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New psychoactive substances (NPS) are compounds designed to mimic both licit and illicit drugs, and these substances are being discovered each year through forensic toxicology, drug enforcement agencies, and health authorities. However, there is limited information surrounding their international popularity. In this work, influent wastewater samples (n = 144) were collected from 25 sites in 10 countries: Australia, Belgium, Canada, China, Fiji, Italy, New Zealand, Republic of Korea, Spain, and the United States over the 2020-2021 New Year period. All samples were extracted in the country of origin then shipped and analyzed centrally at the University of South Australia using validated liquid chromatography-mass spectrometry methods. This study focused on 28 NPS stimulants, with 11 detected. The emerging substances eutylone and 3-methylmethcathinone (3-MMC) were detected most frequently and with the highest mass loads, indicating international popularity. Interestingly, the "older"generation stimulants, para-methoxyamphetamine (PMA), methylone, and mephedrone, were also detected. From the sites monitored in this work, areas in New Zealand had the highest loads of NPS stimulant consumption. Results here show that wastewater analysis can elucidate the dynamic nature of the NPS market, providing near real-time information on changing consumption patterns whose information can be used to minimize public risk. Refereed/Peer-reviewed

Dust samples were collected from four indoor environments, including childcare facilities, houses, hair salons, and a research facility from the USA and were analyzed for brominated compounds using full scan liquid chromatography high-resolution mass spectrometry. A total of 240 brominated compounds were detected in these dust samples, and elemental formulas were predicted for 120 more abundant ions. In addition to commonly detected brominated flame retardants (BFRs), nitrogen-containing brominated azo dyes (BADs) were among the most frequently detected and abundant. Specifically, greater abundances of BADs were detected in indoor dusts from daycares and salons compared to houses and the research facility. Using authentic standards, a quantitative method was established for two BADs (DB373: Disperse Blue 373 and DV93: Disperse Violet 93) and 2-bromo-4,6-dinitroaniline, a commonly used precursor in azo dye production, in indoor dust. Generally, greater concentrations of DB373 (≤3850 ng/g) and DV93 (≤1190 ng/g) were observed in indoor dust from daycares highlighting children as a susceptible population to potential health risk from exposure to BADs. These data are important because, to date, targeted analysis of brominated compounds in indoor environments has focused mainly on BFRs and appears to underestimate the total amount of brominated compounds.

A recent surge in the use and abuse of diverse prescribed psychotic and illicit drugs necessitates the surveillance of drug residues in source water and the associated ecological impacts of chronic exposure to the aquatic organism. Thirty-six psychotic and illicit drug residues were determined in discharged wastewater from two centralized municipal wastewater treatment facilities and two wastewater receiving creeks for seven consecutive days in Kentucky. Zebrafish (Danio rerio) larvae were exposed to the environmental relevant mixtures of all drug residues, all illicit drugs, and all prescribed psychotic drugs. The extracted RNA from fish homogenates was sequenced, and differentially expressed sequences were analyzed for known or predicted nervous system expression, and screened annotated protein-coding genes to the true environmental cocktail mixture. Illicit stimulant (cocaine and one metabolite), opioids (methadone, methadone metabolite, and oxycodone), hallucinogen (MDA), benzodiazepine (oxazepam and temazepam), carbamazepine, and all target selective serotonin reuptake inhibitors including sertraline, fluoxetine, venlafaxine, and citalopram were quantified in 100% of collected samples from both creeks. The high dose cocktail mixture exposure group revealed the largest group of differentially expressed genes: 100 upregulated and 77 downregulated (p ≤ 0.05; q ≤ 0.05). The top 20 differentially expressed sequences in each exposure group comprise 82 unique transcripts corresponding to 74% annotated genes, 7% non-coding sequences, and 19% uncharacterized sequences. Among 61 differentially expressed sequences that corresponded to annotated protein-coding genes, 23 (38%) genes or their homologs are known to be expressed in the nervous system of fish or other organisms. Several of the differentially expressed sequences are associated primarily with the immune system, including several major histocompatibility complex class I and interferon-induced proteins. Interleukin-1 beta (downregulated in this study) abnormalities are considered a risk factor for psychosis. This is the first study to assess the contributions of multiple classes of psychotic and illicit drugs in combination with developmental gene expression.

Consumption of licit and/or illicit compounds during sporting events has traditionally been monitored using population surveys, medical records, and law enforcement seizure data. This pilot study evaluated the temporal and geospatial patterns in drug consumption during a university football game from wastewater using liquid chromatography tandem mass spectrometry (LC-MS/MS). Untreated wastewater samples were collected from three locations within or near the same football stadium every 30 min during a university football game. This analysis leveraged two LCMS/ MS instruments (Waters Acquity TQD and a Shimadzu 8040) to analyze samples for 58 licit or illicit compounds and some of their metabolites. Bayesian multilevel models were implemented to estimate mass load and population-level drug consumption, while accounting for multiple instrument runs and concentrations censored at the lower limit of quantitation. Overall, 29 compounds were detected in at least one wastewater sample collected during the game. The 10 most common compounds included opioids, anorectics, stimulants, and decongestants. For compounds detected in more than 50% of samples, temporal trends in median mass load were correlated with the timing of the game; peak loads for cocaine and tramadol occurred during the first quarter of the game and for phentermine during the third quarter. Stadium-wide estimates of the number of doses of drugs consumed were rank ordered as follows: oxycodone (n = 3246) > hydrocodone (n = 2260) > phentermine (n = 513) > cocaine (n = 415) > amphetamine (n = 372) > tramadol (n = 360) > pseudoephedrine (n = 324). This analysis represents the most comprehensive assessment of drug consumption during a university football game and indicates that wastewater-based epidemiology has potential to inform public health interventions focused on reducing recreational drug consumption during large-scale sporting events.

