Publications by authors named "Noelia Salgueiro-Gonzalez"

20 Publications

  • Page 1 of 1

Changes in drug use in European cities during early COVID-19 lockdowns - A snapshot from wastewater analysis.

Environ Int 2021 08 26;153:106540. Epub 2021 Mar 26.

Environmental and Public Health Analytical Chemistry, Research Institute for Pesticides and Water, University Jaume I, Castellón, Spain; Institute for Biodiversity and Ecosystem Dynamics, University of Amsterdam, the Netherlands. Electronic address:

The COVID-19 outbreak has forced countries to introduce severe restrictive measures to contain its spread. In particular, physical distancing and restriction of movement have had important consequences on human behaviour and potentially also on illicit drug use and supply. These changes can be associated with additional risks for users, in particular due to reduced access to prevention and harm reduction activities. Furthermore, there have been limitations in the amount of data about drug use which can be collected due to restrictions. To goal of this study was to obtain information about potential changes in illicit drug use impacted by COVID-19 restrictions. Wastewater samples were collected in seven cities in the Netherlands, Belgium, Spain and Italy at the beginning of lockdowns (March-May 2020). Using previously established and validated methods, levels of amphetamine (AMP), methamphetamine (METH), MDMA, benzoylecgonine (BE, the main metabolite of cocaine) and 11-nor-9-carboxy-Δ-tetrahydrocannabinol (THC-COOH, main metabolite of tetrahydrocannabinol (THC)) were measured and compared with findings from previous years. Important differences in levels of consumed drugs were observed across the considered countries. Whilst for some substances and locations, marked decreases in consumption could be observed (e.g., 50% decrease in MDMA levels compared to previous years). In some cases, similar or even higher levels compared to previous years could be found. Changes in weekly patterns were also observed, however these were not clearly defined for all locations and/or substances. Findings confirm that the current situation is highly heterogeneous and that it remains very difficult to explain and/or predict the effect that the present pandemic has on illicit drug use and availability. However, given the current difficulty in obtaining data due to restrictions, wastewater analysis can provide relevant information about the situation at the local level, which would be hard to obtain otherwise.
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http://dx.doi.org/10.1016/j.envint.2021.106540DOI Listing
http://www.ncbi.nlm.nih.gov/pmc/articles/PMC7997602PMC
August 2021

New psychoactive substances in several European populations assessed by wastewater-based epidemiology.

Water Res 2021 May 27;195:116983. Epub 2021 Feb 27.

Istituto di Ricerche Farmacologiche Mario Negri IRCCS, Department of Environmental Sciences, Via Mario Negri 2, 20156, Milan, Italy.

Wastewater-based epidemiology (WBE) can be a useful tool to face some of the existing challenges in monitoring the use of new psychoactive substances (NPS), as it can provide objective and updated information. This Europe-wide study aimed to verify the suitability of WBE for investigating the use of NPS. Selected NPS were monitored in urban wastewater by high performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS). The main classical illicit drugs were monitored in the same samples to compare their levels with those of NPS. Raw composite wastewater samples were collected in 2016 and 2017 in 14 European countries (22 cities) following best practice sampling protocols. Methcathinone was most frequent (>65% of the cities), followed by mephedrone (>25% of the cities), and only mephedrone, methcathinone and methylone were found in both years. This study depicts the use of NPS in Europe, confirming that it is much lower than the use of classical drugs. WBE proved able to assess the qualitative and quantitative spatial and temporal profiles of NPS use. The results show the changeable nature of the NPS market and the importance of large WBE monitoring campaigns for selected priority NPS. WBE is valuable for complementing epidemiological studies to follow rapidly changing profiles of use of drugs.
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http://dx.doi.org/10.1016/j.watres.2021.116983DOI Listing
May 2021

International snapshot of new psychoactive substance use: Case study of eight countries over the 2019/2020 new year period.

Water Res 2021 Apr 3;193:116891. Epub 2021 Feb 3.

Health and Biomedical Innovation, UniSA: Clinical and Health Sciences, University of South Australia, Adelaide 5001, South Australia, Australia. Electronic address:

There is considerable concern around the use of new psychoactive substances (NPS), but still little is known about how much they are really consumed. Analysis by forensics laboratories of seized drugs and post-mortem samples as well as hospital emergency rooms are the first line of identifying both 'new' NPS and those that are most dangerous to the community. However, NPS are not necessarily all seized by law enforcement agencies and only substances that contribute to fatalities or serious afflictions are recorded in post-mortem and emergency room samples. To gain a better insight into which NPS are most prevalent within a community, complementary data sources are required. In this work, influent wastewater was analysed from 14 sites in eight countries for a variety of NPS. All samples were collected over the 2019/2020 New Year period, a time which is characterized by celebrations and parties and therefore a time when more NPS may be consumed. Samples were extracted in the country of origin following a validated protocol and shipped to Australia for final analysis using two different mass spectrometric strategies. In total, more than 200 were monitored of which 16 substances were found, with geographical differences seen. This case study is the most comprehensive wastewater analysis study ever carried out for the identification of NPS and provides a starting point for future, ongoing monitoring of these substances.
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http://dx.doi.org/10.1016/j.watres.2021.116891DOI Listing
April 2021

Identification of contaminants of emerging concern with potential environmental risk in Spanish continental shelf sediments.

