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USGS2013

Comprehensive assessment of hormones, phytoestrogens, and estrogenic activity in an anaerobic swine waste lagoon

In this study, the distribution of steroid hormones, phytoestrogens, and estrogenic activity was thoroughly characterized within the anaerobic waste lagoon of a typical commercial swine sow operation. Three independent rounds of sampling were conducted in June 2009, April 2010, and February 2011. Thirty-seven analytes in lagoon slurry and sludge were assessed using LC/MS-MS, and yeast estrogen screen was used to determine estrogenic activity. Of the hormone analytes, steroidal estrogens were more abundant than androgens or progesterone, with estrone being the predominant estrogen species. Conjugated hormones were detected only at low levels. The isoflavone metabolite equol was by far the predominant phytoestrogen species, with daidzein, genistein, formononetin, and coumestrol present at lower levels. Phytoestrogens were often more abundant than steroidal estrogens, but contributed minimally towards total estrogenic activity. Analytes were significantly elevated in the solid phases of the lagoon; although low observed log KOC values suggest enhanced solubility in the aqueous phase, perhaps due to dissolved or colloidal organic carbon. The association with the solid phase, as well as recalcitrance of analytes to anaerobic degradation, results in a markedly elevated load of analytes and estrogenic activity within lagoon sludge. Overall, findings emphasize the importance of adsorption and transformation processes in governing the fate of these compounds in lagoon waste, which is ultimately used for broadcast application as a fertilizer.

Environmental Science & Technology↗

USGS2015

Chemicals of emerging concern in water and bottom sediment in the Great Lakes Basin, 2012: collection methods, analytical methods, quality assurance, and study data

In synoptic surveys of surface-water quality across the United States, a large group of organic chemicals associated with agricultural, household, and industrial waste have been detected. These chemicals are referred to collectively as chemicals of emerging concern (CECs) and include prescription drugs and antibiotics, over-the-counter medications, reproductive hormones, personal-care products, detergent metabolites, and flame retardants. The U.S. Geological Survey (USGS) collaborated with the U.S. Fish and Wildlife Service and the U.S. Environmental Protection Agency on a study to identify the presence of CECs in water and bottom-sediment samples collected during 2012 at 66 sites throughout the Great Lakes Basin. The 2012 effort is part of a long-term study that was initiated in 2010. The purposes of this report are to document the collection and analytical methods, provide the quality-assurance data and analyses, and provide the water and bottom-sediment data for this study of CECs in the Great Lakes Basin for 2012. A previous report documents data collected during 2010 and 2011. The methods used for chemical analyses were identical between the 2010–11 and 2012 studies, with the exception that a method to determine nontarget chemicals was used during 2010–11. The data from this study are published as a USGS Data Series Report to ensure adequate documentation of the original methods and provide a citable source for study data. This report contains no interpretations of the study data. The chemical data are as reported by the laboratory and have not been censored or adjusted unless otherwise noted. Field measurements were recorded and samples were collected in April and May and in September 2012, by U.S. Geological Survey, U.S. Fish and Wildlife Service, and U.S. Environmental Protection Agency personnel. Study sites included tributaries to the Great Lakes located near Duluth, Minnesota; King, Wisconsin; Green Bay, Wis.; Detroit, Michigan; Monroe, Mich.; Toledo, Ohio, and Rochester, New York. Water and bottom-sediment samples were analyzed at the USGS National Water Quality Laboratory in Denver, Colorado, for a broad suite of CECs. During this 2012 study, 140 environmental and 8 field duplicate samples of surface water and wastewater effluent, 1 field blank water sample, and 5 field spike water samples were collected or prepared. Water samples were analyzed at the USGS National Water Quality Laboratory using laboratory schedule 4433 for wastewater indicators, research method 8244 for pharmaceuticals, and laboratory schedule 4434 for steroid hormones, sterols, and bisphenol A. For wastewater indicators in unfiltered water, 61 of the 68 chemicals analyzed using laboratory schedule 4433 had detectable concentrations ranging from 0.002 to 64.4 micrograms per liter. Thirty-eight of the 48 chemicals analyzed using research method 8244 for pharmaceuticals in unfiltered water had detectable concentrations ranging from 0.002 to 3.32 micrograms per liter. Twelve of the 20 chemicals analyzed using laboratory schedule 4434 for steroid hormones, sterols, and bisphenol A in unfiltered water had detectable concentrations ranging from 0.43 to 120,000 nanograms per liter. During this study, 53 environmental samples, 4 field duplicate samples, and 8 field spike samples of bottom sediment and laboratory matrix-spike samples were analyzed for a wide variety of CECs at the USGS National Water Quality Laboratory using laboratory schedule 5433 for wastewater indicators; research method 6434 for steroid hormones, sterols, and bisphenol A; and research method 9008 for human-use pharmaceuticals and antidepressants. Forty of the 57 chemicals analyzed using laboratory schedule 5433 had detectable concentrations ranging from 1 to 49,000 micrograms per kilogram. Fourteen of the 20 chemicals analyzed using research method 6434 had detectable concentrations ranging from 0.04 to 24,940 nanograms per gram. Ten of the 20 chemicals analyzed using research method 9008 had detectable concentrations ranging from 0.59 to 197.5 micrograms per kilogram. Five of the 11 chemicals analyzed using research method 9008 had detectable concentrations ranging from 1.16 to 25.0 micrograms per kilogram.