In this study, residues of the neuropsychiatric and illicit drugs including stimulants, opioids, hallucinogens, anti-schizophrenics, sedatives, and antidepressants were determined in influent and effluent samples from a small wastewater treatment plant, a receiving creek, and river waters in the Four Rivers region of the Midwestern United States. Nineteen neuropsychiatric drugs, eight illicit drugs, and three metabolites of illicit drugs were detected and quantitated in the water samples using HPLC–MS/MS. Residual concentrations of the drugs varied from below the detection limit to sub-μg/L levels. The source of residual cocaine and benzoylecgonine in wastewater is primarily from human consumption of cocaine rather than direct disposal. Wastewater based epidemiology is utilized to estimate the community usage of drugs based on the concentration of drug residues in wastewater, wastewater inflow, and the population served by the centralized wastewater treatment plant. The per-capita consumption rate of methamphetamine (1740 mg/d/1000 people) and amphetamine (970 mg/d/1000 people) found in this study were the highest reported per-capita consumption rates in the USA. Antidepressant venlafaxine found to have the highest environmental emission from the WWTP(333 ± 160 mg/d/1000 people) followed by citalopram (132 ± 60.2 mg/d/1000 people), methamphetamine (111 ± 43.6 mg/d/1000 people), and hydrocodone (108 ± 90.1 mg/d/1000 people). Bee Creek, an immediate receiving water body, is found to be a source of several neuropsychiatric and illicit drugs including methamphetamine, methadone, alprazolam, oxazepam, temazepam, carbamazepine, venlafaxine, citalopram, sertraline, oxycodone, and hydrocodone (p < 0.036) in the Clarks River.

Sewage epidemiology is a cost-effective, comprehensive, and non-invasive technique capable of determining semi-real-time community usage of drugs utilizing the concentration of drug residues in wastewater, wastewater inflow, and the population size served by a wastewater treatment plant. In this study, semi-real-time consumption rates of ten illicit drugs were determined using sewage epidemiology during special events including Independence Day, the 2017 solar eclipse, and the first week of an academic semester in the Midwestern United States. The average per-capita consumption rate of amphetamine, methamphetamine, cocaine, and THC were significantly different between two similar-sized communities during Independence Day observation week (p

There is a growing concern over the contamination of surface water and the associated environmental and public health consequences from the recent proliferation of hydraulic fracturing in the USA. Petroleum hydrocarbon-derived contaminants of concern [benzene, toluene, ethylbenzene, and xylenes (BTEX)] and various dissolved cations and anions were spatially determined in surface waters around 15 coalbed methane fracking wells in Sullivan County, IN, USA. At least one BTEX compound was detected in 69% of sampling sites (n = 13) and 23% of sampling sites were found to be contaminated with all of the BTEX compounds. Toluene was the most common BTEX compound detected across all sampling sites, both upstream and downstream from coalbed methane fracking wells. The average concentration of toluene at a reservoir and its outlet nearby the fracking wells was ~2× higher than other downstream sites. However, one of the upstream sites was found to be contaminated with BTEX at similar concentrations as in a reservoir site nearby the fracking well. Calcium (~60 ppm) and sulfates (~175 ppm) were the dominant cations and anions, respectively, in surface water around the fracking sites. This study represents the first report of BTEX contamination in surface water from coalbed methane hydraulic fracturing wells.

Little information exists on the occurrence and the ultimate fate of pharmaceuticals in the water bodies in India despite being one of the world leaders in pharmaceutical production and consumption. This paper has reviewed 19 published reports of pharmaceutical occurrence in the aquatic environment in India [conventional activated sludge wastewater treatment plants (WTPs), hospital WTPs, rivers, and groundwater]. Carbamazepine (antipsychoactive), atenolol (antihypertensive), triclocarban and triclosan (antimicrobials), trimethoprim and sulfamethoxazole (antibacterials), ibuprofen and acetaminophen (analgesics), and caffeine (stimulant) are the most commonly detected at higher concentrations in Indian WTPs that treat predominantly the domestic sewage. The concentration of ciprofloxacin, sulfamethoxazole, amoxicillin, norfloxacin, and ofloxacin in Indian WTPs were up to 40 times higher than that in other countries in Europe, Australia, Asia, and North America. A very few studies in Indian rivers reported the presence of ciprofloxacin, enoxacin, ketoprofen, erythromycin, naproxen, ibuprofen, diclofenac and enrofloxacin. Similar compounds were reported in rivers in China, indicating a similar usage pattern in both of these developing countries. In a study reported from an open well in southern India, the groundwater showed the presence of cetirizine, ciprofloxacin, enoxacin, citalopram and terbinafine, which was close to a WTP receiving effluents from pharmaceutical production.

