Publications by authors named "Lubertus Bijlsma"

56 Publications

Ecological risk assessment of pesticides in the Mijares River (eastern Spain) impacted by citrus production using wide-scope screening and target quantitative analysis.

J Hazard Mater 2021 Jun 2;412:125277. Epub 2021 Feb 2.

IMDEA Water Institute, Science and Technology Campus of the University of Alcalá, Avenida Punto Com 2, Alcalá de Henares, Madrid 28805, Spain; Cavanilles Institute of Biodiversity and Evolutionary Biology, University of Valencia, c/ Catedrático José Beltrán 2, Paterna, Valencia 46980, Spain.

The widespread use of pesticides, especially in agricultural areas, makes necessary to control their presence in surrounding surface waters. The current study was designed to investigate the occurrence and ecological risks of pesticides and their transformation products in a Mediterranean river basin impacted by citrus agricultural production. Nineteen sites were monitored in three campaigns distributed over three different seasons. After a qualitative screening, 24 compounds was selected for subsequent quantitative analysis. As expected, the lower section of the river was most contaminated, with total concentration >5 µg/L in two sites near to the discharge area of wastewater treatment plants. The highest concentrations were found in September, after agricultural applications and when the river flow is reduced. Ecological risks were calculated using two mixture toxicity approaches (Toxic Unit and multi-substance Potentially Affected Fraction), which revealed high acute and chronic risks of imidacloprid to invertebrates, moderate-to-high risks of diuron, simazine and 2,4-D for primary producers, and moderate-to-high risks of thiabendazole for invertebrates and fish. This study shows that intensive agricultural production and the discharge of wastewater effluents containing pesticide residues from post-harvest citrus processing plants are threatening freshwater biodiversity. Further actions are recommended to control pesticide use and to reduce emissions.
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http://dx.doi.org/10.1016/j.jhazmat.2021.125277DOI Listing
June 2021

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

Environ Int 2021 Mar 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
March 2021

Use of ion mobility-high resolution mass spectrometry in metabolomics studies to provide near MS/MS quality data in a single injection.

J Mass Spectrom 2021 Mar 10;56(5):e4718. Epub 2021 Mar 10.

Analytical Chemistry and Public Health, Research Institute for Pesticides and Water (IUPA). Avda. Sos Baynat, s/n. University Jaume I, Castellón, Spain.

The use of ion mobility separations (IMSs) in metabolomics approaches has started to be deeply explored in the last years. In this work, the use of liquid chromatography (LC) coupled to IMS-quadrupole time-of-flight mass spectrometry (QTOF MS) has been evaluated in a metabolomics experiments using single injection of the samples. IMS has allowed obtaining cleaner fragmentation spectra, of nearly tandem MS quality, in data-independent acquisition mode. This is much useful in this research area as a second injection, generally applied in LC-QTOF MS workflows to obtain tandem mass spectra, is not necessary, saving time and evading possible compound degradation. As a case study, the smoke produced after combustion of herbal blends used to spray synthetic cannabinoids has been selected as study matrix. The smoke components were trapped in carbon cartridges, desorbed and analyzed by LC-IMS-QTOF MS using different separation mechanisms (reversed phase and HILIC) and acquiring in both positive and negative mode to widen the chemical domain. Partial Least Squares-Discriminant Analysis highlighted several compounds, and ratio between N-Isopropyl-3-(isoquinolinyl)-2-propen-1-amine and quinoline allowed differentiating between tobacco and herbal products. These two compounds were tentatively identified using the cleaner fragmentation spectra from a single injection in the IMS-QTOF MS, with additional confidence obtained by retention time (Rt) and collisional cross section (CCS) prediction using artificial neural networks. Data from this work show that LC-IMS-QTOF is an efficient technique in untargeted metabolomics, avoiding re-injection of the samples for elucidation purposes. In addition, the prediction models for Rt and CCS resulted of help in the elucidation process of potential biomarkers.
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http://dx.doi.org/10.1002/jms.4718DOI Listing
March 2021

The embodiment of wastewater data for the estimation of illicit drug consumption in Spain.

Sci Total Environ 2021 Jun 26;772:144794. Epub 2021 Jan 26.

Department of Analytical Chemistry, Nutrition and Food Sciences, Institute of Research in Chemical and Biological Analysis (IAQBUS), Universidade de Santiago de Compostela, Santiago de Compostela, Spain. Electronic address:

