The Anthropocene fingerprint: Hazardous elements in waters of a coastal Mediterranean alluvial plain (Valencia, Spain).

This study focuses on the alluvial plain spanning between the Turia and Jucar rivers (486 km2) in Valencia, Spain - a highly productive agricultural area that also involves a Natural Park (La Albufera). Thirty-five points across different water sources and land uses were sampled to map the spatial distribution of 14 heavy metals (Al, As, B, Cd, Co, Cr, Cu, Fe, Li, Ni, Pb, Sr, Tl, and Zn), and to study the potential influence of water characteristics and environmental factors on them. Two pollution indexes were applied, Heavy Metal Evaluation Index (HEI) and Water Pollution Index (WPI), to assess the water quality state in the area. High levels were predominantly found in the southern region, particularly within rice farming areas. For B, Sr, and Tl, all samples exceeded WHO limits, EU legislation, or EPA benchmarks, with 61.76 % and 85.71 % of samples surpassing standards for Al and Li, respectively. Water salinization parameters greatly influenced the dynamics of Al, As, B, Li, Sr, and Tl. Analysis using both indexes (HEI and WPI) revealed poor water quality in the area, particularly in rice fields, posing potential toxic effects on ecosystems and human health. The findings of this work are valuable for understanding elements of concern in coastal wetlands under global change.

Fingerprinting of emerging contaminants in L'Albufera natural park (Valencia, Spain): Implications for wetland ecosystem health.

Wetlands are crucial ecosystems that are increasingly threatened by anthropogenic activities. L'Albufera Natural Park, the second-largest coastal wetland in Spain, faces significant pressures from surrounding agricultural lands, industrial activities, human settlements, and associated infrastructures, including treated wastewater inputs. This study aimed at (i) establishing pathways of emerging pollutants entering the natural wetland using both target and non-target screening (NTS) for management purposes, (ii) distinguishing specific contamination hotspots through Geographic Information System (GIS) and (iii) performing basic ecological risk assessment to evaluate ecosystem health. Two sampling campaigns were conducted in the spring and summer of 2019, coinciding with the start and end of the rice cultivation season, the region's primary agricultural activity. Each campaign involved the collection of 51 samples. High-resolution mass spectrometry (HRMS) was employed, using a simultaneous NTS approach with optimized gradients for pesticides and moderately polar compounds, along with complementary NTS methods for polar compounds, to identify additional contaminants of emerging concern (CECs). Quantitative analysis revealed that fungicides comprised a substantial portion of detected CECs, constituting approximately 50% of the total quantified pesticides. Tebuconazole emerged as the predominant fungicide, with the highest mean concentration (>16.9 µg L-1), followed by azoxystrobin and tricyclazole. NTS tentatively identified 16 pesticides, 43 pharmaceuticals and personal care products (PPCPs), 24 industrial compounds, and 12 other CECs with high confidence levels. Spatial distribution analysis demonstrated significant contamination predominantly in the southwestern region of the park, gradually diminishing towards the north-eastern outlet. The composition of contaminants varied between water and sediment samples, with pharmaceuticals predominating in water and industrial compounds in sediments. Risk assessment, evaluated through risk quotient calculations based on parent compound concentrations, revealed a decreasing trend towards the outlet, suggesting wetland degradation capacity. However, significant risk levels persist throughout much of the Natural Park, highlighting the urgent need for mitigation measures to safeguard the integrity of this vital ecosystem.

Trace elements and legacy and emerging organic contaminants concentrations datasets in sediments cores in L'Albufera Natural Park (Valencia, East of Spain): Association with "in-deep" sediment characteristics and risk assessment to the aquatic biota.

The chronological information provided by sediment cores about the beginning and evolution of anthropogenic contaminants is crucial for understanding the influence of humans on the environment. The dataset provides information about the vertical distribution of heavy metals (HMs), metalloids and various organic contaminants (OCs) including contemporary contaminants of emerging concern (CECs), such as pharmaceuticals and personal care products (PPCPs) and pesticides; as well as persistent organic contaminants (POPs) such as polycyclic aromatic hydrocarbons (PAHs), perfluoroalkyl substances (PFASs), organophosphorus flame retardants (OPFRs) in sediment cores of two different sampling areas (North and South) of L'Albufera lake. Additional information about the 14C-data of the organic matter present in the different layers of the sediment cores, and the 14C-data of the seashells found in some of them are shown. The dataset includes physico-chemical analyses of sediment characteristics at the different selected depth levels such as Organic Carbon (Corg), Inorganic Carbon (IC), Total Nitrogen (TN), Total Sulphur (TS) and texture. Furthermore, ecological risk assessment of these contaminants in surface sediment layers is performed to ascertain is potential toxicity. These data supplement the findings presented and considered in the research article "Exploring Organic and Inorganic Contaminant Histories in Sediment Cores Across the Anthropocene: Accounting for Site/Area Dependent Factors". Therefore, these data altogether are useful for researchers seeking to assess long-term impact of contamination.