A cost-effective alternative approach capable of determining the prevalence of substance use in communities can complement the existing efforts of combating drug abuse and addiction. In this study, the prevalence of 10 illicit and 19 prescribed psychoactive drugs of potential abuse was determined utilizing wastewater-based epidemiology, and compared in two adjoined urban communities and a rural community. This is the first application of the Monte Carlo simulation method to account multiple uncertainties and propagation of errors associated with the individual parameter of wastewater based epidemiological estimations in the U.S. A significantly higher prevalence of cocaine [3830 (mean difference, MD: 2960) mg/d/1000 people] was found in the central business district while the per-capita consumption rates of amphetamine [738 (MD: 338) mg/d/1000 people] and methamphetamine [1660 (MD: 629) mg/d/1000 people] were higher in a rural community. Among narcotics, the per-capita consumption rate of fentanyl and morphine was significantly higher in urban communities while codeine, hydrocodone, hydromorphone, and buprenorphine were dominant in a rural community. The significantly higher prevalence of buprenorphine ((~)20-30 folds), oxycodone ((~)2-3 folds), and alprazolam ((~)2-3 folds) determined in these communities compared to the conventional estimates based on the electronically reported prescriptions and drug-related inpatient hospitalizations suggest the abuse of these drugs.

High school sports gather a significantly larger number of fans than college and professional sports in the U.S. Adolescent and adult students in high schools and colleges (aged 12–25) are among the most vulnerable population to substance use. Event planners, risk managers, and emergency medical service personnel can extrapolate the mass loads of drugs in wastewater in this study to evaluate the spectator behavior in relatively larger basketball gatherings. Thirty-three illicit and prescribed psychotic drug residues (out of target 36) and five new psychoactive substances (NPS, out of target 40) were quantified in wastewater, using ultra-performance liquid chromatography and tandem mass spectrometry, discharged during a college and a high school basketball games that were played in the same stadium in Kentucky. The wastewater concentrations of amphetamine, methylphenidate, hydromorphone were significantly higher (p ≤ 0.040) during a high school basketball game whereas cocaine, hydrocodone, and gabapentin was significantly higher (p ≤ 0.006) in a college basketball game. Higher cocaine to its metabolite ratio suggested that a significant amount of cocaine may have directly discharged down the drain during the college basketball game. Two synthetic cathinones (methcathinone and 4-methyl pentedrone) and three other NPSs (4-ANPP, mCPP, and 4-methylamphetamine) were also quantified in wastewater indicate the prevalence of NPSs in Kentucky. This is the first report of quantified substances of potential abuses at basketball games.

Isoprostanes are the potential biomarkers of endogenous human metabolism and proven clinically to provide the quantitative measure of systematic oxidative injury. An ultra-performance liquid chromatography-tandem mass spectrometric analytical method capable of determining four biomarkers of oxidative stress (8-iso-PGF2α, 2,3-dinor-iPF2α-III, PGE2, and 5-iPF2α-VI) in wastewater was developed and validated. Isoprostanes were quantified in the range of 31.1–1270 ng/L in raw wastewater samples in two communities in western Kentucky and Tennessee during the first four months of the COVID-19 pandemic. Consistent detection of PGE2 and 5-iPF2α-VI in wastewater suggested that PGE2 and 5-iPF2α-VI can be a reliable biomarker of community oxidative anxiety. The higher 4-month average mass load of isoprostanes [(ranged from 22.9 mg/d/1000 people to 807 mg/d/1000 people] may be attributed to the elevated community level oxidative anxiety owing COVID-19 uncertainties. The average mass loads of PGE2 and 5-iPF2α-VI in a community were significantly increased (two-tailed p, Graphical abstract Image 1, Highlights • Four oxidative stress hormones were determined in wastewater. • PGE2 and 5-iPF2α-VI can be a reliable biomarker of community oxidative anxiety. • Average mass load of isoprostanes ranged from 22.9 to 807 mg/d/1000 people. • Mass load of isoprostanes increased from the first to second month but decreased in the third month of COVID-pandemic.

Despite the high consumption of pharmaceuticals, mass loading and removal of these compounds in sewage treatment plants (STPs) in India have not been investigated. In this study, 43 pharmaceuticals and personal care products as well as 13 of their metabolites were analyzed in five domestic STPs (wastewater influent, effluent, and sludge) and in raw domestic sewage collected in open sewerage channels in residential areas in India. The mean concentrations of amphetamine in two of the five STPs (mean: 4300 ng/L and 4720 ng/L) were the highest ever reported for wastewater influents, globally. Among artificial sweeteners, saccharin was the most abundant compound in influents (mean: 303,000 ng/L, df: 100%), followed by cyclamate [3460 ng/L, detection frequency (df): 75%] and sucralose (1460 ng/L, df: 100%). Elevated mean concentrations of an antimicrobial (triclocarban = 6180 ng/L), analgesic (ibuprofen = 2320 ng/L), antihypertensive (atenolol = 3180 ng/L), illicit drug (amphetamine = 984 ng/L), and saccharin (419,000 ng/L) were found in the Cooum River in Chennai. The median removal efficiencies of pharmaceuticals and personal care products (PPCPs) ranged from 5% (norcocaine) to 100% (triclosan) for the five STPs. On the basis of the concentrations measured in influents, the mass loadings of PPCPs were estimated to range from 0.1 (norquetiapine) to 77,800 (saccharin) mg/d/1000 people. An estimated 2.55 kg of triclocarban, 3.24 kg of carbamazepine, 6.93 kg of amphetamine, and 252 kg of saccharin were discharged from a typical STP with an average flow rate of 20.7 million liters per day (serving a population of 325,000) in India.