Data obtained from wastewater analysis can provide rapid and complementary insights in illicit drug consumption at community level. Within Europe, Spain is an important country of transit of both cocaine and cannabis. The quantity of seized drugs and prevalence of their use rank Spain at the top of Europe. Hence, the implementation of a wastewater monitoring program at national level would help to get better understanding of spatial differences and trends in use of illicit drugs. In this study, a national wastewater campaign was performed for the first time to get more insight on the consumption of illicit drugs within Spain. The 13 Spanish cities monitored cover approximately 6 million inhabitants (12.8% of the Spanish population). Untreated wastewater samples were analyzed for urinary biomarkers of amphetamine, methamphetamine, MDMA, cocaine, and cannabis. In addition, weekend samples were monitored for 17 new psychoactive substances. Cannabis and cocaine are the most consumed drugs in Spain, but geographical variations showed, for instance, comparatively higher levels of methamphetamine in Barcelona and amphetamine in Bilbao, with about 1-fold higher consumption of these two substances in such metropolitan areas. For amphetamine, an enantiomeric profiling was performed in order to assure the results were due to consumption and not to illegal dumping of production residues. Furthermore, different correction factors for the excretion of cannabis were used to compare consumption estimations. All wastewater results were compared with previously reported data, national seizure data and general population survey data, were a reasonable agreement was found. Daily and yearly drug consumption were extrapolated to the entire Spanish population with due precautions because of the uncertainty associated. These data was further used to estimate the retail drug market, where for instance cocaine illicit consumption alone was calculated to contribute to 0.2-0.5% of the Spanish gross domestic product (ca. 3000-6000 million Euro/year).
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http://dx.doi.org/10.1016/j.scitotenv.2020.144794DOI Listing
June 2021

Isotope pattern deconvolution as a successful alternative to calibration curve for application in wastewater-based epidemiology.

Anal Bioanal Chem 2021 May 17;413(13):3433-3442. Epub 2021 Mar 17.

Research Institute for Pesticides and Water, Universitat Jaume I, Avda. Sos Baynat, s/n, 12071, Castelló, Spain.

An isotope pattern deconvolution (IPD) quantification method has been applied for the determination of five substances (amphetamine, benzoylecgonine, cocaine, methamphetamine and MDMA) in wastewater for the application in wastewater-based epidemiology (WBE). A previously validated method that used a calibration curve for quantification was modified to apply IPD. The two approaches were compared in terms of analytical uncertainty in recovery studies of quality control samples, i.e. six wastewater samples from different geographical origins spiked at two concentration levels. Both methods were reliable as they passed (z-score < 2) in an interlaboratory exercise. After 60 individual determinations, IPD provided 11 results outside recovery limits (70-120%) while the previous method produced 31 adverse results. All mean values for IPD were accurate whereas 6 out of 10 results showed RSD values higher than 30% or recoveries outside limits when using the former method. Moreover, the calculated method bias for the latter doubles that of IPD, which, in turn, makes the combined uncertainty (u(c)) much higher. Consequently, a simple change of data treatment-IPD quantification methodology-resulted in a lower uncertainty of the estimated illicit drug concentration, one of the main steps contributing to the final uncertainty in the normalized daily drug consumption through WBE. The current study demonstrated that the employment of IPD can also be very interesting for future applications of WBE, especially when matrix effects are high, complicating accurate quantification. In addition, when a high number of samples and/or compounds need to be analysed, IPD is faster than calibration and, eventually, cost-effective when isotopically labelled internal standard is highly expensive.
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http://dx.doi.org/10.1007/s00216-021-03287-7DOI Listing
http://www.ncbi.nlm.nih.gov/pmc/articles/PMC7966919PMC
May 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

Improving Target and Suspect Screening High-Resolution Mass Spectrometry Workflows in Environmental Analysis by Ion Mobility Separation.

Environ Sci Technol 2020 12 19;54(23):15120-15131. Epub 2020 Nov 19.

Environmental and Public Health Analytical Chemistry, Research Institute for Pesticides and Water, University Jaume I, Avda. Sos Baynat s/n, E-12071 Castellón, Spain.

Currently, the most powerful approach to monitor organic micropollutants (OMPs) in environmental samples is the combination of target, suspect, and nontarget screening strategies using high-resolution mass spectrometry (HRMS). However, the high complexity of sample matrices and the huge number of OMPs potentially present in samples at low concentrations pose an analytical challenge. Ion mobility separation (IMS) combined with HRMS instruments (IMS-HRMS) introduces an additional analytical dimension, providing extra information, which facilitates the identification of OMPs. The collision cross-section (CCS) value provided by IMS is unaffected by the matrix or chromatographic separation. Consequently, the creation of CCS databases and the inclusion of ion mobility within identification criteria are of high interest for an enhanced and robust screening strategy. In this work, a CCS library for IMS-HRMS, which is online and freely available, was developed for 556 OMPs in both positive and negative ionization modes using electrospray ionization. The inclusion of ion mobility data in widely adopted confidence levels for identification in environmental reporting is discussed. Illustrative examples of OMPs found in environmental samples are presented to highlight the potential of IMS-HRMS and to demonstrate the additional value of CCS data in various screening strategies.
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http://dx.doi.org/10.1021/acs.est.0c05713DOI Listing
December 2020

Metabolism of N-ethylhexedrone and buphedrone: An in vivo study in mice using HPLC-MS/MS.

