced fish kills in previous years. However, during the 2007 passive sampler sampling, a few dead fish were found at the Cedar Creek control site and a substantial fish kill was observed at the Cowpasture

Reconnaissance of persistent and emerging contaminants in the Shenandoah and James River Basins, Virginia, during Spring of 2007