Drug abuse is considered to be a national epidemic in many countries including the USA, and is associated with impaired social indicators including economic loss and adverse public health. The conventional methods of estimation of drug usage in communities are based on self-reported surveys, overdose or toxicological reports, drug-related crime statistics, and hospital admissions. Conventional methods suffer from several shortcomings including cost and time intensiveness, nonresponse bias, bias in the selection of sample population, and consumer's unawareness on the actual composition of used drugs. Sewage epidemiology utilizes the mass load of drugs in wastewater influent to estimate the drug usage in a community. Despite several challenges to the determination of the human excretion profile of drugs, the stability of drugs in wastewater, the dynamics of the population, sewage epidemiology provides several opportunities, including a cost-effective, comprehensive, noninvasive, and nearly real-time measure of trends of drug use over time.

Consumption of illicit drugs is considered to be a global socioeconomic burden of adverse ecological and public health. Proper identification and quantification of trace level residues of illicit drugs in wastewater allow for an estimation of drug usage in a community, the amount of drug discharge into the environment, and the overall fate of drugs in the environment. This chapter provides a procedural detail of the determination of select illicit drugs and their metabolites in wastewater, suspended particulate matter, and sewage sludge using high-performance liquid chromatography-electrospray ionization-tandem mass spectrometry.

Consumption of illicit drugs is considered to be a global socioeconomic burden of adverse ecological and public health. Proper identification and quantification of trace level residues of illicit drugs in wastewater allow for an estimation of drug usage in a community, the amount of drug discharge into the environment, and the overall fate of drugs in the environment. This chapter provides a procedural detail of the determination of select illicit drugs and their metabolites in wastewater, suspended particulate matter, and sewage sludge using high-performance liquid chromatography-electrospray ionization-tandem mass spectrometry.

Drug abuse is considered to be a national epidemic in many countries including the USA, and is associated with impaired social indicators including economic loss and adverse public health. The conventional methods of estimation of drug usage in communities are based on self-reported surveys, overdose or toxicological reports, drug-related crime statistics, and hospital admissions. Conventional methods suffer from several shortcomings including cost and time intensiveness, nonresponse bias, bias in the selection of sample population, and consumer's unawareness on the actual composition of used drugs. Sewage epidemiology utilizes the mass load of drugs in wastewater influent to estimate the drug usage in a community. Despite several challenges to the determination of the human excretion profile of drugs, the stability of drugs in wastewater, the dynamics of the population, sewage epidemiology provides several opportunities, including a cost-effective, comprehensive, noninvasive, and nearly real-time measure of trends of drug use over time.

Sample preparation represents about two-thirds of the cost of analysis and often presents logistical bottlenecks in analytical and environmental chemistry laboratories, thus reducing our capacity and preparedness to quantify organic pollutants rapidly and accurately. Selective pressurized liquid extraction (SPLE) is an analytical technique that builds upon PLE by incorporating matrix-compound (i.e. interference) retainers into the extraction step, thereby reducing sample-preparation steps and increasing sample throughput. SPLE methods offer distinct advantages over traditional methods, namely reduction in the costs intrinsic to sample preparation (i.e. time, solvents, labor, laboratory space, training, and potential loss of analytes). The ability to analyze and to evaluate rapidly a large number of samples directly increases the analytical capacity and preparedness of a laboratory for certain situations (e.g. large-scale studies or environmental emergencies). We review the analytical improvements via SPLE and its wide-ranging applications.

The fates of psychoactive pharmaceuticals, including two antischizophrenics, six sedative-hypnotic-anxiolytics, four antidepressants, four antihypertensives, and their select metabolites, were determined in two wastewater treatment plants (WWTPs) in the Albany area of New York. All target psychoactive pharmaceuticals and their metabolites were found at a mean concentration that ranged from 0.98 (quetiapine) to 1220 ng/L (atenolol) in wastewater and from 0.26 (lorazepam) to 1490 ng/g dry weight (sertraline) in sludge. In this study, the fraction of psychoactive pharmaceuticals that was sorbed to suspended particulate matter (SPM) was calculated for the first time. Over 50% of the total mass of aripiprazole, norquetiapine, norsertraline, citalopram, desmethyl citalopram, propranolol, verapamil, and norverapamil was found sorbed to SPM in the influent. The mass loadings, i.e., influx, of target psychoactive pharmaceuticals in WWTPs ranged from 0.91 (diazepam) to 347 mg/d/1000 inhabitants (atenolol), whereas the environmental emissions ranged from 0.01 (dehydro-aripiprazole) to 316 mg/d/1000 inhabitants (atenolol). The highest calculated removal efficiencies were found for antischizophrenics (quetiapine=88%; aripiprazole=71%). However, the removal of some psychoactive pharmaceuticals through adsorption onto sludge was minimal (

