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USGS2005

Disparate effects of constant and annually-cycling daylength and water temperature on reproductive maturation of striped bass (Morone saxatilis)

Adult striped bass ( Morone saxatilis ) were exposed to various combinations of constant or anually-cycling daylength and water temperature. Constant conditions (15 h days, 18 °C) were those normally experienced at spawning and cycling conditions simulated natural changes at Chesapeake Bay latitude. Females exposed to constant long (15 h) days and cycling water temperature (TEMPERATURE group) had blood plasma levels of sex steroids (testosterone [T] and estradiol-17β [E 2 ]) and vitellogenin (Vg), and profiles of oocyte growth, that were nearly identical to those of females held under a natural photothermal cycle (CONTROL group). Several fish from these two groups were induced to spawn fertile eggs. Females constantly exposed to warm water (18 °C), with or without a natural photoperiod cycle (PHOTOPERIOD and STATIC groups, respectively), had diminished circulating levels of gonadal steroid hormones and Vg, impaired deposition of yolk granules in their ooplasm, and decreased oocyte growth, and they underwent premature ovarian atresia. Males exposed to cycling water temperature (CONTROL and TEMPERATURE groups) spermiated synchronously during the natural breeding season, at which time they also had had high plasma androgen (T and 11-ketotestosterone [11-KT]) levels. The timing of spermiation was highly asynchronous among males in groups of fish held constantly at 18 °C (STATIC and PHOTOPERIOD groups) and this asynchrony was associated with diminished plasma androgen levels. Termination of spermiation by males exposed to cycling water temperature coincided with a sharp decline in levels of plasma androgens about a month after water temperature rose above 18 °C. In contrast, most males held constantly at 18 °C sustained intermediate levels of plasma androgens and spermiated until the end of the study in late July. The annual cycle of water temperature clearly plays a prominent role in the initiation, maintenance, and termination of the striped bass reproductive cycle. In females, a decrease in water temperature below values experienced at spawning appears to be required for vitellogenesis and oocyte growth to proceed normally. Constant exposure of males to spawning temperature disrupts synchronous spermiation but also delays testicular regression, which may be useful for spawning fish after the natural reproductive season.

Aquaculture↗

USGS2016

Comparison of wastewater-associated contaminants in the bed sediment of Hempstead Bay, New York, before and after Hurricane Sandy

Changes in bed sediment chemistry of Hempstead Bay (HB) have been evaluated in the wake of Hurricane Sandy, which resulted in the release of billions of liters of poorly-treated sewage into tributaries and channels throughout the bay. Surficial grab samples (top 5 cm) collected before and (or) after Hurricane Sandy from sixteen sites in HB were analyzed for 74 wastewater tracers and steroid hormones, and total organic carbon. Data from pre- and post-storm comparisons of the most frequently detected wastewater tracers and ratios of steroid hormone and of polycyclic aromatic hydrocarbon concentrations indicate an increased sewage signal near outfalls and downstream of where raw sewage was discharged. Median concentration of wastewater tracers decreased after the storm at sites further from outfalls. Overall, changes in sediment quality probably resulted from a combination of additional sewage inputs, sediment redistribution, and stormwater runoff in the days to weeks following Hurricane Sandy.

New York↗

USGS2020

Comparability and reproducibility of biomarker ratio values measured by GC-QQQ-MS

The Norwegian Geochemical Standard North Sea Oil-1 was analyzed by gas chromatography triple quadrupole mass spectrometry (GC-QQQ-MS) on two instruments using independently developed analytical methods. Biomarker ratios determined by GC-QQQ-MS were compared to each other and to previously reported values determined by gas chromatography single quadrupole mass spectrometry (GC-Q-MS) or flame ionization detection (GC-FID). Hopane, sterane, and tricyclic ratio values determined by GC-QQQ-MS in multiple reaction monitoring (MRM) mode are comparable to each other, but their comparability to reported values measured by GC-Q-MS in selected ion monitoring (SIM) mode depends in part on whether the compounds in the ratio have similar or dissimilar mass spectral responses. For example, sterane and hopane stereoisomer thermal maturity ratios measured by GC-QQQ-MS in MRM mode agree with previously reported GC-Q-MS SIM values, but an offset is observed for ratios of rearranged hopanes or steranes to their non-rearranged counterparts. Triaromatic steroid, monoaromatic steroid, phenanthrene, and methylphenanthrene ratios measured by GC-QQQ-MS are comparable to each other and to reported GC-Q-MS SIM values. The carbon preference index is comparable across GC-QQQ-MS measurements and reported GC-FID values, while comparability is more variable for other ratios based on pristane, phytane, and/or n -alkanes. Comparability of variably acquired biomarker data could be enhanced in the future by developing instrument- and ratio-specific correction factors or by modifying GC-QQQ-MS parameters and MRM transitions to more closely reproduce previously reported values.