J Chromatogr B Analyt Technol Biomed Life Sci 2020 Nov 25;1159:122340. Epub 2020 Aug 25.

Faculdade de Farmácia, Universidade de Lisboa, Av. Prof. Gama Pinto, 1649-019 Lisboa, Portugal; iMed.ULisboa (Research Institute for Medicines), Faculdade de Farmácia, Universidade de Lisboa, Av. Prof. Gama Pinto, 1649-003 Lisboa, Portugal; IBET - Instituto de Biologia Experimental e Tecnológica, Apartado 12, 2780-901 Oeiras, Portugal.

N-ethylhexedrone (NEH) and buphedrone (BUPH) are synthetic drugs structurally related to natural cathinone. These synthetic cathinones (SC) are members of the heterogenous family of new psychoactive substances (NPS), which have caused major concern in scientific and forensic communities over the past years, due to their widespread consume. Thus, there is a constant need for monitoring the use of these new substances and gather knowledge on their metabolism and excretion profiles, in order to try to identify markers of NPS consumption. This study aimed at the identification and quantification of NEH, BUPH and selected phase I metabolites using HPLC-MS/MS. NEH, BUPH and some related metabolites were synthesized in-house and quantified in 24 h mice urine, following single dose administration of each drug (64 mg kg, i.p.). NEH and BUPH were quantified in mice urine at 58.3 ± 14.4 and 146.2 ± 14.9 µg mL, respectively. Similar metabolic pathways were observed for both drugs. Among the metabolites studied, the most excreted ones derived from N-dealkylation of either NEH or BUPH (at around 80 µg mL of urine). Other metabolites resulting from ketone reduction and ketone reduction combined with N-dealkylation or 4-aryl hydroxylation (detected for the first time in non-ring substituted SC) were also identified and quantified. Urine samples were screened using liquid chromatography-high resolution mass spectrometry and various phase II metabolites, including N-acetylated, glucuronides and dicarboxylic acid conjugates were tentatively identified, some of them for the first time. This work is a contribution to the identification of metabolites from SC that can become potential markers to estimate drug consumption.
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http://dx.doi.org/10.1016/j.jchromb.2020.122340DOI Listing
November 2020

Assessing alcohol consumption through wastewater-based epidemiology: Spain as a case study.

Drug Alcohol Depend 2020 10 19;215:108241. Epub 2020 Aug 19.

Water, Environmental, and Food Chemistry Unit (ENFOCHEM), Department of Environmental Chemistry, Institute of Environmental Assessment and Water Research (IDAEA-CSIC), Barcelona, Spain. Electronic address:

Background: In this study, an alternative and complementary method to those approaches currently used to estimate alcohol consumption by the population is described. This method, known as wastewater-based epidemiology (WBE), allows back-calculating the alcohol consumption rate in a given population from the concentrations of a selected biomarker measured in wastewater.

Methods: Composite (24-h) wastewater samples were collected at the inlet of 17 wastewater treatment plants located in 13 Spanish cities for seven consecutive days in 2018. The sampled area covered 12.8% of the Spanish population. Wastewater samples were analyzed to determine the concentration of ethyl sulfate, the biomarker used to back-calculate alcohol consumption.

Results: Alcohol consumption ranged from 4.5 to 46 mL/day/inhabitant. Differences in consumption were statistically significant among the investigated cities and between weekdays and weekends. WBE-derived estimates of alcohol consumption were comparable to those reported by its corresponding region in the Spanish National Health Survey in most cases. At the national level, comparable results were obtained between the WBE-derived annual consumption rate (5.7 ± 1.2 L ethanol per capita (aged 15+)) and that reported by the National Health Survey (4.7 L ethanol per capita (aged 15+)).

Conclusions: This is the largest WBE study carried out to date in Spain to estimate alcohol consumption rates. It confirms that this approach is useful for establishing spatial and temporal patterns of alcohol consumption, which could contribute to the development of health care management plans and policies. Contrary to established methods, it allows obtaining information in a fast and relatively economical way.
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http://dx.doi.org/10.1016/j.drugalcdep.2020.108241DOI Listing
October 2020

Occurrence and ecological risks of pharmaceuticals in a Mediterranean river in Eastern Spain.

Environ Int 2020 11 31;144:106004. Epub 2020 Jul 31.