On-site wastewater treatment systems (OWTSs or septic systems) are designed to treat and dispose effluents on the same property that produces the wastewater. Approximately 25% of the U.S. population is served by such facilities. Nevertheless, studies on the treatment efficiency and discharge of organic contaminants through septic effluents are lacking. This pilot study showed the occurrence of organic contaminants including pharmaceuticals and personal care products (PPCPs), perfluoroalkyl surfactants (PFASs), polybrominated diphenyl ethers (PBDEs), and polychlorinated biphenyls (PCBs) in septic effluents, adjacent lake water samples, household drinking water in homes that use lake water or a well adjacent to the lake as a source of drinking water, and offshore lake water samples. Septic effluent as well as lake and tap water samples were collected from several households with OWTSs around Skaneateles Lake located in central New York. The advanced on-site systems were installed in some households for the purpose of limiting nutrient levels in the effluent to protect the local surface water. Additionally, because many of these systems serve homes with limited land, advanced treatment systems were needed. The median concentrations of ten PPCPs (ranged from 0.45 to 388 ng/L) and eleven PFASs (ranged from 0.20 to 14.6 ng/L) in septic water were significantly higher ( p ≤ 0.01) than in lake water samples. The median concentrations of PPCPs and PFASs in lake and tap water samples were not significantly different ( p ≥ 0.65). The median concentrations of ∑PBDEs in septic, lake, and tap water samples were 7.47, 3.49, and 2.22 ng/L, respectively, and those for ∑PCBs were 33.1, 29.2, and 28.6 ng/L, respectively. The mass flux of PPCPs (i.e. the mass flow of PPCPs per unit area per unit time) through the disposal of treated septic effluent from textile biofilter and aerobic treatments to the dispersal unit ranged from 12 (carbamazepine) to 66900 μg/m 2 /day (caffeine) whereas that for PFASs ranged from 7.0 (perfluorobutanesulfonate) to 833 μg/m 2 /day (perfluorooctanoic acid). Based on the ratio of measured concentrations and method detection limit, triclocarban, perfluorooctanoic acid, and perfluorooctanesulfonate have the potential to be used as chemical tracers of septic water contamination in Skaneateles Lake. The median concentrations of atenolol, a beta-blocker drug, in septic water were significantly ( ρ = 0.86, p = 0.01) correlated with enterococci counts.

Very few studies describe the fate of artificial sweeteners (ASWs) in wastewater treatment plants (WWTPs). In this study, mass loadings, removal efficiencies, and environmental emission of sucralose, saccharin, aspartame, and acesulfame were determined based on the concentrations measured in wastewater influent, primary effluent, effluent, suspended particulate matter (SPM), and sludge collected from two WWTPs in the Albany area of New York State, U.S.A. All ASWs were detected at a mean concentration that ranged from 0.13 (aspartame) to 29.4 μg/L (sucralose) in wastewater influent, 0.49 (aspartame) to 27.7 μg/L (sucralose) in primary influent, 0.11 (aspartame) to 29.6 μg/L (sucralose) in effluent, and from 0.08 (aspartame) to 0.65 μg/g dw (sucralose) in sludge. Aspartame was found in 92% of influent SPM samples at a mean concentration of 444 ng/g dw, followed by acesulfame (92 ng/g) and saccharin (49 ng/g). The fraction of the total mass of ASWs sorbed to SPM was in the rank order: aspartame (50.4%) > acesulfame (10.9%) > saccharin and sucralose (0.8%). The sorption coefficients of ASWs ranged from 4.10 (saccharin) to 4540 L/kg (aspartame). Significant removal of aspartame (68.2%) and saccharin (90.3%) was found in WWTPs; however, sucralose and acesulfame were less efficiently removed (

Dust from indoor environments can contain significant amounts environmental contaminants and is an important source of human exposure to several toxicants. In this article, studies on the occurrence of several emerging environmental contaminants, namely bisphenol A (BPA), tetrabromobisphenol A (TBBPA), phthalates, parabens, and other environmental phenolic compounds in indoor dust from various countries, were reviewed. Issues associated with sampling of dust and the uncertainties introduced in the analytical proce- dures were also summarized. Finally, exposure to environmental phenolic compounds through dust ingestion was evaluated, and the contribution of indoor dust to the total daily exposure of toxicants was estimated. Overall, the reported concentrations of target chemicals in dust were found, in decreasing order, as phthalates (overall mean: 949 ± 669 μg/g, range: 0.9-10,900 μg/g) >>> nonylphenol (8.9 ± 6.8 μg/g, 2.6-29.2 μg/g) > BPA (3.6 ± 4.5 μg/g, 0.35-16.6 μg/g) > � parabens (1.53 ± 0.52 μg/g, 0.03-125 μg/g) > pentachlorophenol (1.39 ± 2.31 μg/g, 0.050- 5.76 μg/g) > triclosan (0.65 ± 0.23 μg/g, 0.38-0.93 μg/g) > TBBPA (0.18 ± 0.14 μg/g, 0.049-0.505 μg/g). Despite the elevated levels of the target phenolic compounds reported in indoor dust, exposure of humans through dust ingestion was minor. Never- theless, dust can be a significant source of exposure to phenolic compounds for infants and toddlers. Elevated levels of phenolic com- pounds were found in dust collected from certain microenvironments such as offices and laboratories.