Organic Geochemistry↗

USGS2020

Oil-source rock correlation studies in the unconventional Upper Cretaceous Tuscaloosa marine shale (TMS) petroleum system, Mississippi and Louisiana, USA

The U.S. Geological Survey assessed undiscovered unconventional hydrocarbon resources reservoired in the Upper Cretaceous Tuscaloosa marine shale (TMS) of southern Mississippi and adjacent Louisiana in 2018. As part of the assessment, oil-source rock correlations were examined in the TMS play area where operators produce light (38–45° API), sweet oil from horizontal, hydraulically-fractured wells in an overpressured ‘high-resistivity’ (>5 Ω-m) zone at the base of the TMS. Geochemical data from 39 oil samples and 17 source rock solvent extracts collected from the TMS play area indicate close correspondence for Tuscaloosa Group oils [from lower Tuscaloosa, middle Tuscaloosa (the TMS) and upper Tuscaloosa reservoirs] in thermal maturity (computed from MPI), SARA proportions, n- alkane distributions, isoprenoid and DBT/P ratios, monoaromatic steroids, and δ 13 C isotopic compositions (from whole oils, saturate and aromatic fractions). Other parameters (normal steranes, extended homohopanes, C 31 R/C 30 hopane, norhopane/hopane and tricyclic terpane ratios, gammacerane/hopane) show most oil samples have similar values, suggesting all Tuscaloosa Group oils are from a common mixed marine-terrigenous source rock. Tighter distributions for triaromatic steroid (TAS) and δ 13 C isotopic composition for conventional oils in lower and upper Tuscaloosa reservoirs may indicate charge occurred in a single or shorter pulse relative to TMS oils which show broader TAS and δ 13 C properties, possibly from their generation over an extended period of burial maturation. Dissimilarity in geochemical properties between lower Tuscaloosa source rock solvent extracts and Tuscaloosa Group oils indicates lower Tuscaloosa source rocks did not contribute significantly to conventional and unconventional Tuscaloosa Group hydrocarbon accumulations. Whereas, TMS solvent extracts are similar to Tuscaloosa Group oils, suggesting an oil-source rock correlation. Excluding the possibility for long-distance lateral migration from a similar source downdip (which is unnecessary given thermal maturity considerations), the observations indicate 1. the TMS is a self-sourced reservoir, 2. the TMS is the source of oils accumulated in nearby conventional Tuscaloosa Group reservoirs, and 3. thin organic-rich shales in the lower Tuscaloosa did not contribute substantially to any oil accumulations in the Tuscaloosa Group.

Louisiana, Mississippi↗

USGS2011

Effects of biologically-active chemical mixtures on fish in a wastewater-impacted urban stream

Stream flow in urban aquatic ecosystems often is maintained by water-reclamation plant (WRP) effluents that contain mixtures of natural and anthropogenic chemicals that persist through the treatment processes. In effluent-impactedstreams, aquatic organisms such as fish are continuously exposed to biologically-activechemicals throughout their life cycles. The North Shore Channel of the Chicago River (Chicago, Illinois) is part of an urban ecosystem in which > 80% of the annual flow consists of effluent from the North Side WRP. In this study, multiple samplings of the effluent and stream water were conducted and fish (largemouth bass and carp) were collected on 2 occasions from the North Shore Channel. Fish also were collected once from the Outer Chicago Harbor in Lake Michigan, a reference site not impacted by WRP discharges. Over 100 organic chemicals with differing behaviors and biological effects were measured, and 23 compounds were detected in all of the water samples analyzed. The most frequently detected and highest concentration (> 100 μg/L) compounds were ethylenediaminetetraacetic acid and 4-nonylphenolmono-to-tetraethoxycarboxylic acids. Other biologically-activechemicals including bisphenol A, 4-nonylphenol, 4-nonylphenolmono-to-tetraethoxylates, 4- tert -octylphenol, and 4- tert -octylphenolmono-to-tetraethoxylates were detected at lower concentrations (< 5 μg/L). The biogenic steroidal hormones 17β-estradiol, estrone, testosterone, 4-androstene-3,17-dione, and cis -androsterone were detected at even lower concentrations (< 0.005 μg/L). There were slight differences in concentrations between the North Side WRP effluent and the North Shore Channel, indicating minimal in-stream attenuation. Fish populations are continuously exposed to mixtures of biologically-activechemicals because of the relative persistency of the chemicals with respect to stream hydraulic residence time, and the lack of a fresh water source for dilution. The majority of male fish exhibited vitellogenin induction, a physiological response consistent with exposure to estrogenic compounds. Tissue-level signs of reproductive disruption, such as ovatestis, were not observed.