Exploring organic and inorganic contaminant histories in sediment cores across the anthropocene: Accounting for site/area dependent factors.

Sedimentary records help chronologically identify anthropogenic contamination in environmental systems. This study analysed dated sediment cores from L'Albufera Lake (Valencia, Spain), to assess the occurrence of heavy metals (HMs), polycyclic aromatic hydrocarbons (PAHs), perfluoroalkyl substances (PFASs), organophosphorus flame retardants (OPFRs), pesticides and pharmaceuticals and personal care products (PPCPs). The results evidence the continuing vertical presence of all types of contaminants in this location. The sediment age was difficult to establish. However, the presence of shells together with an historical estimation and the knowledge of sedimentary rates could help. HMs contents are higher in the upper layer reflecting the most recent increase of the industrial and agricultural practices in the area since the middle 20th century. Higher availability index of these HMs in the upper sediment layers is associated with point and diffuse contamination sources in the area. PAHs and OPFRs were homogeneous distributed through the sediments with few exceptions such as phenanthrene in the North and fluoranthene in the South. Perfluorooctanoic acid (PFOA) and perfluorooctanesulfonate (PFOS) were detected throughout the sediment core while short-chain PFASs (except perfluoropentanoic acid (PFPeA)) were detected only in the top layer. Pesticides and PPCPs showed appreciable down-core mobility. The vertical concentration profiles of organic contaminants did not exhibit a clear trend with depth, then, it is difficult to develop a direct relationship between sediment age and contaminant concentrations, and to elucidate the historical trend of contamination based on dated sediment core. Consequently, linking contaminant occurrence in sediments directly to their historical use is somewhat speculative at least in the conditions of L'Albufera Lake.

Dataset of pharmaceuticals and personal care products in a Mediterranean coastal wetland.

The dataset provides information on Pharmaceutical and Personal Care Products (PPCPs) detected in the Albufera Natural Park (Valencia, Spain), a typical Mediterranean coastal wetland. These PPCPs constitute an important group of organic pollutants highly representative of the human impact. The concentrations values measured in soil, sediment and water and the statistical relationship of contaminants between them and with the environmental parameters could help to understand their fate in different compartments. The data also reported the occurrence and removal efficiency (%) for each contaminant in ten wastewater treatment plants (WWTPs), located in the surrounding area. This dataset could provide an idea on the effectiveness of WWTP treatments and the capacity of released PPCPs to affect the ecosystem. The extraction of analytes was based on solid-phase extraction (SPE) for water and solvent extraction followed by the previous SPE as clean-up for soil and sediment. Determination was carried out by high performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS) with a triple-quadrupole. The present dataset was analyzed within the article entitled: "Pharmaceuticals and personal care products in a Mediterranean coastal wetland: Impact of anthropogenic and spatial factors and environmental risk assessment"[1].

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

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).

Pharmaceuticals and personal care products in a Mediterranean coastal wetland: Impact of anthropogenic and spatial factors and environmental risk assessment.

The present study focused on the occurrence, distribution and risk assessment of 32 pharmaceuticals and personal care products (PPCPs) in water and sediment, as well as the surrounding soil of the irrigation channels and lake of a Mediterranean coastal wetland, the Albufera Natural Park (Valencia, Spain). Moreover, the influent and effluent of ten wastewater treatment plants (WWTPs) that treat wastewater from Valencia and the surrounding areas were also studied. BPA, caffeine, diclofenac, ethyl paraben, methyl paraben, metformin, tramadol and salicylic acid were the predominant PPCPs detected in the channels and the lake, and are in good agreement with those detected in the effluent. Furthermore, 22 PPCPs were detected in >47% of the sediment samples. Of them, BPA, ethyl paraben, furosemide, ibuprofen and salicylic acid were at higher concentrations. In contrast, only seven PPCPs were detected in >44% of the soil samples. Spatial variation showed that the concentration of many PPCPs was higher in the northern area of the park, whereas the ibuprofen concentrations were higher in the south. Differences were also observed according to the type of water used for irrigation and the land uses of the area. A risk assessment based on the hazardous quotient (HQ) indicated that caffeine is a compound of concern, and tramadol at the highest concentration showed a moderate risk for the organisms assessed. Considering the mixture of the PPCPs found at each sampling point, the green algae are at risk, particularly in those points located near the city of Valencia (the most important nearby human settlement). These results indicate the need for further studies.