Environmental and Public Health Analytical Chemistry, Research Institute for Pesticides and Water (IUPA), University Jaume I, Avda. Sos Baynat s/n, E-12071, Castellón, Spain. Electronic address:

Pharmaceuticals are biologically active molecules that may exert toxic effects to a wide range of aquatic organisms. They are considered contaminants of emerging concern due to their common presence in wastewaters and in the receiving surface waters, and the lack of specific regulations to monitor their environmental occurrence and risks. In this work, the environmental exposure and risks of pharmaceuticals have been studied in the Mijares River, Eastern Mediterranean coast (Spain). A total of 57 surface water samples from 19 sampling points were collected in three monitoring campaigns between June 2018 and February 2019. A list of 40 compounds was investigated using a quantitative target UHPLC-MS/MS method. In order to complement the data obtained, a wide-scope screening of pharmaceuticals and metabolites was also performed by UHPLC-HRMS. The ecological risks posed by the pharmaceutical mixtures were evaluated using species sensitivity distributions built with chronic toxicity data for aquatic organisms. In this study, up to 69 pharmaceuticals and 9 metabolites were identified, out of which 35 compounds were assessed using the quantitative method. The highest concentrations in water corresponded to acetaminophen, gabapentin, venlafaxine, valsartan, ciprofloxacin and diclofenac. The compounds that were found to exert the highest toxic pressure on the aquatic ecosystems were principally analgesic/anti-inflammatory drugs and antibiotics. These were: phenazone > azithromycin > diclofenac, and to a lower extent norfloxacin > ciprofloxacin > clarithromycin. The monitored pharmaceutical mixtures are expected to exert severe ecological risks in areas downstream of WWTP discharges, with the percentage of aquatic species affected ranging between 65% and 82% in 3 out of the 19 evaluated sites. In addition, five antibiotics were found to exceed antibiotic resistance thresholds, thus potentially contributing to resistance gene enrichment in environmental bacteria. This work illustrates the wide use and impact of pharmaceuticals in the area under study, and the vulnerability of surface waters if only conventional wastewater treatments are applied. Several compounds included in this study should be incorporated in future water monitoring programs to help in the development of future regulations, due to their potential risk to the aquatic environment.
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http://dx.doi.org/10.1016/j.envint.2020.106004DOI Listing
November 2020

Assessing population exposure to phthalate plasticizers in thirteen Spanish cities through the analysis of wastewater.

J Hazard Mater 2021 01 22;401:123272. Epub 2020 Jun 22.

Department of Analytical Chemistry, Institute of Research on Chemical and Biological Analysis (IAQBUS), Universidade de Santiago de Compostela, 15782 Santiago de Compostela, Spain.

Phthalates are widely used plasticizers that produce endocrine-disrupting disorders. Quantifying exposure is crucial to perform risk assessments and to develop proper health measures. Herein, a wastewater-based epidemiology approach has been applied to estimate human exposure to six of the mostly used phthalates within the Spanish population. Wastewater samples were collected over four weekdays from seventeen wastewater treatment plants serving thirteen cities and ca. 6 million people (12.8 % of the Spanish population). Phthalate metabolite loads in wastewater were transformed into metabolite concentrations in urine and into daily exposure levels to the parent phthalates. Considering all the sampled sites, population-weighted overall means of the estimated concentrations in urine varied between 0.7 ng/mL and 520 ng/mL. Very high levels, compared to human biomonitoring data, were estimated for monomethyl phthalate, metabolite of dimethyl phthalate. This, together with literature data pointing to other sources of this metabolite in sewage led to its exclusion for exposure assessments. For the remaining metabolites, estimated concentrations were closer to those found in urine. Their 4-days average exposure levels ranged from 2 to 1347 μg/(day∙inh), exceeding in some sites the daily exposure thresholds set for di-i-butyl phthalate and di-n-buthyl phthalate by the European Food Safety Authority.
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http://dx.doi.org/10.1016/j.jhazmat.2020.123272DOI Listing
January 2021

First nation-wide estimation of tobacco consumption in Spain using wastewater-based epidemiology.

Sci Total Environ 2020 Nov 20;741:140384. Epub 2020 Jun 20.

Department of Analytical Chemistry, Institute of Research on Chemical and Biological Analysis (IAQBUS), Universidade de Santiago de Compostela, 15782 Santiago de Compostela, Spain. Electronic address:

Wastewater-based epidemiology (WBE) has become a very useful tool to monitor a population's drug consumption or exposure to environmental and food contaminants. In this work, WBE has been applied to estimate tobacco consumption in seven Spanish regions. To this end, 24 h composite wastewater samples were taken daily for one week in 17 wastewater treatment plants, covering altogether a population of ca. 6 million inhabitants. The samples were treated by enzymatic deconjugation and the wastewater content of two human-specific nicotine metabolites (namely, cotinine and trans-3'-hydroxycotinine) was measured to estimate the daily consumption of nicotine. The population-weighted average nicotine consumption in the seven analyzed regions was 2.2 g/(day∙1000 inh.), without any daily pattern. This average estimated nicotine consumption value agreed with the value derived from official tobacco sales data. Differences in consumption among the seven studied regions were found, being Galicia, the region with the lowest rate, and the Basque Country and Catalonia those with the highest rates. However, no conclusive correlation was found between those values and the prevalence data taken from two different national surveys, nor sociodemographic and health data. This study demonstrates that this tool can complement other indicators in order to accurately assess tobacco consumption rates at regional and national levels and provides the most extensive application of the approach in the Spanish territory.
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http://dx.doi.org/10.1016/j.scitotenv.2020.140384DOI Listing
November 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

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

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

A Refined Nontarget Workflow for the Investigation of Metabolites through the Prioritization by in Silico Prediction Tools.

