It is well known that pharmaceuticals are not completely removed by conventional activated sludge wastewater treatment plants. Hospital effluents are of major concern, as they present high ...concentrations of pharmaceutically active compounds. Despite this, these specific effluents are usually co-treated with domestic wastewaters. Separate treatment has been recommended. However, there is a lack of information concerning the efficiency of separate hospital wastewater treatment by activated sludge, especially on the removal of pharmaceuticals. In this context, this article presents the results of a 2-year monitoring of conventional parameters, surfactants, gadolinium, and 13 pharmaceuticals on the specific study site SIPIBEL. This site allows the characterization of urban and hospital wastewaters and their separate treatment using the same process. Flow proportional sampling, solid-phase extraction, and liquid chromatography coupled with tandem mass spectrometry were used in order to obtain accurate data and limits of quantification consistent with ultra-trace detection. Thanks to these consolidated data, an in-depth characterization of urban and hospital wastewaters was realized, as well as a comparison of treatment efficiency between both effluents. Higher concentrations of organic carbon, AOX, phosphates, gadolinium, paracetamol, ketoprofen, and antibiotics were observed in hospital wastewaters compared to urban wastewaters. Globally higher removals were observed in the hospital wastewater treatment plant, and some parameters were shown to be of high importance regarding removal efficiencies: hydraulic retention time, redox conditions, and ambient temperature. Eleven pharmaceuticals were still quantified at relevant concentrations in hospital and urban wastewaters after treatment (e.g., up to 1 μg/L for sulfamethoxazole). However, as the urban flow was about 37 times higher than the hospital flow, the hospital contribution appeared relatively low compared to domestic discharges. Thanks to the SIPIBEL site, data obtained from this 2-year program are useful to evaluate the relevance of separate hospital wastewater treatment.
A multi residue analysis was developed for screening, quantification and confirmation of 36 priority organic compounds included in the 2000/60/EC European Water Framework Directive. The compounds ...analyzed included 19 pesticides, 8 PAH, 5 endocrine-disruptors and 4 organochlorine compounds. The method was developed in three steps. First, automated off-line solid-phase extraction using Strata X cartridges was optimized to trap simultaneously the 36 studied compounds. Second, the more volatile compounds were analysed by gas chromatography coupled to mass spectrometry with electron impact ionisation in selected ion monitoring mode (SIM). Third, the last 20 compounds were detected and quantified, in one run, by liquid chromatography coupled to fluorescence detector and tandem mass spectrometry. The excellent selectivity and sensitivity allowed us satisfactory quantification and confirmation at levels as low as 0.2–67ngL−1 with recoveries between 59 and 105%. Such methodology was then applied to French surface waters: all the waters present organic contaminants, and their concentration varied according to the origin and nature of substances.
► A multi-residues multi-families method for the analysis of 31 emerging pollutants. ► An innovative, rapid and simple sample extraction based on QuEChERS. ► Analytical method allowing the ...determination of the analytes at the low ng/g range. ► Application of the method to real soil samples.
The aim of this study was to develop an analytical method for the analysis of traces of hormonal steroids and veterinary and human drugs in soil. Thus, 31 substances were selected, including 14 veterinary products, 11 hormonal steroids and 6 other well-known human contaminant compounds. The procedure inspired by the quick, easy, cheap, effective, rugged and safe (QuEChERS) extraction method was developed. First the acetonitrile-based extraction was optimized. This step was followed by a solid-phase extraction (SPE) clean-up using both a strong anion-exchange cartridge and a polymeric cartridge. The analysis was then performed using liquid chromatography coupled to a triple quadrupole analyser operated with tandem mass spectrometry. This analytical procedure was validated using the ICH/2005 standard by evaluating the linearity (from 0.01ng/g to 1000ng/g –R2>0.99), the intra-day precision (relative standard deviation (RSD)<20%), the inter-day precision (RSD<30%), recoveries (40–110% for most of the compounds) and limits of detection and quantification. This method allowed for the determination of the target analytes in the lower ng/g concentration range. The methodology was then applied to real soil samples collected in several areas of France that received different manure or sludge treatments. Some target compounds were detected at very low level (inferior to the ng/g). Veterinary antibiotics, mainly from the sulfonamide family, were found in soils treated by manure (0.02–0.12ng/g). On the other hand, pharmaceuticals usually used by humans (carbamazepine, ibuprofen) were detected in soils treated by domestic sludge.
Most analytical methodologies currently available for the determination of steroids in water only identify a few representative compounds (mainly estrogens). In this context, a multi-residue ...methodology based on liquid chromatography–tandem mass spectrometry was developed for the determination of 26 steroids including natural and synthetic estrogens, progestagens and androgens. The method described involves limited sample preparation as it includes a filtration followed by a single solid-phase extraction step using a C18 cartridge. The analytical procedure allows the determination of the target analytes in the lower ng/L range, with recoveries above 80%. The methodology was successfully applied to the analysis of steroids in several surface and ground-waters. In all the waters, estrogens, androgens and/or progestagens were determined.