Sewage epidemiology is a rapidly expanding field that can provide information on illicit drug usage in communities, based on the measured concentrations in samples from wastewater treatment plants (WWTPs). In this study, select illicit drugs (six drugs and eight metabolites) were determined on a daily basis for a week in wastewater, suspended particulate matter (SPM), and sludge from two WWTPs in the Albany area in New York State. The WWTP that served a larger population (∼100 000, with a flow rate of 83 300 m(3)/d) showed 3.2 (methadone) to 51 (3,4-methylenedioxyamphetamine; MDA) times higher mass flows of illicit drugs than did the WWTP that served a smaller population (∼15 000, with a flow rate of 6850 m(3)/d). The consumption rate of target illicit drugs in the communities served by the two WWTPs was estimated to range from 1.67 to 3510 mg/d/1000 people. Between the dissolved and particulate phases, the fraction of methadone, 2-ethylidene-1,5-dimethyl-3,3-diphenylpyrrolidine (EDDP), amphetamine, and MDA sorbed to SPM ranged from 34.3% to 41.1% of the total mass in the waste stream. The removal efficiencies of illicit drugs from the two WWTPs ranged from 4% (norcocaine) to 99% (cocaine); however, methamphetamine, methadone, and EDDP showed a negative removal in WWTPs. The environmental emission of illicit drugs from WWTP discharges was calculated to range from 0.38 (MDEA) to 67.5 (EDDP) mg/d/1000 people. Other markers such as caffeine, paraxanthine, nicotine, and cotinine were found to predict the concentrations of select illicit drugs in raw wastewater (r(2) = 0.20-0.79; p ≤ 0.029).

A selective pressurized liquid extraction technique (SPLE) was developed for the analysis of polychlorodibenzo-p-dioxins, polychlorodibenzofurans (PCDD/Fs) and dioxin-like polychlorobiphenyls (dl-PCBs) in clam and crab tissue. The SPLE incorporated multiple cleanup adsorbents (alumina, florisil, silica gel, celite, and carbopack) within the extraction cell. Tissue extracts were analyzed by high resolution gas chromatography coupled with electron capture negative ionization mass spectrometry. Mean recovery (n = 3) and percent relative standard deviation for PCDD/Fs and dl-PCBs in clam and crabs was 89 ± 2.3 and 85 ± 4.0, respectively. The SPLE method was applied to clams and crabs collected from the San Jacinto River Waste Pits, a Superfund site in Houston, TX. The dl-PCBs concentrations in clams and crabs ranged from 50 to 2,450 and 5 to 800 ng/g ww, respectively. Sample preparation time and solvents were reduced by 92 % and 65 %, respectively, as compared to USEPA method 1613.

Concern over the occurrence of pharmaceuticals and their metabolites in the environment is mounting due to the potential adverse effects on nontarget organisms. This study draws upon a nationwide survey of psychoactive pharmaceuticals (i.e., antischizophrenics, anxiolytics, and antidepressants) in sludge from 40 representative wastewater treatment plants (WWTPs) that receive domestic, industrial, or mixed (domestic plus industrial) wastewaters in Korea. A total of 16 psychoactive pharmaceuticals (0.12-460 ng/g dry weight) and nine of their metabolites (0.97-276 ng/g dry weight) were determined in sludge. The median concentrations of psychoactive drugs in sludge from domestic WWTPs were 1.2-3.2 times higher than the concentrations found in WWTPs that receive combined domestic and industrial wastewaters. Among the psychoactive drugs analyzed, the median environmental emission rates of alprazolam (APZ) and carbamazepine (CBZ) through domestic WWTPs (both sludge and effluent discharges combined) were calculated to be ≥ 15.5 μg/capita/day, followed by quetiapine (QTP; 8.51 μg/capita/day), citalopram (CLP; 5.45 μg/capita/day), and venlafaxine (VLF; 3.59 μg/capita/day). The per-capita emission rates of some of the metabolites of psychoactive drugs through WWTP discharges were higher than those calculated for parent compounds. Significant correlations (ρ = 0.432-0.780, p0.05) were found between the concentrations of typically coprescribed antischizophrenics and antidepressants in sludge. Multiple linear regression analysis of measured concentrations of drugs in sludge revealed that several WWTP parameters such as treatment capacity, population-served, sludge production rate, composition of wastewater (domestic versus industrial), and hydraulic retention time can affect the concentrations of psychoactive drugs in sludge.

Environmental contamination by pharmaceuticals and personal care products (PPCPs) is barely studied in India despite being one of the largest global producers and consumers of pharmaceuticals. In this study, 29 pharmaceuticals and six metabolites were determined in sewage treatment plants (STPs) in Udupi (STPU: population served ∼150,000) and Mangalore (STPM: population served ∼450,000); the measured mean concentrations ranged from 12 to 61,000 ng/L and 5.0 to 31,000 ng/L, respectively. Atorvastatin (the most prescribed antihypercholesterolemic in India), mefenamic acid, and paraxanthine were found for the first time in wastewater in India at the mean concentrations of 395 ng/L, 1100 ng/L, and 13,000 ng/L, respectively. Select pharmaceutical metabolites (norverapamil and clopidogrel carboxylic acid) were found at concentrations of upto 7 times higher than their parent drugs in wastewater influent and effluent. This is the first study in India to report mass loading and emission of PPCPs and their select metabolites in STPs. The total mass load of all PPCPs analyzed in this study at STPU (4.97 g/d/1000 inhabitants) was 3.6 times higher than calculated for STPM. Select recalcitrant PPCPs (carbamazepine, diazepam, and clopidogrel) were found to have negative or no removal from STPU while additional treatment with upflow anaerobic sludge blanket reactor at STPM removed (up to 95%) these PPCPs from STPM. Overall, 5.1 kg of caffeine, 4.1 kg of atenolol, 2.7 kg of ibuprofen, and 1.9 kg of triclocarban were discharged annually from STPU. The PPCP contamination profile in the Indian STP was compared with a similar study in the USA.