Illinois↗

USGS2020

De facto water reuse: Bioassay suite approach delivers depth and breadth in endocrine active compound detection

Although endocrine disrupting compounds (EDCs) have been detected in wastewater and surface waters worldwide using a variety of in vitro effects-based screening tools, e.g. bioassays, few have examined potential attenuation of environmental contaminants by both natural (sorption, degradation, etc) and anthropogenic (water treatment practices) processes. This study used several bioassays and quantitative chemical analyses to assess residence-time weighted samples at six sites along a river in the northeastern United States beginning upstream of a waste water treatment plant (WWTP) outfall and proceeding downstream along the stream reach to a drinking water treatment plant (DWTP). Known steroidal estrogens were quantified and changes in signaling pathway molecular initiating events (activation of estrogen, androgen, glucocorticoid, peroxisome proliferator-activated, pregnane X receptor, and aryl hydrocarbon receptor signaling networks) were identified in water extracts. In initial multi-endpoint assays geographic and receptor-specific endocrine activity patterns in transcription factor signatures and nuclear receptor activation were discovered. In subsequent single endpoint receptor-specific bioassays, estrogen (16 of 18 samples; 0.01 to 28 ng estradiol equivalents [E2Eqs]/L) glucocorticoid (3 of 18 samples; 1.8 to 21 ng dexamethasone equivalents [DexEqs]/L), and androgen (2 of 18 samples; 0.95 to 2.1 ng dihydrotestosterone equivalents [DHTEqs]/L) receptor transcriptional activation occurred above respective assay method detection limits (0.04 ng E2Eqs/L, 1.2 ng DexEqs/L, and 0.77 ng DHTEqs/L) in multiple sampling events. Estrogen activity, the most often detected, correlated well with measured concentrations of known steroidal estrogens (R2 = 0.890). Overall, activity indicative of multiple types of endocrine active compounds was highest in wastewater effluent samples, while activity downstream was progressively lower, and negligible in (unfinished) treated water. This multiple bioassay approach, in conjunction with targeted analytical chemistry methods, has gained acceptance among water quality screening programs. Not only was estrogenic and glucocorticoid activity confirmed in the effluent by utilizing multiple methods concurrently, but other activated signaling networks that historically received less attention (i.e. peroxisome proliferator-activated receptor) were also detected.

Science of the Total Environment↗

USGS1997

The effect of diet on dorsal fin erosion in steelhead trout (Oncorhynchus mykiss)

A 2 × 2 factorial experiment of diet type (krill vs. fish meal) and steroid supplementation (0 vs. 30 μg 17α-methyltestosterone kg − ) was conducted to determine the effects on dorsal fin erosion in steelhead trout. Triplicate tanks of 250 fry were fed one of the four diets at a rate calculated to produce 115 g fish in 34 weeks. Fish were transferred to larger tanks when mean density index reached 0.40. Dorsal fin index (DFI, measured as mean dorsal fin height × 100/total fish length) was greater ( P < 0.001) among fish fed krill-based diets than for fish fed fish-based diets at weeks 12, 22, and 34 of the trial. Added testosterone decreased ( P = 0.04) DPI among fish fed the krill diet at week 12 but otherwise had no effect on fin condition. Addition of testosterone to either diet type decreased ( P = 0.02) critical thermal maximum, which is a measure of fish resistance to thermal stress. The results suggest that diet composition can influence the rate of dorsal fin erosion in steelhead trout through a metabolic, behavioral, or combined change.