Emerging contaminants are suspected to cause adverse effects in humans and wildlife. Aquatic ecosystems are continuously contaminated by agricultural and industrial sources. To establish a causality ...relationship between the occurrence of contaminants in the environment and disease, experiments including all environmental matrices must be performed. Consequently, the current analytical tools must be improved. A new multi-residue method for analysing 15 emerging pollutants in sediments based on the Quick, Easy, Cheap, Effective, Rugged and Safe approach is reported. The development of such a multirisque, inter-family method for sediment including pharmaceuticals, pesticides, personal care products and plasticizers is reported for the first time. The procedure involves salting-out liquid–liquid extraction using acetonitrile and clean-up with dispersive solid phase extraction, followed by liquid chromatography coupled with tandem mass spectrometry. The validated analytical procedure exhibited recoveries between 40 and 98 % for every target compound. This methodology facilitated the determination of pollutant contents at nanogram-per-gram concentrations.
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Healthcare facility discharges, by their nature, are often considered as non-domestic effluent, which can provide significant pollution comparatively to other domestic sources. In this context, a ...total of 12 monthly sampling campaigns were collected from a healthcare facility as well as the output of a sewerage system of Site Pilote de Bellecombe (SIPIBEL) observatory. This study focuses more specifically on 12 surfactants and biocides: four anionics, four cationic, two non-ionic, one zwitterionic, and one dispersive agent, among the most commonly used commercial surfactants. Particular attention was also provided to routine wastewater quality parameters. Both effluents were heavily contaminated by most anionic surfactants; they displayed median concentrations up to 1 to 2 mg/L for linear alkylbenzene sulfonates and between 10 and 100 μg/L for other sodium sulfate congeners (lauryl and laureth). Overall, for the majority of surfactants, the healthcare facility contribution to the total flux reaching the wastewater treatment plant ranges between 5 and 9%.
One of the most adopted solutions in developed countries to manage stormwater is detention/retention basins which generate large quantities of sediments that have to be removed regularly. In order to ...manage them properly, accurate data are needed about their physical and chemical characteristics, particularly on micropollutant concentrations and their associated risk. This work consisted in a two-year sampling of dry sediments from a detention-settling basin. Priority substances, including pesticides, polybrominated diphenyl ethers (PBDE), alkylphenols and bisphenol A (BPA), were monitored. Different sites in the basin bottom were sampled in order to investigate spatial distribution of the contamination. Results show that the increase of the sediment thickness in the basin was heterogeneous with a maximum of 15 cm after two years. Pesticides and PBDE were, if detected, mainly found in low concentrations from 2 ng/g to 286 ng/g. Conversely, alkylphenols and bisphenol A were always quantified at concentrations varying from 6 ng/g to 3400 ng/g. These high levels suggest that these sediments should be managed with precautions. Spatial heterogeneity of alkylphenol ethoxylates and BPA concentrations was observed, with higher contamination of alkylphenol ethoxylates in anaerobic zones and BPA levels correlated with total organic carbon and in a lesser extent to fine particles.
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•Strong impregnation of stormwater sediments with 4-nonylphenol and bisphenol A.•Contamination of sediments did not increase with time.•Spatial heterogeneity was different from one substance to another.•Bisphenol A concentrations and total organic carbon were correlated.•Some sources of priority substances in an industrial catchment were highlighted.
Forty four priority substances, including endocrine disruptors, were followed during two years in stormwater sediments from a dry detention basin.
Pesticide residues in fish muscle are an environmental and a health safety concern which requires analytical methods presenting high sensitivity and low limits of quantification. In this study, ...adapted QuEChERS method, coupled to liquid chromatography tandem mass spectrometry (Scheduled MRM-5500 QTRAP), was developed to quantify 13 pesticides (azoxystrobin, clomazone, diflufenican, dimethachlor, carbendazim, iprodion, isoproturon, mesosulfuron-methyl, metazachlor, napropamid, quizalofop and thifensulfuron-methyl) in muscle of fish. Quantification limits were below 1 ng g
−1
except for clomazone (1.8 ng g
−1
) and quizalofop (7.4 ng g
−1
). Best recoveries were observed for perch (>80%) and roach (>68%), except for thifensulfuron-methyl. Lower recoveries had been observed for carp (6% to 86%). Relative standard deviation was lower than 28% for intra-day and 29% for inter-day analysis, respectively. This method was successfully tested on three fish species, naturally or orally exposed: roach (
Rutilus rutilus
), perch (
Perca fluviatilis
) and carp (
Cyprinus carpio
). Few levels were observed in fish naturally exposed, but carp and perch orally contaminated showed measurable levels in their muscles.
Pesticides residues in aquatic ecosystems are an environmental concern which requires efficient analytical methods. In this study, we proposed a generic method for the quantification of 13 pesticides ...(azoxystrobin, clomazone, diflufenican, dimethachlor, carbendazim, iprodion, isoproturon, mesosulfuron-methyl, metazachlor, napropamid, quizalofop and thifensulfuron-methyl) in three environmental matrices. Pesticides from water were extracted using a solid phase extraction system and a single solid–liquid extraction method was optimized for sediment and fish muscle, followed by a unique analysis by liquid chromatography coupled with tandem mass spectrometry (LC–MS/MS). Limits of quantification were below 5ngL−1 for water (except for fluroxypyr and iprodion) and ranged between 0.1ngg−1 and 57.7ngg−1 for sediments and regarding fish, were below 1ngg−1 for 8 molecules and were determined between 5 and 49ngg−1 for the 5 other compounds. This method was finally used as a new routine practice for environmental research.
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