Sci Total Environ 2020 Nov 30;742:140505. Epub 2020 Jun 30.

Instituto Español de Oceanografía, Centro Oceanográfico de Murcia, C/Varadero 1, 30740 San Pedro del Pinatar, Murcia, Spain.

The distribution of per- and polyfluoroalkyl substances (PFAS), alkylphenols, organotin compounds, phthalates, alkylated polycyclic aromatic hydrocarbons, current-use pesticides (CUPs) and personal care products (PCPs) was characterized in 29 surface sediments from two Spanish Iberian continental shelf areas (14 on the Atlantic and 15 on the Mediterranean coasts). Concretely, 115 organic contaminants were determined and a specific methodology was used for each contaminant group, including contaminants of emerging concern (CECs) and traditional ones, such as polycyclic aromatic hydrocarbons (PAHs), polychlorinated biphenyls (PCBs) and organochlorinated pesticides (OCPs). PAHs, alkylated PAHs, alkylphenols and phthalates were found in all samples, showing mean concentrations per group higher than 20 ng/g (16-4974 ng/g d.w.) in the subregions under consideration (Galician, Cantabrian, Levantine-Balearic and Strait-Alboran). CUPs and PCPs were found in the majority of samples at very low concentrations of ng/g (1.4-46.8 ng/g d.w.), whereas organotins and PFAS were found principally in sediments from the Mediterranean subregions (2.5-3.9 ng/g d.w.). Different distribution patterns were observed for the contaminant groups and subregions under consideration as a consequence of the diverse predominant sources (industrial, urban, transport and agricultural activities) and environmental behavior (mainly hydrophobicity and persistence). Risk assessment confirmed the impact of phthalates, alkylphenols, PAHs and PCBs on Atlantic ecosystems and of alkylphenols, chlorpyrifos, phthalates, TBT, PAHs, OCPs and PCBs on the Mediterranean ones. Furthermore, the presence of CUPs, PCPs and PFAS in sediments from the Spanish continental shelf located between 2 and 31 km from the coast suggested that those contaminants may also provoke adverse effects on coastal marine ecosystems between their sources and their depositional areas. CAPSULE: Alkylphenols, phthalates and organotins may provoke adverse effects on Spanish coastal marine ecosystems from their sources to the sediment depositional areas.
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http://dx.doi.org/10.1016/j.scitotenv.2020.140505DOI Listing
November 2020

Wastewater-based epidemiology to assess the occurrence of new psychoactive substances and alcohol consumption in Slovakia.

Ecotoxicol Environ Saf 2020 Sep 23;200:110762. Epub 2020 May 23.

Institute of Chemical and Environmental Engineering, Faculty of Chemical and Food Technology, Slovak University of Technology, Radlinského 9, 812 37, Bratislava, Slovakia. Electronic address:

Consumption of alcohol and new psychoactive substances (NPS) in a population or during special events (music festivals) is usually monitored through individual questionnaires, forensic and toxicological data, and drug seizures. However, consumption estimates have some biases due mostly to the unknown composition of drug pills for NPS and stockpiling for alcohol. The aim of this study was to evaluate for the first time the real use of alcohol and the occurrence of NPS in Slovakia by wastewater-based epidemiology (WBE). Urban wastewater samples were collected from nine Slovak cities over two years (2017-2018) and during three music festivals. The study included about 20% of the Slovak population and 50 000 festival attendees. The urinary alcohol biomarker ethyl sulfate (EtS) and thirty NPS were analyzed by liquid chromatography tandem mass spectrometry (LC - MS/MS). EtS concentrations were used for estimating the per capita alcohol consumption in each city. The average alcohol consumption in the selected cities and festivals in 2017-2018 ranged between 7 and 126 L/day/1000 inhabitants and increased during the weekends and music festivals. Five NPS belonging to the classes of synthetic cathinones (mephedrone, methcathinone, buphedrone and pentedrone) and phenethylamines (25-iP-NBoMe) were found in the low ng/L range. Methcathinone was the most frequently detected NPS, while the highest normalized mass load corresponded to mephedrone (3.1 mg/day/1000 inhabitants). Wastewater-based epidemiology can provide timely information on alcohol consumption and NPS occurrence at the community level that is complementary to epidemiology-based monitoring techniques (e.g. population surveys, police seizures, sales statistics).
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http://dx.doi.org/10.1016/j.ecoenv.2020.110762DOI Listing
September 2020

Methamphetamine exposure modulated oxidative status and altered the reproductive output in Daphnia magna.