Aquaculture↗

USGS2002

Pharmaceuticals, hormones, and other organic wastewater contaminants in U.S. streams, 1999-2000: A national reconnaissance

To provide the first nationwide reconnaissance of the occurrence of pharmaceuticals, hormones, and other organic wastewater contaminants (OWCs) in water resources, the U.S. Geological Survey used five newly developed analytical methods to measure concentrations of 95 OWCs in water samples from a network of 139 streams across 30 states during 1999 and 2000. The selection of sampling sites was biased toward streams susceptible to contamination (i.e. downstream of intense urbanization and livestock production). OWCs were prevalent during this study, being found in 80% of the streams sampled. The compounds detected represent a wide range of residential, industrial, and agricultural origins and uses with 82 of the 95 OWCs being found during this study. The most frequently detected compounds were coprostanol (fecal steroid), cholesterol (plant and animal steroid), N , N -diethyltoluamide (insect repellant), caffeine (stimulant), triclosan (antimicrobial disinfectant), tri(2-chloroethyl)phosphate (fire retardant), and 4-nonylphenol (nonionic detergent metabolite). Measured concentrations for this study were generally low and rarely exceeded drinking-water guidelines, drinking-water health advisories, or aquatic-life criteria. Many compounds, however, do not have such guidelines established. The detection of multiple OWCs was common for this study, with a median of seven and as many as 38 OWCs being found in a given water sample. Little is known about the potential interactive effects (such as synergistic or antagonistic toxicity) that may occur from complex mixtures of OWCs in the environment. In addition, results of this study demonstrate the importance of obtaining data on metabolites to fully understand not only the fate and transport of OWCs in the hydrologic system but also their ultimate overall effect on human health and the environment.

Environmental Science & Technology↗

USGS2014

Contaminants of emerging concern in fresh leachate from landfills in the conterminous United States

To better understand the composition of contaminants of emerging concern (CECs) in landfill leachate, fresh leachate from 19 landfills was sampled across the United States during 2011. The sampled network included 12 municipal and 7 private landfills with varying landfill waste compositions, geographic and climatic settings, ages of waste, waste loads, and leachate production. A total of 129 out of 202 CECs were detected during this study, including 62 prescription pharmaceuticals, 23 industrial chemicals, 18 nonprescription pharmaceuticals, 16 household chemicals, 6 steroid hormones, and 4 plant/animal sterols. CECs were detected in every leachate sample, with the total number of detected CECs in samples ranging from 6 to 82 (median = 31). Bisphenol A (BPA), cotinine, and N , N -diethyltoluamide (DEET) were the most frequently detected CECs, being found in 95% of the leachate samples, followed by lidocaine (89%) and camphor (84%). Other frequently detected CECs included benzophenone, naphthalene, and amphetamine, each detected in 79% of the leachate samples. CEC concentrations spanned six orders of magnitude, ranging from ng L −1 to mg L −1 . Industrial and household chemicals were measured in the greatest concentrations, composing more than 82% of the total measured CEC concentrations. Maximum concentrations for three household and industrial chemicals, para -cresol (7 020 000 ng L −1 ), BPA (6 380 000 ng L −1 ), and phenol (1 550 000 ng L −1 ), were the largest measured, with these CECs composing 70% of the total measured CEC concentrations. Nonprescription pharmaceuticals represented 12%, plant/animal sterols 4%, prescription pharmaceuticals 1%, and steroid hormones <1% of the total measured CEC concentrations. Leachate from landfills in areas receiving greater amounts of precipitation had greater frequencies of CEC detections and concentrations in leachate than landfills receiving less precipitation.

Environmental Science: Processes and Impacts↗

USGS2012

Influence of sex and reproductive status on seasonal movement of Lake Sturgeon in Namakan Reservoir, Minnesota–Ontario

We evaluated the influence of sex and reproductive condition on seasonal distribution and movement patterns of Lake Sturgeon Acipenser fulvescens in Namakan Reservoir, Minnesota–Ontario. Blood samples were collected from 133 Lake Sturgeon prior to spawning and plasma concentrations of testosterone and estradiol-17ß were analyzed using radioimmunoassay. Steroid concentrations were used to determine sex and the reproductive stage of each sturgeon. A subset of 60 adults were implanted with acoustic transmitters prior to spawning in 2007 and 2008. Movement was monitored using an array of 15 stationary receivers covering U.S. and Canadian waters of Namakan Reservoir and its tributaries. Of the monitored sturgeon, there was no significant difference in the minimum distance traveled between sexes or among seasons. Site residency did not differ between sexes but differed significantly among seasons, and Lake Sturgeon of both sexes had higher residency during winter (mean = 24 d). Five females implanted with transmitters were characterized as presumed reproductive and 14 as nonreproductive based on plasma steroid concentrations. In general, movement patterns (i.e., migration) of presumed reproductive females corresponded positively with availability of spawning habitat in tributaries. Moreover, presumed reproductive females traveled greater distances than nonreproductive females, particularly during prespawn, spawning, and fall time periods. Distance traveled by presumed reproductive females was highest in the fall compared with other seasons and may be linked to increased energy requirements during late oogenesis before spawning in spring. Combining movement data with information on Lake Sturgeon reproductive status and habitat suitability provided a robust approach for understanding their seasonal migration patterns and identifying spawning locations.