Anal Chem 2019 05 22;91(9):6321-6328. Epub 2019 Apr 22.

Research Institute for Pesticides and Water , University Jaume I , Avenida Sos Baynat s/n , E-12071 Castellón , Spain.

The application of nontargeted strategies based on high-resolution mass spectrometry (HRMS) directed toward the discovery of metabolites of known contaminants in fish is an interesting alternative to true nontarget screening. To reduce prolonged and costly laboratory experiments, recent advances in computing power have permitted the development of comprehensive knowledge-based software to predict the metabolic fate of chemicals. In addition, machine-based learning tools allow the prediction of chromatographic retention times (RT) or collision cross section (CCS) values when using ion mobility spectrometry (IMS). These tools can ease data evaluation and strengthen the confidence in the identification of compounds. The current work explores the capabilities of in silico prediction tools, refined by the use of RT and CCS prediction, to prioritize and facilitate nontarget liquid chromatography (LC)-IMS-HRMS data processing. The fate of the insecticide pirimiphos-methyl (PM) in farmed Atlantic salmon exposed to contaminated feed was used as a case study. The theoretical prediction of 60 potentially relevant biological PM metabolites permitted the prioritization of screening in different salmon tissues (liver, kidney, bile, muscle, and fat) of known and unknown PM metabolites. An average of 43 potential positives was found in the sample matrixes based on the accurate mass of protonated molecules (mass error ≤5 ppm). The application of different tolerance filters for RT (Δ ≤ 2 min) and CCS (Δ ≤ 6%) based on predicted values permitted us to reduce this number up to 66% of the features. Finally, five PM metabolites could be identified; two known metabolites (2-DAMP and N-desethyl PM) were confirmed with a standard, whereas three previously unknown metabolites (2-DAMP glucuronide, didesethyl PM, and hydroxy-2-DAMP glucuronide) were tentatively identified in different matrixes, allowing the first proposition of a metabolic pathway in fish.
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http://dx.doi.org/10.1021/acs.analchem.9b01218DOI Listing
May 2019

Investigating the appearance of new psychoactive substances in South Australia using wastewater and forensic data.

Drug Test Anal 2019 Feb 12;11(2):250-256. Epub 2018 Sep 12.

School of Pharmacy and Medical Sciences, University of South Australia, Adelaide, 5001, Australia.

New psychoactive substances (NPS) have increased in use and popularity worldwide. Wastewater analysis has been successfully applied to evaluate illicit drugs use within a population. However, for NPS, such an approach may be limited due to low doses of NPS combined with their ever-changing composition and usage. The dynamic nature of the NPS market means use may be opportunistic, infrequent, and with few users. Hence, the use of complementary information sources is recommended to improve the knowledge on NPS consumption. The aim of this study was to investigate the changing landscape of NPS use on a community scale by combining wastewater analysis and forensic toxicology. Forensic analysis provided specific information on NPS prevalence in post-mortem blood samples in Adelaide, South Australia over five years, while wastewater analysis showed community use over the same period. A qualitative liquid chromatography--high resolution mass spectrometry method was initially used to screen the wastewater samples. A total of 24 NPS were found: 6 in wastewater only, 13 in forensic post-mortem toxicology samples only, and 5 in both. As these results showed the presence of NPS, a targeted method was subsequently employed to quantify levels of these NPS in wastewater. Temporal trends were found in wastewater with distinct tendencies for synthetic cathinones visible over the period studied.
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http://dx.doi.org/10.1002/dta.2484DOI Listing
February 2019

[Wastewater-based epidemiology: applications towards the estimation of drugs of abuse consumption and public health in general. The Spanish network ESAR-Net].

Rev Esp Salud Publica 2018 Aug 20;92. Epub 2018 Aug 20.

Departamento de Química Analítica, Nutrición e Bromatoloxía, IIAA. Instituto de Investigacións e Análises Alimentarias. Universidade de Santiago de Compostela. Santiago de Compostela. España.

This manuscript introduces Wastewater-Based Epidemiology (WBE) and its potential in the assessment of diverse aspects related to public health. This methodology can provide data in a relatively short temporal and local scale (typically dialy-weekly at the municipal level) on consumption patterns of illicit drugs (e.g. cocaine or cannabis), licit substances of abuse (e.g. alcohol) by measuring their consumption biomarkers (i.e. the original unmetabolized substance or some of its metabolite) in wastewater. Besides discussing the fundaments, advantages and shortcomings of WBE, it reviews some of the main precedents at international level and most remarkable activities that have been taken place in this field in Spain. Finally, the Spanish Network of Wastewater-Based Epidemiology (ESAR-Net) as is presented. ESAR-Net is an Excellence Network that sums up the efforts of the most relevant Spanish researchers in the field of WBE, aiming to investigate future perspectives of this methodology and its impact on Public Health competences in Spain.
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August 2018

Development of a Retention Time Interpolation scale (RTi) for liquid chromatography coupled to mass spectrometry in both positive and negative ionization modes.