Sci Total Environ 2020 Jun 10;721:137728. Epub 2020 Mar 10.

Department of Environmental Science and Policy, University of Milan, via Celoria 26, I-20133 Milan, Italy.

Methamphetamine (METH) is a central nervous system stimulant drug whose use has increased in the last few years worldwide. After the ingestion of even a single dose, METH is excreted by the organism and enters the aquatic ecosystems, whereby concentrations up to hundreds of ng/L were measured in both sewage and surface waters. Although the environmental concentrations are currently quite low, the high biological activity of METH might cause adverse effects towards non-target organisms. However, to date the information on METH toxicity towards aquatic organisms is limited. Thus, the present study aimed at investigating biochemical and behavioral effects induced by METH exposure towards the Cladoceran Daphnia magna. A 21-days exposure to two environmental concentrations of METH (50 ng/L and 500 ng/L) was performed. At selected time points (7, 14 and 21 days) the amount of pro-oxidant molecules, the activity of antioxidant enzymes (SOD, CAT, GPx) and levels of lipid peroxidation (LPO) were measured as oxidative stress-related endpoints. Changes in swimming activity and reproductive output were assessed as behavioral endpoints. METH exposure affected the oxidative status of D. magna specimens at both tested concentrations, although no oxidative damage occurred. Although METH did not modulate the swimming activity of D. magna, a significant, positive effect on reproductive output, in terms of number of offspring was found. Our results showed that low concentrations of METH might represent a threat for D. magna, affecting the health status of this aquatic species at different level of biological organization.
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http://dx.doi.org/10.1016/j.scitotenv.2020.137728DOI Listing
June 2020

Effects of new generation progestins, including as mixtures and in combination with other classes of steroid hormones, on zebrafish early life stages.

Sci Total Environ 2020 Mar 23;709:136262. Epub 2019 Dec 23.

University of Applied Sciences and Arts Northwestern Switzerland, School of Life Sciences, Hofackerstrasse 30, CH-4132 Muttenz, Switzerland; Swiss Federal Institute of Technology (ETH Zürich), Institute of Biogeochemistry and Pollution Dynamics, Department of Environmental Systems Science, CH-8092 Zürich, Switzerland. Electronic address:

Fish are exposed to progestins and steroid mixtures in contaminated waters but the ecotoxicological implications are not sufficiently known. Here we analyze effects of the new generation progestin dienogest (DNG) followed by investigating effects of mixtures of new generation progestins containing DNG, cyproterone acetate and drospirenone and the hormone progesterone. Furthermore, effects of this mixture were studied after adding 17β-estradiol (E2) and clobetasol propionate (CLO) in zebrafish embryos and larvae at concentrations between 0.01 and 10 μg/L. DNG showed only very minor transcriptional alterations among the 24 assessed genes with downregulation of the fshb transcript only. The progestin mixture caused weak induction of the lhb, cyp2k22 and sult2st3 transcripts. Addition of E2 to the mixture caused strong induction vtg1, cyp19b, esr1 and lhb, as well as downregulation of fshb from 0.01 μg/L onwards. Besides altering the same transcripts, addition of CLO altered glucocorticoid regulated genes mmp-9, mmp-13, g6pca, fkbp5 and irg1l. While each steroid class exhibited its specific activity independently in the mixture, sult2st3 and cyp2k22 were regulated by both E2 and CLO. Furthermore, CLO alone and in mixtures decreased spontaneous muscle contractions, increased heartrate and induced edema. Our study highlights the prominent effects of E2 and CLO in environmental steroid mixtures, while new generation progestins show relatively low activity.
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http://dx.doi.org/10.1016/j.scitotenv.2019.136262DOI Listing
March 2020

Physiological and Transcriptional Effects of Mixtures of Environmental Estrogens, Androgens, Progestins, and Glucocorticoids in Zebrafish.

Environ Sci Technol 2020 01 2;54(2):1092-1101. Epub 2020 Jan 2.

School of Life Sciences , University of Applied Sciences and Arts Northwestern Switzerland , Hofackerstrasse 30 , CH-4132 Muttenz , Switzerland.