Minnesota, Ontario↗

USGS2007

Selection for rapid embryo development correlates with embryo exposure to maternal androgens among passerine birds

Greater offspring predation favors evolution of faster development among species. We hypothesized that greater offspring predation exerts selection on mothers to increase levels of anabolic androgens in egg yolks to achieve faster development. Here, we tested whether (1) concentrations of yolk androgens in passerine species were associated with offspring predation and (2) embryo and nestling development rates were associated with yolk androgen concentrations. We examined three androgens that increase in potency along the synthesis pathway: androstenedione (A4) to testosterone (T) to 5??- dihydrotestosterone (5??-DHT). Concentrations of none of these steroids were related to clutch size; only A4 was allometrically related to egg volume. Species that experience greater predation showed higher yolk concentrations of T and 5??-DHT. Higher concentrations of T and particularly 5??-DHT were strongly correlated with faster development during the embryo period and less so during the nestling period. Development rates were most strongly correlated with 5??-DHT, suggesting that potency increases along the androgen synthesis pathway and that effects are mediated by the androgen receptor pathway. These results are consistent with the hypothesis that selection for faster development by time-dependent offspring mortality may be achieved epigenetically by varying embryo exposure to maternal anabolic steroids. ?? 2007 by The University of Chicago. All rights reserved.

American Naturalist↗

USGS2021

Feather corticosterone reveals developmental challenges in a long-term study of juvenile northern spotted owls

Corticosterone is a steroid hormone integral to a variety of physiological pathways and is strongly associated with the vertebrate stress response. In avian species, circulating corticosterone is sequestered into developing feathers and is used as an indicator of energy allocation during feather growth and widely applied in conservation physiology. The northern spotted owl Strix occidentalis caurina is a federally threatened old-growth forest obligate of conservation concern endemic to the Pacific Northwest of the United States and Canada. The effects of landscape characteristics and individual variation on early development in spotted owls remain unstudied despite long recognition of this knowledge gap and its potential importance to species conservation. We quantified corticosterone concentrations in 4,720 feathers from 1,056 juvenile spotted owls across seven study areas between 2001 and 2017. We used an information-theoretic approach to examine the environmental and individual factors related to feather corticosterone in juvenile spotted owls as an indicator of challenges during early development. Feather corticosterone was positively related to temperature and precipitation, and negatively related to juvenile mass at banding. We found strong support for an interaction between mass and precipitation, with greater amounts of precipitation being associated with higher levels of feather corticosterone in lighter juveniles. The temperature and precipitation metric with the strongest relationship with feather corticosterone occurred during the fledging period, suggesting that this period presents an energetic challenge for juvenile spotted owls. Greater juvenile mass decreased the effect of precipitation, suggesting that greater mass was important for juveniles to maintain homeostasis during fledgling. Feather corticosterone in juvenile spotted owls provided insights to the challenges faced during early development, adding to our understanding of spotted owl life history and potential for population recovery.

Oregon, Washington↗

USGS2009

Sex assignment of lake sturgeon (Acipenser fluvescens) based on plasma sex hormone and vitellogenin levels