Great Lakes Basin↗

USGS2016

Compounds of emerging concern in the San Antonio River Basin, Texas, 2011–12

The City of San Antonio and the surrounding municipalities in Bexar County, Texas, are among the fastest growing cities in the Nation. Increases in residential and commercial development are changing runoff patterns and likely will increase chemical loads into streams. The U.S. Geological Survey, in cooperation with the San Antonio River Authority, evaluated the concentrations and distributional patterns of selected “compounds of emerging concern” (CECs) by collecting and analyzing water-quality samples from 20 sites in the San Antonio River Basin, Tex., during 2011–12. On the basis of their chemical composition or similar uses, the CECs discussed in this fact sheet are wastewater compounds, pharmaceutical compounds (hereinafter referred to as “pharmaceuticals”), and steroidal hormone and sterol compounds (hereinafter referred to as “steroidal hormones and sterols”). Three synoptic sampling events were completed during 2011–12 to analyze for CECs in the San Antonio River Basin. Samples were analyzed for 54 wastewater compounds, 13 pharmaceuticals, 17 steroidal hormones, and 4 sterols. Overall, the concentrations of all CECs analyzed for during this study were low, generally close to or less than the laboratory reporting level.

Texas↗

USGS1997

Reconnaissance of 17 beta-estradiol, 11-ketotestosterone, vitellogenin, and gonad histopathology in common carp of United States streams; potential for contaminant-induced endocrine disruption

A reconnaissance of sex steroid hormones and other biomarkers in common carp was used to assess whether endocrine disruption may be occurring in fish in United States streams, to evaluate relations between endocrine disruption and contaminant levels, and to determine requirements for further studies. 17?-estradiol, 11-ketotestosterone, vitellogenin, and gonadal histopathology were measured in adult carp (usually 10--15 for each sex) at 25 sites (647 fish), representing a wide range of environmental settings typical of major regions of the nation. Fish were collected during August--December 1994, a period of gonadal maturation after spawning. Contaminants evaluated were organochlorine pesticides and polychlorinated biphenyls in tissue; phthalates, phenols, and polycyclic aromatic hydrocarbons in bed sediment; and dissolved pesticides in water. Mean site concentrations of steroid hormones spanned two orders of magnitude for both sexes. No significant regional differences in steroid hormones were detected for males, but females from the Northern and Southern Midcontinent were significantly different from other regions of the country in one or both hormones. Within all regions there were significant differences between sites in one or both hormones for both sexes. Most correlation coefficients between biomarkers and contaminants were negative. Contaminants that had significant (a=0.05) correlations with biomarkers were organochlorine pesticides, phenols, and dissolved pesticides. The strongest pattern common to both males and females was a negative correlation between the hormone ratio (E2/11-KT) and dissolved pesticides. The significant site-to-site differences in biomarkers, and the presence of significant correlations between biomarkers and contaminants, are evidence that fish in some streams may be experiencing endocrine disruption. Improved information is needed to evaluate whether endocrine disruption is actually occurring and if there are reproductive effects on individual or populations of carp or other species. Future studies should shift to more intensive study of fewer sites, including reference and contaminated sites, in order to address these additional questions.