Fishes are exposed to mixtures of different classes of steroids, but ecotoxicological implications are not sufficiently known. Here, we systematically analyze effects of different combinations of steroid mixtures in zebrafish embryos to assess their joint activities on physiology and transcriptional alterations of steroid-specific target genes at 96 and 120 h post fertilization. In binary mixtures of clobetasol propionate (CLO) with estradiol (E2) or androstenedione (A4), each steroid exhibited its own expression profile. This was also the case in mixtures of 5-, 8-, and 13-different classes of steroids in exposure concentrations of 10-10,000 ng/L. The transcriptional expression of most genes in different mixtures was steroid-specific except for genes encoding aromatase (), sulfotransferase (), and that were induced by androgens, progestins, and glucocorticoids. Marked alterations occurred for in binary mixtures of CLO + E2 and CLO + A4. Glucocorticoids increased the heart rate and muscle contractions. In mixtures containing estrogens, induction of the transcript occurred at 10 ng/L and from the anticoagulation system at 100 ng/L. Our study demonstrates that steroids can act independently in mixtures; the sum of individual steroid profiles is expressed. However, some genes, including , , and , are regulated by several steroids. This joint effect on different pathways may be of concern for fish development.
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http://dx.doi.org/10.1021/acs.est.9b05834DOI Listing
January 2020

Spatio-temporal assessment of illicit drug use at large scale: evidence from 7 years of international wastewater monitoring.

Addiction 2020 01 23;115(1):109-120. Epub 2019 Oct 23.

Faculty of Fisheries and Protection of Waters, University of South Bohemia in Ceske Budejovice, Zatisi, Czech Republic.

Background And Aims: Wastewater-based epidemiology is an additional indicator of drug use that is gaining reliability to complement the current established panel of indicators. The aims of this study were to: (i) assess spatial and temporal trends of population-normalized mass loads of benzoylecgonine, amphetamine, methamphetamine and 3,4-methylenedioxymethamphetamine (MDMA) in raw wastewater over 7 years (2011-17); (ii) address overall drug use by estimating the average number of combined doses consumed per day in each city; and (iii) compare these with existing prevalence and seizure data.

Design: Analysis of daily raw wastewater composite samples collected over 1 week per year from 2011 to 2017.

Setting And Participants: Catchment areas of 143 wastewater treatment plants in 120 cities in 37 countries.

Measurements: Parent substances (amphetamine, methamphetamine and MDMA) and the metabolites of cocaine (benzoylecgonine) and of Δ -tetrahydrocannabinol (11-nor-9-carboxy-Δ -tetrahydrocannabinol) were measured in wastewater using liquid chromatography-tandem mass spectrometry. Daily mass loads (mg/day) were normalized to catchment population (mg/1000 people/day) and converted to the number of combined doses consumed per day. Spatial differences were assessed world-wide, and temporal trends were discerned at European level by comparing 2011-13 drug loads versus 2014-17 loads.

Findings: Benzoylecgonine was the stimulant metabolite detected at higher loads in southern and western Europe, and amphetamine, MDMA and methamphetamine in East and North-Central Europe. In other continents, methamphetamine showed the highest levels in the United States and Australia and benzoylecgonine in South America. During the reporting period, benzoylecgonine loads increased in general across Europe, amphetamine and methamphetamine levels fluctuated and MDMA underwent an intermittent upsurge.

Conclusions: The analysis of wastewater to quantify drug loads provides near real-time drug use estimates that globally correspond to prevalence and seizure data.
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http://dx.doi.org/10.1111/add.14767DOI Listing
http://www.ncbi.nlm.nih.gov/pmc/articles/PMC6973045PMC
January 2020

Drug Use by Music Festival Attendees: A Novel Triangulation Approach Using Self-Reported Data and Test Results of Oral Fluid and Pooled Urine Samples.

Subst Use Misuse 2019 9;54(14):2317-2327. Epub 2019 Aug 9.

Istituto di Ricerche Farmacologiche Mario Negri IRCCS, Milan, Italy.

Self-reported data are commonly used when investigating illicit substance use. However, self-reports have well-known limitations such as limited recall and socially desirable responding. Mislabeling or adulteration of drugs on the illicit market may also cause incorrect reporting. We aimed to examine what could be gained in terms of illicit drug use findings among music festival attendees when including biological sample test results in the assessment. We included 651 attendees at three music festivals in Norway from June to August 2016. Self-reported drug use was recorded using questionnaires, and samples of oral fluid were analyzed to detect use of illicit drugs. In addition, we analyzed samples of pooled urine from portable toilets at each festival. All methods identified cannabis, MDMA, and cocaine as the most commonly used drugs. Overall, 6.6% of respondents reported use of illicit substances during the previous 48 hours. Oral fluid testing identified a larger number of drug users as 12.6% tested positive for illicit drugs. In oral fluid testing, we identified ketamine and three new psychoactive substances (NPS) that had not been reported on the questionnaire. In pooled urine testing, we identified amphetamine and three additional NPS that were neither reported used nor found in oral fluid samples. Drug testing of biological samples proved to be an important supplement to self-reports as a larger number of illicit substances could be detected.
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http://dx.doi.org/10.1080/10826084.2019.1646285DOI Listing
May 2020

Polyethylene microplastics do not increase bioaccumulation or toxicity of nonylphenol and 4-MBC to marine zooplankton.