This study focused on identifying the sex of lake sturgeon by measuring the sex hormones estradiol and testosterone, and the phosphoprotein vitellogenin (Vtg) in blood plasma by radioimmunoassay and enzyme-linked immunosorbent assay, respectively, and evaluating these techniques as tools in lake sturgeon population management. Surveys of the St Clair River (SCR) lake sturgeon population have characterized it as rebounding by having steady or increasing recruitment since 1997. However, researchers have not been able to effectively determine the sex for most of the sturgeon they capture because few fish caught during surveys are releasing gametes. A total of 115 fish were sampled from May through June in 2004 and 2005 from the SCR, Michigan, USA. Of these, only four females and eight males were verified (i.e. they were releasing gametes at time of capture), resulting in very few fish with which to validate blood hormone and Vtg biomarkers of sex. Fifty-six percent of the fish were assigned a sex designation based on biomarker criteria. Correspondence between actual gonadal sex and biomarker-directed classification was good for the small subset of fish for which gonadal sex was definitively determined. Moreover, application of the steroid values in a predictive sex assignment model developed for white sturgeon misclassified only the same two fish that were misclassified with the steroid and Vtg biomarkers. The experimental results suggest a sex ratio of 1 : 2.7 (F:M), however more conclusive methods are needed to confirm this ratio because so few fish were available for sex validation. Of the 43 males, 14 were within the legal slot limit, 11 were smaller than 1067 mm total length (TL), and 18 were larger than 1270 mm TL. All 15 females were larger than 1270 mm TL, and thus protected by the slot limit criteria. Considering that lake sturgeon are threatened in Michigan, an advantage to using blood plasma assays was that fish were not harmed, and sample collection was quick, simple, and inexpensive. However, because a sufficiently large number of fish could not be validated for gonadal sex due to handling restrictions given the fish's protected status, assignment of sex is not based on a robust multi-variate model. An immediate alternative may be to use other non-invasive field methods (e.g. ultrasound, fiber-optic endoscope) to provide a more timely classification while establishing well-validated plasma hormone and Vtg-based predictive models for sex assignment of lake sturgeon. ?? 2009 Blackwell Verlag, Berlin.

Conference Paper↗

USGS2017

Reversible reduction of estrone to 17β-estradiol by Rhizobium, Sphingopyxis, and Pseudomonas isolates from the Las Vegas Wash

Environmental endocrine-disrupting compounds (EDCs) are a growing concern as studies reveal their persistence and detrimental effects on wildlife. Microorganisms are known to affect the transformation of steroid EDCs; however, the diversity of estrogen-degrading microorganisms and the range of transformations they mediate remain relatively little studied. In mesocosms, low concentrations of added estrone (E1) and 17β-estradiol (E2) were removed by indigenous microorganisms from Las Vegas Wash water within 2 wk. Three bacterial isolates, Rhizobium sp. strain LVW-9, Sphingopyxis sp. strain LVW-12, and Pseudomonas sp. strain LVW-PC, were enriched from Las Vegas Wash water on E1 and E2 and used for EDC transformation studies. In the presence of alternative carbon sources, LVW-9 and LVW-12 catalyzed near-stoichiometric reduction of E1 to E2 but subsequently reoxidized E2 back to E1; whereas LVW-PC minimally reduced E1 to E2 but effectively oxidized E2 to E1 after a 20-d lag. In the absence of alternative carbon sources, LVW-12 and LVW-PC oxidized E2 to E1. This report documents the rapid and sometimes reversible microbial transformation of E1 and E2 and the slow degradation of 17α-ethinylestradiol in urban stream water and extends the list of known estrogen-transforming bacteria to the genera Rhizobium and Sphingopyxis . These results suggest that discharge of steroid estrogens via wastewater could be reduced through tighter control of redox conditions and may assist in future risk assessments detailing the environmental fate of estrogens through evidence that microbial estrogen transformations may be affected by environmental conditions or growth status.

Nevada↗

USGS2011

Endocrine active chemicals, pharmaceuticals, and other chemicals of concern in surface water, wastewater-treatment plant effluent, and bed sediment, and biological characteristics in selected streams, Minnesota: Design, methods, and data, 2009