J Chromatogr A 2018 Sep 6;1568:101-107. Epub 2018 Jul 6.

Research Institute for Pesticides and Water, University Jaume I, Avda. Sos Baynat s/n, E-12071 Castellón, Spain. Electronic address:

The accuracy and sensitivity of high resolution mass spectrometry (HRMS) enables the identification of candidate compounds with the use of mass spectrometric databases among other tools. However, retention time (RT) data in identification workflows has been sparingly used since it could be strongly affected by matrix or chromatographic performance. Retention Time Interpolation scaling (RTi) strategies can provide a more robust and valuable information than RT, gaining more confidence in the identification of candidate compounds in comparison to an analytical standard. Up to our knowledge, no RTi has been developed for LC-HRMS systems providing information when acquiring in either positive or negative ionization modes. In this work, an RTi strategy was developed by means of the use of 16 isotopically labelled reference standards, which can be spiked into a real sample without resulting in possible false positives or negatives. For testing the RTi performance, a mixture of several reference standards, emulating suspect analytes, were used. RTi values for these compounds were calculated both in solvent and spiked in a real matrix to assess the effect of either chromatographic parameters or matrix in different scenarios. It has been demonstrated that the variation of injection volume, chromatographic gradient and initial percentage of organic solvent injected does not considerably affect RTi calculation. Column aging and solid support of the stationary phase of the column, however, showed strong effects on the elution of several test compounds. Yet, RTi permitted the correction of elution shifts of most compounds. Furthermore, RTi was tested in 47 different matrices from food, biological, animal feeding and environmental origin. The application of RTi in both positive and negative ionization modes showed in general satisfactory results for most matrices studied. The RTi developed can be used in future LC-HRMS screening analysis giving an additional parameter, which facilitates tedious processing tasks and gain more confidence in the identification of (non)-suspect analytes.
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http://dx.doi.org/10.1016/j.chroma.2018.07.030DOI Listing
September 2018

What about the herb? A new metabolomics approach for synthetic cannabinoid drug testing.

Anal Bioanal Chem 2018 Aug 16;410(21):5107-5112. Epub 2018 Jun 16.

Research Institute for Pesticides and Water, University Jaume I, Avda Sos Baynat s/n, 12071, Castellón, Spain.

Synthetic cannabinoids (SCs) are consumed as legal alternative to cannabis and often allow passing drug-screening tests. Their rapid transience on the drug scene, combined with their mostly unknown metabolic profiles, creates a scenario with constantly moving analytical targets, making their monitoring and identification challenging. The development of fast screening strategies for SCs, not directly focused on their chemical structure, as an alternative to the commonly applied target acquisition methods, would be highly appreciated in forensic and public health laboratories. An innovative untargeted metabolomics approach, focused on herbal components commonly used for 'spice' products, was applied. Saliva samples of healthy volunteers were collected at pre-dose and after smoking herbal components and analysed by high-resolution mass spectrometry. The data obtained, combined with appropriate statistical analysis, allowed to highlight and elucidate two markers (scopoletin and N,N-bis(2-hydroxyethyl)dodecylamine), which ratio permitted to differentiate herbal smokers from non-smokers. The proposed strategy will allow discriminating potential positives, on the basis of the analysis of two markers identified in the herbal blends. This work is presented as a step forward in SC drug testing, promoting a smart first-line screening approach, which will allow reducing the number of samples to be further investigated by more sophisticated HRMS methods. Graphical abstract The development of an alternative, generic screening methods of synthetic cannabinoids, not directly based on the chemical structure, in order to provide fast response on its potential consumption.
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http://dx.doi.org/10.1007/s00216-018-1182-8DOI Listing
August 2018

Wastewater Analysis for Community-Wide Drugs Use Assessment.

Handb Exp Pharmacol 2018;252:543-566

Department of Chemistry, University of Bath, Bath, UK.

Wastewater-based epidemiology (WBE) complements existing epidemiology-based estimation techniques and provides objective, evidence-based estimates of illicit drug use. After consumption, biomarkers - drugs and their metabolites - excreted to toilets and flushed into urban sewer networks can be measured in raw wastewater samples. The quantified loads can serve as an estimate for the collective consumption of all people contributing to the wastewater sample. This transdisciplinary approach, further explained in this chapter, has developed, matured and is now established for monitoring substances such as cocaine and amphetamine-type stimulants. Research currently underway is refining WBE to new applications including new psychoactive substances (NPS).
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http://dx.doi.org/10.1007/164_2018_111DOI Listing
June 2019

Improving wastewater-based epidemiology to estimate cannabis use: focus on the initial aspects of the analytical procedure.