Open-File Report↗

USGS2022

Nonlethal tools to identify mass ovarian follicular atresia in Burbot

Skipped spawning, or variation in spawning periodicity, occurs in many annual spawning fish species and is an important consideration for population management. We assessed plasma sex steroid concentrations and measured gonad size and ovarian follicle diameter as metrics to nonlethally identify mass ovarian follicular atresia, which may contribute to skipped spawning in Burbot Lota lota . We maintained wild fish in captivity and exposed them to increasing water temperatures during a 3-wk period before the spawning season to induce mass ovarian follicular atresia. We collected ovarian follicles, blood plasma, and gonadal sonograms from fish weekly between January 28, 2018, and March 25, 2018. We histologically analyzed ovarian follicles to confirm stage of maturity. We measured concentrations of plasma sex steroids testosterone (T) and estradiol-17β (E2) by radioimmunoassay. We measured gonad diameter and circumference by ultrasonography and ovarian follicle diameter by image analysis. Mean plasma T concentration decreased from 8.94 ng/mL during late vitellogenesis to 1.83 ng/mL during atresia, suggesting that plasma T concentrations may be used to identify mass ovarian follicular atresia. We do not recommend using plasma E2 concentrations to identify mass ovarian follicular atresia because E2 concentrations rapidly decreased during the completion of vitellogenesis and the initiation of atresia in Burbot; therefore, plasma E2 may not accurately identify mass ovarian follicular atresia. Mean gonad diameter measured by ultrasonography decreased from 4.05 cm during late vitellogenesis to 3.65 cm during atresia. Mean diameter of ovarian follicles decreased during the final week of the study, suggesting that ovarian follicle diameter may be used to identify advanced mass ovarian follicular atresia. The nonlethal tools assessed—plasma sex steroid concentrations, ultrasonography, and ovarian follicle diameter—enable fisheries biologists to determine the occurrence and frequency of mass ovarian follicular atresia among Burbot in Lake Roosevelt and may be applied to other Burbot populations.

Journal of Fish and Wildlife Management↗

USGS2002

Characterization of annual reproductive cycles for pond-reared Florida largemouth bass Micropterus salmoides floridanus

The annual reproductive cycle of hatchery-raised largemouth bass (Florida subspecies Micropterus salmoides floridanus) was characterized over a one-year period. Largemouth bass have a distinct annual reproductive cycle with a spring spawning season (approximately between mid-January and mid-June). Cycle characterization focused on an evaluation of gonadal development and plasma concentrations of several sex steroids and vitellogenin (VTG). Adult largemouth bass (n = 20: 10 females and 10 males) were collected monthly from hatchery ponds for one full calendar year. Plasma samples were analyzed for estradiol-17?? (E2), 11-ketotestosterone (11-KT), testosterone (T), progesterone (P), and VTG. Gonadal tissues were weighed to calculate gonadosomatic index (GSI) and evaluated histologically to characterize reproductive stage. In both sexes, GSI began to increase in November, and peaked in February-March. Increases in gonad weights were correlated with maturation of gonads as evidenced by histological evaluations. Bass exhibited seasonal changes in plasma sex steroids and VTG. In males, 11-KT was the only sex steroid that showed strong seasonality, with highest values in February. In females, although E2 and T concentrations followed a similar annual cycle, with highest and lowest values in February and August, respectively, the strongest pattern was observed with E2. 11-KT concentrations were less variable across months, and values were about half of those observed in males. In females, P peaked two months after E2, with high values still in May and June and decreased thereafter, and VTG began to increase in October, but peaked a month prior to the observed peaked in E2. VTG was also detected in males but at concentrations that were about 1/12 that of females, and no seasonal pattern was evident. This study is the first to fully characterize the seasonal endocrine cycle for largemouth bass. These data will be useful when conducting reproductive evaluations of free-ranging populations of largemouth bass and for assessing potential reproductive effects due to environmental contaminants in this species. ?? 2002 by the American Fisheries Society.