A high-throughput enhanced pressurized liquid extraction technique was developed by incorporating pressurized liquid extraction and multiple cleanup techniques. USEPA methods of polychlorodibenzo- p -dioxins, polychlorodibenzofurans (PCDD/Fs) and dioxin-like polychlorobiphenyls (dl-PCBs) analysis in fish tissue include independent silica gel, florisil, alumina, and carbopack/celite column cleanup techniques following extraction. Under the improved method, fish composites (∼10 g) were extracted and cleaned simultaneously using alumina (∼10 g), florisil (∼10 g), silica gel (∼5 g), celite (∼5 g), and carbopack (∼0.5 g). Clean extracts were concentrated and then analyzed by high resolution gas chromatography coupled with electron capture negative ionization mass spectrometry. Carbopack/celite within the extraction cell provided the analytical separation of dl-PCBs from PCDD/Fs, reducing potential molecular interferences. The average recoveries ( n = 3) of dl-PCBs in dichloromethane:hexane (1:1, v/v) extracts were 93 ± 2.4% and PCDD/Fs in toluene extracts were 85 ± 3.0%. The developed method was applied to measure the PCDD/Fs and dl-PCBs in catfish from San Jacinto River Waste Pits, a Superfund site in Houston, TX. The dl-PCBs were measured at 5.0–17,000 pg g −1 ww. Sample preparation time and solvents were reduced as much as 95% and 65%, respectively, as compared to USEPA method 1613.

Since the 1970s, the brominated flame retardants (BFRs), polybrominated diphenyl ethers (PBDEs), hexabromocyclododecanes (HBCDs), and tetrabromobisphenol A (TBBPA) have been used as additive or reactive flame retardants (FRs) in household products including foam furniture, baby products, mattresses, textiles, electronics, food packaging, and housing insulation to meet flammability standards. Many of these chemicals are now recognized as global contaminants and are associated with adverse health effects including endocrine disruption, reproductive toxicity, developmental neurotoxicity, and cancer. Additive BFRs migrate out of products and accumulate in dust of indoor environments. Dust ingestion is the primary route of human exposure to BFRs, and studies link body burdens of adults and children to indoor dust concentrations. Because of health concerns, PentaBDE and OctaBDE mixtures were phased out of production in 2005, and DecaBDE and HBCDs are scheduled for global elimination by 2013. However, large amounts of in-use and discarded household products will continue to release these BFRs into the environment and TBBPA is still in high-volume use worldwide. Following the PBDE phase-out, many replacement FRs with known or suspected toxicity have been detected at increasing levels in household products and dust. Exposure of infants and children to FRs in baby products and house dust is of special concern. The continued use of FRs with known toxicities and introduction of untested replacement chemicals highlights the need to update flammability standards and modernize chemical policies to require disclosure and safety testing of FR chemicals prior to sale.

Concern over the occurrence of artificial sweeteners (ASWs) as well as pharmaceuticals and personal care products (PPCPs) in the environment is growing, due to their high use and potential adverse effects on non-target organisms. The data for this study are drawn from a nationwide survey of ASWs in sewage sludge from 40 representative wastewater treatment plants (WWTPs) that receive domestic (WWTPD), industrial (WWTPI), or mixed (domestic plus industrial; WWTPM) wastewaters in Korea. Five ASWs (concentrations ranged from 7.08 to 5220 ng/g dry weight [dw]) and ten PPCPs (4.95–6930 ng/g dw) were determined in sludge. Aspartame (concentrations ranged from 28.4 to 5220 ng/g dw) was determined for the first time in sewage sludge. The median concentrations of ASWs and PPCPs in sludge from domestic WWTPs were 0.8–2.5 and 1.0–3.4 times, respectively, the concentrations found in WWTPs that receive combined domestic and industrial wastewaters. Among the five ASWs analyzed, the median environmental emission rates of aspartame through domestic WWTPs (both sludge and effluent discharges combined) were calculated to be 417 μg/capita/day, followed by sucralose (117 μg/capita/day), acesulfame (90 μg/capita/day), and saccharin (66 μg/capita/day). The per-capita emission rates of select PPCPs, such as antimicrobials (triclocarban: 158 μg/capita/day) and analgesics (acetaminophen: 59 μg/capita/day), were an order of magnitude higher than those calculated for antimycotic (miconazole) and anthelmintic (thiabendazole) drugs analyzed in this study. Multiple linear regression analysis of measured concentrations of ASWs and PPCPs in sludge revealed that several WWTP parameters, such as treatment capacity, population-served, sludge production rate, and hydraulic retention time could influence the concentrations found in sludge. Keywords: Artificial sweeteners, Aspartame, Saccharin, Triclocarban, Acetaminophen, Antibiotics, Sludge, Wastewater treatment plant, Pharmaceuticals and personal care products