Anal Chim Acta 2017 Oct 18;988:27-33. Epub 2017 Aug 18.

Research Institute for Pesticides and Water, University Jaume I, Avda. Sos Baynat s/n, E-12071, Castellón, Spain. Electronic address:

Wastewater-based epidemiology is a promising and complementary tool for estimating drug use by the general population, based on the quantitative analysis of specific human metabolites of illicit drugs in urban wastewater. Cannabis is the most commonly used illicit drug and of high interest for epidemiologists. However, the inclusion of its main human urinary metabolite 11-nor-9-carboxy-Δ-tetrahydrocannabinol (THC-COOH) in wastewater-based epidemiology has presented several challenges and concentrations seem to depend heavily on environmental factors, sample preparation and analyses, commonly resulting in an underestimation. The aim of the present study is to investigate, identify and diminish the source of bias when analysing THC-COOH in wastewater. Several experiments were performed to individually assess different aspects of THC-COOH determination in wastewater, such as the number of freeze-thaw cycles, filtration, sorption to different container materials and in-sample stability, and the most suitable order of preparatory steps. Results highlighted the filtration step and adjustment of the sample pH as the most critical parameters to take into account when analysing THC-COOH in wastewater. Furthermore, the order of these initial steps of the analytical procedure is crucial. Findings were translated into a recommended best-practice protocol and an inter-laboratory study was organized with eight laboratories that tested the performance of the proposed procedure. Results were found satisfactory with z-scores ≤ 2.
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http://dx.doi.org/10.1016/j.aca.2017.08.011DOI Listing
October 2017

Prediction of Collision Cross-Section Values for Small Molecules: Application to Pesticide Residue Analysis.

Anal Chem 2017 06 7;89(12):6583-6589. Epub 2017 Jun 7.

Research Institute for Pesticides and Water, University Jaume I , Avda. Sos Baynat s/n, E-12071 Castellón, Spain.

The use of collision cross-section (CCS) values obtained by ion mobility high-resolution mass spectrometry has added a third dimension (alongside retention time and exact mass) to aid in the identification of compounds. However, its utility is limited by the number of experimental CCS values currently available. This work demonstrates the potential of artificial neural networks (ANNs) for the prediction of CCS values of pesticides. The predictor, based on eight software-chosen molecular descriptors, was optimized using CCS values of 205 small molecules and validated using a set of 131 pesticides. The relative error was within 6% for 95% of all CCS values for protonated molecules, resulting in a median relative error less than 2%. In order to demonstrate the potential of CCS prediction, the strategy was applied to spinach samples. It notably improved the confidence in the tentative identification of suspect and nontarget pesticides.
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http://dx.doi.org/10.1021/acs.analchem.7b00741DOI Listing
June 2017

Monitoring a large number of pesticides and transformation products in water samples from Spain and Italy.

Environ Res 2017 07 14;156:31-38. Epub 2017 Mar 14.

RCCS - Istituto di Ricerche Farmacologiche "Mario Negri", Environmental Biomarkers Unit, Food Toxicology Laboratory, Department of Environmental Health Sciences, Via La Masa 19, 20156 Milan, Italy. Electronic address:

Assessing the presence of pesticides in environmental waters is particularly challenging because of the huge number of substances used which may end up in the environment. Furthermore, the occurrence of pesticide transformation products (TPs) and/or metabolites makes this task even harder. Most studies dealing with the determination of pesticides in water include only a small number of analytes and in many cases no TPs. The present study applied a screening method for the determination of a large number of pesticides and TPs in wastewater (WW) and surface water (SW) from Spain and Italy. Liquid chromatography coupled to high-resolution mass spectrometry (HRMS) was used to screen a database of 450 pesticides and TPs. Detection and identification were based on specific criteria, i.e. mass accuracy, fragmentation, and comparison of retention times when reference standards were available, or a retention time prediction model when standards were not available. Seventeen pesticides and TPs from different classes (fungicides, herbicides and insecticides) were found in WW in Italy and Spain, and twelve in SW. Generally, in both countries more compounds were detected in effluent WW than in influent WW, and in SW than WW. This might be due to the analytical sensitivity in the different matrices, but also to the presence of multiple sources of pollution. HRMS proved a good screening tool to determine a large number of substances in water and identify some priority compounds for further quantitative analysis.
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http://dx.doi.org/10.1016/j.envres.2017.03.013DOI Listing
July 2017

Measuring biomarkers in wastewater as a new source of epidemiological information: Current state and future perspectives.

Environ Int 2017 Feb 27;99:131-150. Epub 2016 Dec 27.