Sci Total Environ 2019 Nov 8;692:1-9. Epub 2019 Jul 8.

Department of Analytical Chemistry, Nutrition and Food Science, IIAA-Institute for Food Analysis and Research, Universidade de Santiago de Compostela, 15782 Santiago de Compostela, Galicia, Spain.

Global production of synthetic polymers, led by polyethylene (PE), rose steadily in the last decades, and marine ecosystems are considered as a global sink. Although PE is not biodegradable, in coastal areas it fragments into microplastics (MP) readily taken up by biota, and have been postulated as vectors of hydrophobic chemicals to marine organisms. We have tested this hypothesis using two organisms representative of the marine plankton, the holoplanktonic copepod Acartia clausi, and the meroplanktonic larva of the Paracentrotus lividus sea-urchin, and two model chemicals with similar hydrophobic properties, the 4-n-Nonylphenol and the 4-Methylbenzylidene-camphor used as plastic additive and UV filter in cosmetics. Both test species actively ingested the MP particles. However, the presence of MP never increased the bioaccumulation of neither model chemicals, nor their toxicity to the exposed organisms. Bioaccumulation was a linear function of waterborne chemical disregarding the level of MP. Toxicity, assessed by the threshold (EC) and median (EC) effect levels, was either independent of the level of MP or even in some instances significantly decreased in the presence of MPs. These consistent results challenge the assumption that MP act as vectors of hydrophobic chemicals to planktonic marine organisms.
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http://dx.doi.org/10.1016/j.scitotenv.2019.07.106DOI Listing
November 2019

Flexible high resolution-mass spectrometry approach for screening new psychoactive substances in urban wastewater.

Sci Total Environ 2019 Nov 26;689:679-690. Epub 2019 Jun 26.

Istituto di Ricerche Farmacologiche Mario Negri - IRCCS, Department of Environmental Health Sciences, Via Giuseppe La Masa 19, 20156 Milan, Italy.

The number of new psychoactive substances (NPS) on the recreational drug market has increased rapidly in the last years, creating serious challenges for public health agencies and law enforcement authorities. Epidemiological surveys and forensic analyses to monitor the consumption of these substances face some limitations for investigating their use on a large scale in a shifting market. The aim of this work was to develop a comprehensive and flexible screening approach for assessing the presence of NPS in urban wastewater by liquid chromatography-high resolution mass spectrometry (LC-HRMS). Almost 200 substances were selected as "priority NPS" among those most frequently and recently reported by the Early Warning Systems (EWS) of different agencies and were included in the screening. Wastewater samples were collected from several cities all over Europe in 2016 and 2017, extracted using different solid-phase cartridges and analysed by LC-HRMS. The screening workflow comprised three successive analytical steps and compounds were identified and confirmed following specific criteria from the current guidelines. Thirteen NPS were identified at different confidence levels by using analytical standards or information from libraries and literature, and about half of them were phenethylamines. As far as we know, this is the first time that four of them (i.e. 3,4-dimethoxy-α-pyrrolidinovalerophenone, para-methoxyamphetamine, 2-phenethylamine and α-methyltryptamine) have been found in urban wastewater. The proposed screening approach was successfully applied in the largest NPS European wastewater monitoring, providing an innovative and easily adapted procedure for investigating NPS. In the light of current challenges and specific future research issues, this approach may complement epidemiological information and help in establishing measures for public health protection.
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http://dx.doi.org/10.1016/j.scitotenv.2019.06.336DOI Listing
November 2019

Biochemical and behavioral effects induced by cocaine exposure to Daphnia magna.

Sci Total Environ 2019 Nov 24;689:141-148. Epub 2019 Jun 24.

Department of Environmental Science and Policy, University of Milan, via Celoria 26, I-20133 Milan, Italy. Electronic address:

Illicit drugs and their metabolites have been identified as emerging aquatic pollutants. Cocaine (COC) is one of the most used illicit drug worldwide. After human consumption, COC enters the aquatic ecosystems, where it is commonly detected in ng L concentration range. Although a number of studies have shown that the exposure to environmental concentrations of COC can induce diverse biochemical, molecular and histological effects on aquatic organisms, the information of COC-induced behavioral alterations is scant. Thus, the present study aimed at exploring both biochemical and behavioral effects induced by the exposure to two environmental concentrations (50 ng L and 500 ng L) of COC on the freshwater cladoceran Daphnia magna. Specimens were exposed to selected COC concentrations for 21 days and the effects on the oxidative status, including the amount of reactive oxygen species and the activity of antioxidant (SOD, CAT and GPx) and detoxifying (GST) enzymes, and swimming activity were investigated after 7, 14 and 21 days of treatment, while effects on reproductive success was assessed after 21-days only.. Exposure to COC induced an overproduction of reactive oxygen species and a modulation of the activity of defense enzymes. Moreover, COC affected the swimming behavior and altered the reproductive success of treated specimens. Our results highlighted that environmental concentrations of COC can cause adverse effects at different levels of the biological hierarchy in a zooplanktonic species, confirming the potential threat due to this illicit drug for the aquatic community.
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http://dx.doi.org/10.1016/j.scitotenv.2019.06.383DOI Listing
November 2019

Simultaneous determination of new psychoactive substances and illicit drugs in sewage: Potential of micro-liquid chromatography tandem mass spectrometry in wastewater-based epidemiology.