Lipid-rich matrices are often sinks for lipophilic contaminants, such as pesticides, polychlorinated biphenyls (PCBs), and polybrominated diphenyl ethers (PBDEs). Typically methods for contaminant extraction and cleanup for lipid-rich matrices require multiple cleanup steps; however, a selective pressurized liquid extraction (SPLE) technique requiring no additional cleanup has been developed for the simultaneous extraction and cleanup of whale earwax (cerumen; a lipid-rich matrix). Whale earwax accumulates in select whale species over their lifetime to form wax earplugs. Typically used as an aging technique in cetaceans, layers or laminae that comprise the earplug are thought to be associated with annual or semiannual migration and feeding patterns. Whale earplugs (earwax) represent a unique matrix capable of recording and archiving whales’ lifetime contaminant profiles. This study reports the first analytical method developed for identifying and quantifying lipophilic persistent organic pollutants (POPs) in a whale earplug including organochlorine pesticides, polychlorinated biphenyls (PCBs), and polybrominated diphenyl ethers (PBDEs). The analytical method was developed using SPLE to extract contaminants from ∼0.25 to 0.5 g aliquots of each lamina of sectioned earplug. The SPLE was optimized for cleanup adsorbents (basic alumina, silica gel, and Florisil ® ), adsorbent to sample ratio, and adsorbent order. In the optimized SPLE method, the earwax homogenate was placed within the extraction cell on top of basic alumina (5 g), silica gel (15 g), and Florisil ® (10 g) and the target analytes were extracted from the homogenate using 1:1 (v/v) dichloromethane:hexane. POPs were analyzed using gas chromatography–mass spectrometry with electron capture negative ionization and electron impact ionization. The average percent recoveries for the POPs were 91% (±6% relative standard deviation), while limits of detection and quantification ranged from 0.00057 to 0.96 ng g −1 and 0.0017 to 2.9 ng g −1 , respectively. Pesticides, PCBs, and PBDEs, were measured in a single blue whale ( Balaenoptera musculus ) cerumen lamina at concentrations ranging from 0.11 to 150 ng g −1 .

There is an increasing demand for high-throughput analytical methods specifically designed for the quantitation of organic contaminants in biological matrices. This demand exists in the broad fields of environmental chemistry and toxicology as well as medicine, food safety, drug discovery, and criminal forensics. Analytical chemists seek to develop techniques to reduce or eliminate method bottlenecks, which will improve the flow of information and downstream decisions. Advances in analysis of organic contaminants in biological matrices require the development of a novel sample preparation technique as well as more detailed MS/MS optimization. These analytical methods improve the laboratory’s ability to provide routine analysis and scale up its capability for larger, time-sensitive projects, such as environmental disasters. In addition, these advances reduce labor, training, consumption of and exposure to hazardous organic solvents, and laboratory space, thus reducing the time and cost of analysis.

German Environment Specimen Bank (GESB) fish tissue samples, collected from 14 different GESB locations, were analyzed for 15 pharmaceuticals, 2 pharmaceutical metabolites, and 12 personal care products. Only 2 pharmaceuticals, diphenhydramine and desmethylsertraline, were measured above MDL. Diphenhydramine (0.04-0.07 ng g(-1) ww) and desmethylsertraline (1.65-3.28 ng g(-1) ww) were measured at 4 and 2 locations, respectively. The maximum concentrations of galaxolide (HHCB) (447 ng g(-1) ww) and tonalide (AHTN) (15 ng g(-1) ww) were measured at the Rehlingen sampling site in the Saar River. A significant decrease in HHCB and AHTN fish tissue concentrations was observed from 1995 to 2008 at select GESB sampling sites (r(2) = 0.69-0.89 for galaxolide and 0.89-0.97 for tonalide with p < 0.003). Galaxolide and tonalide fish tissue concentrations in Germany were ∼19× and ∼28× lower, respectively, as compared to fish tissue concentrations measured in a United States nationwide PPCP study conducted in 2006. Proximity of the sampling locations to the upstream wastewater treatment plant discharging point and mean annual flow at the sampling location were found to significantly predict galaxolide and tonalide fish tissue concentrations (HHCB: r(2) = 0.79, p = 0.021 and AHTN: r(2) = 0.81, p = 0.037) in Germany.

Analytical improvements were developed and validated for measuring select personal care products (PCPs) and two pharmaceuticals in fish tissue. The method was validated using fortified fillet tissue for twelve PCPs including fragrance materials, alkylphenols, photo initiators, and triclosan as well as two pharmaceuticals including carbamazepine (anti-seizure) and diazepam (anti-convulsant). The analytical method utilized pressurized liquid extraction (PLE) combined with silica gel cleanup, gel permeation chromatography, and gas chromatography ion-trap tandem mass spectrometry. Silica gel cleanup was combined with the PLE to produce one automated extraction/cleanup technique. This analytical improvement served to reduce the incurred cost, time, and loss of potential target analytes associated with independent cleanup steps. The combined extraction/cleanup technique resulted in an average increase of 10% in analyte recoveries. Average triplicate recoveries and relative standard deviations for the entire method, using 2.5 g of fish fillet tissue, were 92 ± 9% (recoveries ranged from 64 to 131%). The sensitivity of the analytical methods was improved by optimizing the resonant collision induced dissociation energy to the hundredths place (0.01 V). Improvements in ion production range from 24 to 122% for six of the 12 PCPs. Statistically derived method detection limits (MDLs) were also lowered on average by a factor of 8 and ranged from 1.2 to 38 ng/g wet weight. MDLs for carbamazepine and diazepam were 18 and 3.7 ng/g wet weight, respectively. Galaxolide and tonalide were measured in an environmental sample at concentrations of 81 and 5.5 ng/g wet weight, respectively.