This report presents the study design, environmental data, and quality-assurance data for an integrated chemical and biological study of selected streams or lakes that receive wastewater-treatment plant effluent in Minnesota. This study was a cooperative effort of the U.S. Geological Survey, the Minnesota Pollution Control Agency, St. Cloud State University, the University of St. Thomas, and the University of Colorado. The objective of the study was to identify distribution patterns of endocrine active chemicals, pharmaceuticals, and other organic and inorganic chemicals of concern indicative of wastewater effluent, and to identify biological characteristics of estrogenicity and fish responses in the same streams. The U.S. Geological Survey collected and analyzed water, bed-sediment, and quality-assurance samples, and measured or recorded streamflow once at each sampling location from September through November 2009. Sampling locations included surface water and wastewater-treatment plant effluent. Twenty-five wastewater-treatment plants were selected to include continuous flow and periodic release facilities with differing processing steps (activated sludge or trickling filters) and plant design flows ranging from 0.002 to 10.9 cubic meters per second (0.04 to 251 million gallons per day) throughout Minnesota in varying land-use settings. Water samples were collected from the treated effluent of the 25 wastewater-treatment plants and at one point upstream from and one point downstream from wastewater-treatment plant effluent discharges. Bed-sediment samples also were collected at each of the stream or lake locations. Water samples were analyzed for major ions, nutrients, trace elements, pharmaceuticals, phytoestrogens and pharmaceuticals, alkylphenols and other neutral organic chemicals, carboxylic acids, and steroidal hormones. A subset (25 samples) of the bed-sediment samples were analyzed for carbon, wastewater-indicator chemicals, and steroidal hormones; the remaining samples were archived. Biological characteristics were determined by using an in-vitro bioassay to determine total estrogenicity in water samples and a caged fish study to determine characteristics of fish from experiments that exposed fish to wastewater effluent in 2009. St. Cloud State University deployed and processed caged fathead minnows at 13 stream sites during September 2009 for the caged fish study. Measured fish data included length, weight, body condition factor, and vitellogenin concentrations.

Minnesota↗

USGS2012

Chemicals of emerging concern in water and bottom sediment in Great Lakes areas of concern, 2010 to 2011-Collection methods, analyses methods, quality assurance, and data

The U.S. Geological Survey (USGS) cooperated with the U.S. Environmental Protection Agency and the U.S. Fish and Wildlife Service on a study to identify the occurrence of chemicals of emerging concern (CECs) in water and bottom-sediment samples collected during 2010–11 at sites in seven areas of concern (AOCs) throughout the Great Lakes. Study sites include tributaries to the Great Lakes in AOCs located near Duluth, Minn.; Green Bay, Wis.; Rochester, N.Y.; Detroit, Mich.; Toledo, Ohio; Milwaukee, Wis.; and Ashtabula, Ohio. This report documents the collection methods, analyses methods, quality-assurance data and analyses, and provides the data for this study. Water and bottom-sediment samples were analyzed at the USGS National Water Quality Laboratory in Denver, Colo., for a broad suite of CECs. During this study, 135 environmental and 23 field duplicate samples of surface water and wastewater effluent, 10 field blank water samples, and 11 field spike water samples were collected and analyzed. Sixty-one of the 69 wastewater indicator chemicals (laboratory method 4433) analyzed were detected at concentrations ranging from 0.002 to 11.2 micrograms per liter. Twenty-eight of the 48 pharmaceuticals (research method 8244) analyzed were detected at concentrations ranging from 0.0029 to 22.0 micrograms per liter. Ten of the 20 steroid hormones and sterols analyzed (research method 4434) were detected at concentrations ranging from 0.16 to 10,000 nanograms per liter. During this study, 75 environmental, 13 field duplicate samples, and 9 field spike samples of bottom sediment were collected and analyzed for a wide variety of CECs. Forty-seven of the 57 wastewater indicator chemicals (laboratory method 5433) analyzed were detected at concentrations ranging from 0.921 to 25,800 nanograms per gram. Seventeen of the 20 steroid hormones and sterols (research method 6434) analyzed were detected at concentrations ranging from 0.006 to 8,921 nanograms per gram. Twelve of the 20 pharmaceuticals (research method 8244) analyzed were detected at concentrations ranging from 2.35 to 453.5 nanograms per gram. Six of the 11 antidepressants (research method 9008) analyzed were detected at concentrations ranging from 2.79 to 91.6 nanograms per gram.

Great Lakes↗

USGS2009

Effects of wastewater discharges on endocrine and reproductive function of Western Mosquitofish (Gambusia spp.) and implications for the threatened Santa Ana Sucker (Catostomus santaanae)