J Chromatogr A 2019 Sep 30;1602:300-309. Epub 2019 May 30.

Research Institute for Pesticides and Water, University Jaume I, Avda. Sos Baynat S/N, E-12071 Castelló, Spain. Electronic address:

Wastewater-based epidemiology (WBE) can give valuable light on the extent and actual use of new psychoactive substances (NPS). In this work, a fully validated methodology for the simultaneous determination of illicit drugs and NPS in wastewater by solid-phase extraction followed by UHPLC-MS/MS has been developed. The small sample volume (5 mL) required for analysis is of high interest, especially when performing large sampling campaigns involving many locations of different geographical origin, as it has been performed in the past. The method was applied to wastewater samples from different European locations and permitted the simultaneous monitoring of conventional drugs and NPS. Cocaine, amphetamine, MDMA, methamphetamine and ketamine were found in all wastewater samples, and several NPS (dipentylone, butylone, mephedrone, methedrone and methylone) were observed in some of the samples monitored. It is noteworthy that dipentylone was detected in wastewater for the very first time. Furthermore, a detailed comparison of micro liquid chromatography (μLC) and UHPLC, both coupled to tandem mass spectrometry, in terms of sensitivity and reproducibility has been made for the first time in the application field of WBE. An average increase factor of 14 (mass normalized data) was observed in sensitivity for μLC-MS/MS. The overall method performance was also compared (un-normalized data), and an average increase sensitivity factor of 4.5 was observed for μLC-MS/MS. However, large deviations in retention time (up to 0.4 min) affected the reproducibility and robustness of the μLC-MS/MS method when it was applied to wastewater analysis. Although in this work μLC-MS/MS was strongly influenced by the amount of matrix loaded in the separation device, its enhanced sensitivity and promotion of green chemistry (faster analysis time and less solvent consumption) allow to expect improved future applications, especially when analytes are present at very low concentrations.
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http://dx.doi.org/10.1016/j.chroma.2019.05.051DOI Listing
September 2019

Glucocorticoid mixtures of fluticasone propionate, triamcinolone acetonide and clobetasol propionate induce additive effects in zebrafish embryos.

J Hazard Mater 2019 07 4;374:101-109. Epub 2019 Apr 4.

University of Applied Sciences and Arts Northwestern Switzerland, School of Life Sciences, Gründenstrasse 40, CH-4132 Muttenz, Switzerland; Swiss Federal Institute of Technology (ETH Zürich), Institute of Biogeochemistry and Pollution Dynamics, Department of Environmental Systems Science, CH-8092 Zürich, Switzerland. Electronic address:

Many synthetic glucocorticoids from medical applications occur in the aquatic environment. Whether they pose a risk for fish health is poorly known. Here we investigate effects of glucocorticoids fluticasone propionate (FLU) and triamcinolone acetonide (TRI) as single steroids and as ternary mixtures with clobetasol propionate (CLO) in zebrafish embryos. Exposure to FLU and TRI in a range of concentrations between 0.099 and 120.08 μg/L led to concentration-related decrease in muscle contractions and increase in heart rate at 0.98 and 1.05 μg/L, respectively, and higher. Genes encoding for proteins related to glucose metabolism (g6pca, pepck1), immune system regulation (fkbp5, irg1l, socs3, gilz) and matrix metalloproteinases mmp-9 and mmp-13 showed expressional alterations, as well as genes encoding for the progestin receptor (pgr) and corticosteroid dehydrogenase (hsd11b2). FLU accelerated hatching and led to embryotoxicity (immobilization and edema). Ternary mixtures (FLU + TRI + CLO) induced the same physiological and toxicological effects at concentrations of individual glucocorticoids of 11.1-16.37 μg/L and higher. Heart rate was increased in the mixture at concentrations as low as 0.0885-0.11 μg/L of each steroid. Glucocorticoids in mixtures showed additive activity; the fold-changes of transcripts of 19 target genes were additive. Together, our data show that glucocorticoids act additively and their joint activity may be of concern for developing fish in contaminated environments.
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http://dx.doi.org/10.1016/j.jhazmat.2019.04.023DOI Listing
July 2019

Environmental glucocorticoids corticosterone, betamethasone and flumethasone induce more potent physiological than transcriptional effects in zebrafish embryos.