American Fisheries Society Symposium↗

USGS2016

Landfill leachate as a mirror of today's disposable society: Pharmaceuticals and other contaminants of emerging concern in final leachate from landfills in the conterminous United States

Final leachates (leachate after storage or treatment processes) from 22 landfills in 12 states were analyzed for 190 pharmaceuticals and other contaminants of emerging concern (CECs), which were detected in every sample, with the number of CECs ranging from 1 to 58 (median = 22). In total, 101 different CECs were detected in leachate samples, including 43 prescription pharmaceuticals, 22 industrial chemicals, 15 household chemicals, 12 nonprescription pharmaceuticals, 5 steroid hormones, and 4 animal/plant sterols. The most frequently detected CECs were lidocaine (91%, local anesthetic), cotinine (86%, nicotine degradate), carisoprodol (82%, muscle relaxant), bisphenol A (77%, component of plastics and thermal paper), carbamazepine (77%, anticonvulsant), and N,N-diethyltoluamide (68%, insect repellent). Concentrations of CECs spanned 7 orders of magnitude, ranging from 2.0 ng/L (estrone) to 17 200 000 ng/L (bisphenol A). Concentrations of household and industrial chemicals were the greatest (&sim;1000-1 000 000 ng/L), followed by plant/animal sterols (&sim;1000-100 000 ng/L), nonprescription pharmaceuticals (&sim;100-10 000 ng/L), prescription pharmaceuticals (&sim;10-10 000 ng/L), and steroid hormones (&sim;10-100 ng/L). The CEC concentrations in leachate from active landfills were significantly greater than those in leachate from closed, unlined landfills (p = 0.05). The CEC concentrations were significantly greater (p < 0.01) in untreated leachate compared with treated leachate. The CEC concentrations were significantly greater in leachate disposed to wastewater treatment plants from modern lined landfills than in leachate released to groundwater from closed, unlined landfills (p = 0.04). The CEC concentrations were significantly greater (p = 0.06) in the fresh leachate (leachate before storage or treatment) reported in a previous study compared with the final leachate sampled for the present study.

Arkansas, Florida, Iowa, Kentucky, Maine, Minnesot↗

USGS2001

Impact of vinclozolin on reproductive behavior and endocrinology in Japanese quail (Coturnix coturnix japonica)

The impact of endocrine-disrupting chemicals (EDCs) has been demonstrated in mammalian models, but less research is available for avian species. The effects of vinclozolin (VIN), an antiandrogenic fungicide, on sexual differentiation and maturation were investigated in Japanese quail ( Coturnix coturnix japonica ). On day 4 of incubation, embryos were exposed to no treatment, oil, or 25, 50, or 100 ppm of VIN. Endpoints measured included adult male reproductive behavior, hypothalamic gonadotropin-releasing hormone I (GnRH-I) content in hatchlings and adults, plasma steroid levels in hatchlings and adults, proctodeal gland growth during maturation, and relative testicular weight at seven weeks of age. Results showed that exposure to VIN significantly ( p < 0.05) altered GnRH-I in male hatchlings, whereas GnRH-I levels in females remained unaffected. Although steroid levels were unaltered by any VIN treatment, the display of male reproductive behavior seemed delayed, with the number of mounts and the number of cloacal contacts being significantly ( p < 0.05) lower in the VIN-treated males. This could have an extreme negative impact on wild avian species that are routinely exposed to similar EDCs.

Environmental Toxicology and Chemistry↗

USGS2020

Gametogenesis and assessment of nonlethal tools to assign sex and reproductive condition in Burbot

Nonlethal tools (plasma sex steroid concentrations and ultrasound) for assigning sex and reproductive condition in Burbot Lota lota from Lake Roosevelt, Washington, were assessed. Gonadal tissue, blood plasma, and gonadal sonograms were collected monthly from November 2016 to March 2018. Gametogenesis was described by gonadal histology during an entire reproductive cycle to confirm sex and reproductive condition. Plasma testosterone (T) and estradiol-17β (E2) concentrations were measured by radioimmunoassay. Plasma 11-ketotestosterone (11-KT) concentrations were measured by liquid chromatography–mass spectrometry. Plasma sex steroid profiles, gonadosomatic index, and ovarian follicle diameter were also described during an entire reproductive cycle. Plasma 11-KT concentration was used to assign sex with 82% accuracy during the entire reproductive cycle, and plasma 11-KT and E2 concentrations were used to assign sex with 98% accuracy when fish were reproductive (i.e., November–March in Lake Roosevelt). Plasma T and E2 concentrations were used to assign reproductive condition in females with 98% accuracy, and plasma T concentration was used to assign reproductive condition in males with 90% accuracy. Ultrasound was used to assign sex with 96% accuracy but was not useful for assigning reproductive condition. Nonlethal tools to assign sex and reproductive condition will enable fisheries biologists to assess reproductive indices of the Burbot population in Lake Roosevelt to inform management decisions.

Washington↗

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↗