Research Institute for Pesticides and Water, Universitat Jaume I, Castellon, Spain. Electronic address:

The information obtained from the chemical analysis of specific human excretion products (biomarkers) in urban wastewater can be used to estimate the exposure or consumption of the population under investigation to a defined substance. A proper biomarker can provide relevant information about lifestyle habits, health and wellbeing, but its selection is not an easy task as it should fulfil several specific requirements in order to be successfully employed. This paper aims to summarize the current knowledge related to the most relevant biomarkers used so far. In addition, some potential wastewater biomarkers that could be used for future applications were evaluated. For this purpose, representative chemical classes have been chosen and grouped in four main categories: (i) those that provide estimates of lifestyle factors and substance use, (ii) those used to estimate the exposure to toxicants present in the environment and food, (iii) those that have the potential to provide information about public health and illness and (iv) those used to estimate the population size. To facilitate the evaluation of the eligibility of a compound as a biomarker, information, when available, on stability in urine and wastewater and pharmacokinetic data (i.e. metabolism and urinary excretion profile) has been reviewed. Finally, several needs and recommendations for future research are proposed.
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http://dx.doi.org/10.1016/j.envint.2016.12.016DOI Listing
February 2017

Liquid chromatography-tandem mass spectrometry determination of synthetic cathinones and phenethylamines in influent wastewater of eight European cities.

Chemosphere 2017 Feb 1;168:1032-1041. Epub 2016 Nov 1.

Research Institute for Pesticides and Water, University Jaume I, Avda. Sos Baynat s/n, E-12071 Castellón, Spain. Electronic address:

The popularity of new psychoactive substances (NPS) has grown in recent years, with certain NPS commonly and preferentially consumed even following the introduction of preventative legislation. With the objective to improve the knowledge on the use of NPS, a rapid and very sensitive method was developed for the determination of ten priority NPS (N-ethylcathinone, methylenedioxypyrovalerone (MDPV), methylone, butylone, methedrone, mephedrone, naphyrone, 25-C-NBOMe, 25-I-NBOMe and 25-B-NBOMe) in influent wastewater. Sample clean-up and pre-concentration was made by off-line solid phase extraction (SPE) with Oasis MCX cartridges. Isotopically labelled internal standards were used to correct for matrix effects and potential SPE losses. Following chromatographic separation on a C column within 6 min, the compounds were measured by tandem mass spectrometry in positive ionization mode. The method was optimised and validated for all compounds. Limits of quantification were evaluated by spiking influent wastewater samples at 1 or 5 ng/L. An investigation into the stability of these compounds in influent wastewater was also performed, showing that, following acidification at pH 2, all compounds were relatively stable for up to 7 days. The method was then applied to influent wastewater samples from eight European countries, in which mephedrone, methylone and MDPV were detected. This work reveals that although NPS use is not as extensive as for classic illicit drugs, the application of a highly sensitive analytical procedure makes their detection in wastewater possible. The developed analytical methodology forms the basis of a subsequent model-based back-calculation of abuse rate in urban areas (i.e. wastewater-based epidemiology).
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http://dx.doi.org/10.1016/j.chemosphere.2016.10.107DOI Listing
February 2017

Mass spectrometric strategies for the investigation of biomarkers of illicit drug use in wastewater.

Mass Spectrom Rev 2018 05 17;37(3):258-280. Epub 2016 Oct 17.

Research Institute for Pesticides and Water, University Jaume I, Castellón, Spain.

The analysis of illicit drugs in urban wastewater is the basis of wastewater-based epidemiology (WBE), and has received much scientific attention because the concentrations measured can be used as a new non-intrusive tool to provide evidence-based and real-time estimates of community-wide drug consumption. Moreover, WBE allows monitoring patterns and spatial and temporal trends of drug use. Although information and expertise from other disciplines is required to refine and effectively apply WBE, analytical chemistry is the fundamental driver in this field. The use of advanced analytical techniques, commonly based on combined chromatography-mass spectrometry, is mandatory because the very low analyte concentration and the complexity of samples (raw wastewater) make quantification and identification/confirmation of illicit drug biomarkers (IDBs) troublesome. We review the most-recent literature available (mostly from the last 5 years) on the determination of IDBs in wastewater with particular emphasis on the different analytical strategies applied. The predominance of liquid chromatography coupled to tandem mass spectrometry to quantify target IDBs and the essence to produce reliable and comparable results is illustrated. Accordingly, the importance to perform inter-laboratory exercises and the need to analyze appropriate quality controls in each sample sequence is highlighted. Other crucial steps in WBE, such as sample collection and sample pre-treatment, are briefly and carefully discussed. The article further focuses on the potential of high-resolution mass spectrometry. Different approaches for target and non-target analysis are discussed, and the interest to perform experiments under laboratory-controlled conditions, as a complementary tool to investigate related compounds (e.g., minor metabolites and/or transformation products in wastewater) is treated. The article ends up with the trends and future perspectives in this field from the authors' point of view. © 2016 Wiley Periodicals, Inc. Mass Spec Rev 37:258-280, 2018.
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http://dx.doi.org/10.1002/mas.21525DOI Listing
http://www.ncbi.nlm.nih.gov/pmc/articles/PMC6191649PMC
May 2018