Sci Total Environ 2019 Jul 28;672:183-191. Epub 2019 Mar 28.

University of Applied Sciences and Arts Northwestern Switzerland, School of Life Sciences, Langackerstrasse 30, CH -4132 Muttenz, Switzerland; Swiss Federal Institute of Technology (ETH Zürich), Institute of Biogeochemistry and Pollution Dynamics, Department of Environmental System Sciences, CH -8092 Zürich, Switzerland. Electronic address:

Many glucocorticoids occur in the aquatic environments but their adverse effects to fish are poorly known. Here we investigate effects of the natural glucocorticoid corticosterone and the synthetic glucocorticoids betamethasone and flumethasone in zebrafish embryos. Besides studying the effects of each steroid, we compared effects of natural with synthetic glucocorticoids, used as drugs. Exposure at concentrations of 1 μg/L and higher led to concentration-related decrease in spontaneous muscle contractions at 24 h post fertilization (hpf) and increase in heart rate at 48 hpf. Betamethasone showed a significant increase at 0.11 μg/L in heart rate. Corticosterone also accelerated hatching at 60 hpf at 0.085 μg/L. Transcription of up to 24 genes associated with different pathways showed alterations at 96 and 120 hpf for all glucocorticoids, although with low potency. Corticosterone caused transcriptional induction of interleukin-17, while betamethasone caused transcriptional down-regulation of the androgen receptor, aromatase and hsd11b2, indicating an effect on the sex hormone system. Furthermore, transcripts encoding proteins related to immune system regulation (irg1l, gilz) and fkbp5 were differentially expressed by corticosterone and betamethasone, while flumethasone caused only little effects, mainly alteration of the irg1l transcript. Our study shows that these glucocorticoids caused more potent physiological effects in early embryos than transcriptional alterations in hatched embryos, likely due to increased metabolism in later developmental stages. Thus, these glucocorticoids may be of concern for early stages of fish embryos in contaminated aquatic environments.
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http://dx.doi.org/10.1016/j.scitotenv.2019.03.426DOI Listing
July 2019

Ecotoxicological evaluation of the risk posed by bisphenol A, triclosan, and 4-nonylphenol in coastal waters using early life stages of marine organisms (Isochrysis galbana, Mytilus galloprovincialis, Paracentrotus lividus, and Acartia clausi).

Environ Pollut 2018 Jan 23;232:173-182. Epub 2017 Sep 23.

Estación de Ciencias Mariñas de Toralla (ECIMAT), Universidade de Vigo, Illa de Toralla, 36331 Vigo, Galicia, Spain; Departamento de Ecoloxía e Bioloxía Animal, Universidade de Vigo, Campus Lagoas-Marcosende, 36200 Vigo, Galicia, Spain. Electronic address:

This study assessed the environmental risk on coastal ecosystems posed by three phenolic compounds of special environmental and human health concern used in plastics and household products: bisphenol A (BPA), triclosan (TCS) and 4-nonylphenol (4-NP). These three chemicals are among the organic contaminants most frequently detected in wastewater. The most toxic compound tested was 4-NP, with 10% effective concentration at 11.1 μg L for Isochrysis galbana, 110.5 μg L for Mytilus galloprovincialis, 53.8 μg L for Paracentrotus lividus, and 29.0 μg L for Acartia clausi, followed by TCS (14.6 μg L for I. galbana, 149.8 μg L for M. galloprovincialis, 129.9 μg L for P. lividus, and 64.8 μg L for A. clausi). For all species tested, BPA was the less toxic chemical, with toxicity thresholds ranging between 400 and 1200 μg L except for A. clausi nauplii (186 μg L). The relatively narrow range of variation in toxicity considering the broad physiological differences among the biological models used point at non-selective mechanisms of toxicity for these aromatic organics. Microalgae, the main primary producers in pelagic ecosystems, showed particularly high susceptibility to the chemicals tested. When the toxicity thresholds experimentally obtained were compared to the maximum environmental concentrations reported in coastal waters, the risk quotients obtained correspond to very low or low risk for BPA and TCS, and from low to high for 4-NP.
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http://dx.doi.org/10.1016/j.envpol.2017.09.031DOI Listing
January 2018

Benzoylecgonine exposure induced oxidative stress and altered swimming behavior and reproduction in Daphnia magna.

Environ Pollut 2018 Jan 18;232:236-244. Epub 2017 Sep 18.

Department of Environmental Science and Policy, University of Milan, via Celoria 2, I-20133 Milan, Italy.