The Santa Ana River (SAR) in southern California is impacted by effluents from wastewater treatment plants (WWTP), which are sources of organic wastewater compounds (OWCs) and urban runoff. The Santa Ana River is one of only three river basins supporting native populations of the federally listed Santa Ana sucker ( Catostomus santaanae ) at the time the fish was included on the list 2000. In 2004 and 2005, a U.S. Geological Survey and U.S. Fish and Wildlife Service study was undertaken to determine if the threatened Santa Ana sucker was potentially exposed to OWCs and endocrine disrupting compounds (EDCs) in the SAR by using the western mosquitofish ( Gambusia affinis ) as a surrogate fish model. Four Santa Ana River sites were chosen along a gradient of proximity to WWTP effluents: (1) a point source of tertiary treated wastewater effluent (TTWE), (2) Rialto Drain (just below a WWTP), (3) Prado Dam (11 kilometers [km] below WWTPs), and (4) Sunnyslope Creek (no WWTP but having urban runoff influence). A reference site having no WWTPs or urban runoff, Thousand Palms, was also sampled. Chemical analyses of passive sampler extracts results showed that 15 OWCs and EDCs were detected in water from the Santa Ana River sites. Many of these compounds contributed to activity from an estrogenic in-vitro assay that showed a significant potential for impacting endocrine and reproductive systems compared to the 25 organochlorine compounds detected in aquatic biota. The site showing compounds having highest influence on sex steroid hormone activities was the point source for TTWE. Sex steroid hormone levels, secondary sex characteristics, organosomatic indices, and sperm quality parameters indicated impairment of endocrine and reproductive function of male western mosquitofish in the Santa Ana River. Exposure to EDCs and consequent impairment in mosquitofish followed the gradient of proximity to WWTP effluents, where the most significant effects were found at TTWE point source and Rialto Drain, followed by Prado Dam and Sunnyslope Creek. Each of these sites is suitable habitat for the Santa Ana sucker, especially Sunnyslope Creek and Rialto Drain where juveniles reside. Various OWCs and EDCs were detected at each Santa Ana River site, although one specific compound or group of compounds could not be singled out as a causative factor. Di (2-ethylhexyl) phthalate was strongly negatively correlated with testosterone in male mosquitofish. One group of potent environmental estrogens that likely contributed to endocrine and reproductive impairment are the natural and synthetic estrogen hormones, especially ethinyl estradiol; however, this compound was not targeted in these investigations. The multiple lines of evidence for impaired reproductive and endocrine function in western mosquitofish due to OWCs and EDCs from the Santa Ana River can be used to identify potential problems for the Santa Ana sucker inhabiting the same and nearby sites.

California↗

USGS2011

Lagrangian sampling of wastewater treatment plant effluent in Boulder Creek, Colorado, and Fourmile Creek, Iowa, during the summer of 2003 and spring of 2005— Hydrological and water-quality data

This report presents methods and data for a Lagrangian sampling investigation into chemical loading and in-stream attenuation of inorganic and organic contaminants in two wastewater treatment-plant effluent-dominated streams: Boulder Creek, Colorado, and Fourmile Creek, Iowa. Water-quality sampling was timed to coincide with low-flow conditions when dilution of the wastewater treatment-plant effluent by stream water was at a minimum. Sample-collection times corresponded to estimated travel times (based on tracer tests) to allow the same "parcel" of water to reach downstream sampling locations. The water-quality data are linked directly to stream discharge using flow- and depth-integrated composite sampling protocols. A range of chemical analyses was made for nutrients, carbon, major elements, trace elements, biological components, acidic and neutral organic wastewater compounds, antibiotic compounds, pharmaceutical compounds, steroid and steroidal-hormone compounds, and pesticide compounds. Physical measurements were made for field conditions, stream discharge, and time-of-travel studies. Two Lagrangian water samplings were conducted in each stream, one in the summer of 2003 and the other in the spring of 2005. Water samples were collected from five sites in Boulder Creek: upstream from the wastewater treatment plant, the treatment-plant effluent, and three downstream sites. Fourmile Creek had seven sampling sites: upstream from the wastewater treatment plant, the treatment-plant effluent, four downstream sites, and a tributary. At each site, stream discharge was measured, and equal width-integrated composite water samples were collected and split for subsequent chemical, physical, and biological analyses. During the summer of 2003 sampling, Boulder Creek downstream from the wastewater treatment plant consisted of 36 percent effluent, and Fourmile Creek downstream from the respective wastewater treatment plant was 81 percent effluent. During the spring of 2005 samplings, Boulder Creek downstream from the wastewater treatment plant was 40 percent effluent, and Fourmile Creek downstream from that wastewater treatment plant was 28 percent effluent. At each site, 300 individual constituents were determined to characterize the water. Most of the inorganic constituents were detected in all of the stream and treatment-plant effluent samples, whereas detection of synthetic organic compounds was more limited and contaminants typically occurred only in wastewater treatment-plant effluents and at downstream sites. Concentrations ranged from nanograms per liter to milligrams per liter.

Colorado, Iowa↗