Several monitoring studies have shown that benzoylecgonine (BE) is the main illicit drug residue commonly measured in the aquatic system worldwide. Few studies have investigated the potential toxicity of this molecule towards invertebrate and vertebrate aquatic non-target organisms focusing on effects at low levels of the biological organization, but no one has assessed the consequences at higher ones. Thus, the present study was aimed at investigating the toxicity of a 48-h exposure to two concentrations of BE, similar to those found in aquatic ecosystems (0.5 μg/L and 1.0 μg/L), on the cladoceran Daphnia magna at different levels of the ecological hierarchy. We relied on a multi-level approach focusing on the effects at biochemical/biomolecular (biomarkers), individual (swimming activity) and population (reproduction) levels. We measured the amount of reactive oxygen species and of the activity of antioxidant (SOD, CAT, and GPx) and detoxifying (GST) enzymes to assess if BE exposure can alter the oxidative status of D. magna specimens, while the lipid peroxidation (TBARS) was measured as a marker of oxidative damage. Moreover, we also measured the acetylcholinesterase (AChE) activity because it is strictly related to behavioral changes in aquatic organisms. Changes in swimming behavior were investigated by a video tracking analysis, while the consequences on reproduction were assessed by a chronic toxicity test. Our results showed that BE concentrations similar to those found in aquatic ecosystems induced oxidative stress and inhibited AChE activity, affecting swimming behavior and the reproduction of Daphnia magna individuals.
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http://dx.doi.org/10.1016/j.envpol.2017.09.038DOI Listing
January 2018

A single-step pesticide extraction and clean-up multi-residue analytical method by selective pressurized liquid extraction followed by on-line solid phase extraction and ultra-high-performance liquid chromatography-tandem mass spectrometry for complex matrices.

J Chromatogr A 2016 Jun 11;1452:10-7. Epub 2016 May 11.

IAREN-Water Institute of the Northern Region, Rua Dr. Eduardo Torres 229, 4450-113 Matosinhos, Portugal. Electronic address:

Pesticides, a group of compounds linked to human activity, may, when in toxic levels, have a profound effect on water quality, and hence result in adverse consequences to aquatic life and ultimately to human health. Analytical challenges arise when successfully trying to determine these levels in environmental complex matrices. Therefore, fast, simple, sensitive and selective analytical methodologies for multi-residue determination of pesticides (atrazine, azoxystrobin, bentazon, λ-cyhalothrin, penoxsulam and terbuthylazine) in sediment, macrophytes (algae and aquatic plants) and aquatic animals were developed and validated. The established methods were matrix-dependent and were based on Selective Pressurized Liquid Extraction (SPLE) followed by on-line Solid Phase Extraction and Ultra Performance Liquid Chromatography-tandem Mass Spectrometry (on-line SPE-UPLC-ESI-MS/MS). This cutting-edge research methodology uses a small amount of sample, is time saving and reduces the use of organic solvents in compliance with Green Chemistry principles. The analytical features were adequate for all compounds in all studied matrices. The established methodology was applied on real marine samples and no pesticide concentrations above their respective method quantification limits were measured in sediments or aquatic plants. However, terbuthylazine was found in the macroalgae Ulva spp. (108ngg(-1)dw) and all the prospected pesticides were measured above their respective method quantification limits in the bivalve Scrobicularia plana (atrazine: 48ngg(-1)dw, azoxystrobin: 64ngg(-1)dw, bentazon: 33ngg(-1)dw, λ-cyhalothrin: 2531ngg(-1)dw, penoxsulam: 50ngg(-1)dw, and terbuthylazine: 44ngg(-1)dw).
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http://dx.doi.org/10.1016/j.chroma.2016.05.036DOI Listing
June 2016

Bioaccumulation of 4-nonylphenol and effects on biomarkers, acetylcholinesterase, glutathione-S-transferase and glutathione peroxidase, in Mytilus galloprovincialis mussel gilla.

Environ Pollut 2015 May 25;200:133-9. Epub 2015 Feb 25.

ECIMAT, Universidade de Vigo, Illa de Toralla s.n., 36331 Vigo, Galicia, Spain.

Wild marine mussels, Mytilus galloprovincialis showed a moderate bioaccumulation ability when exposed to waterborne 4-nonylphenol (4-NP), with a bioconcentration factor (BCF) of 6850 L Kg(-1) (dry weight). Kinetic and concentration-response experiments were performed and three enzymatic biomarkers in mussel gills were measured: Glutathione S-transferase (GST), glutathione peroxidase (GPx) and acetylcholinesterase (AChE). Exposure of mussels to environmentally relevant concentrations (25-100 μg L(-1)) of 4-nonylphenol significantly inhibited the AChE activity and induced the GST and GPx activities. GST induction was dose dependent whilst GPx activity showed a less consistent pattern, but in both cases the induction remained after a 10 d depuration period. Mussels seem capable of eliminating 4-NP from their tissues through a mechanism involving GST induction.
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http://dx.doi.org/10.1016/j.envpol.2015.02.012DOI Listing
May 2015