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

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.

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

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.

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

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.

[Wastewater-based epidemiology: applications towards the estimation of drugs of abuse consumption and public health in general. The Spanish network ESAR-Net]. / Análisis de aguas residuales con fines epidemiológicos: aplicaciones a la estimación del consumo de sustancias de abuso y en salud pública en general. Red española ESAR-Net.

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.

En este artículo se presenta la metodología de análisis de aguas residuales con fines epidemiológicos (wastewater-based epidemiology, WBE) y su potencial para abordar diversos aspectos relacionados con la salud pública. Esta metodología permite obtener datos a una escala temporal y espacial relativamente pequeña (típicamente datos diarios-semanales sobre un municipio) de hábitos de consumo de sustancias de abuso, ilegales (como la cocaína o el cannabis) o legales (como el alcohol) a través de la determinación de biomarcadores de consumo (el compuesto original no metabolizado o alguno de sus metabolitos) en el agua residual. Aparte de discutir los fundamentos, ventajas y limitaciones de WBE, se comentan los precedentes más relevantes a nivel internacional, y las actividades más destacables en España en este ámbito. Finalmente, se exponen, los objetivos de la Red Española de Análisis de Aguas Residuales con Fines Epidemiológicos (ESAR-Net), una "Red de Excelencia" que agrupa a investigadores españoles con amplia experiencia en el área de WBE, así como las perspectivas de futuro de esta metodología puede tener para mejorar las competencias de la Salud Pública en España.

Análisis de aguas residuales con fines epidemiológicos: aplicaciones a la estimación del consumo de sustancias de abuso y en salud pública en general. Red española ESAR-Net / Wastewater-based epidemiology: applications towards the estimation of drugs of abuse consumption and public health in general. The Spanish network ESAR-Net

En este artículo se presenta la metodología de análisis de aguas residuales con fines epidemiológicos (wastewater-based epidemiology, WBE) y su potencial para abordar diversos aspectos relacionados con la salud pública. Esta metodología permite obtener datos a una escala temporal y espacial relativamente pequeña (típicamente datos diarios-semanales sobre un municipio) de hábitos de consumo de sustancias de abuso, ilegales (como la cocaína o el cannabis) o legales (como el alcohol) a través de la determinación de biomarcadores de consumo (el compuesto original no metabolizado o alguno de sus metabolitos) en el agua residual. Aparte de discutir los fundamentos, ventajas y limitaciones de WBE, se comentan los precedentes más relevantes a nivel internacional, y las actividades más destacables en España en este ámbito. Finalmente, se exponen, los objetivos de la Red Española de Análisis de Aguas Residuales con Fines Epidemiológicos (ESAR-Net), una "Red de Excelencia " que agrupa a investigadores españoles con amplia experiencia en el área de WBE, así como las perspectivas de futuro de esta metodología puede tener para mejorar las competencias de la Salud Pública en 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

Multi-residue determination of 47 organic compounds in water, soil, sediment and fish-Turia River as case study.

A sensitive and reliable method based on solid-liquid extraction (SLE) using McIlvaine-Na2EDTA buffer (pH=4.5)-methanol and solid-phase extraction (SPE) clean up prior to ultra-high-performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS) was applied to determine 47 organic contaminants in fish, soil and sediments. The SPE procedure to clean-up the extracts was also used as extraction method to determine these compounds in water. Recoveries ranged from 38 to 104% for all matrices with RSDs<30%. Limits of Quantification for the target compounds were in the range of 10-50ng/g for soil, 2-40ng/g for sediment, 5-30ng/g for fish and 0.3-26ng/L for water. Furthermore, the proposed method was compared to QuEChERS (widely used for environmental matrices) that involves extraction with buffered acetonitrile (pH 5.5) and dispersive SPE clean-up. The results obtained (recoveries>50% for 36 compounds in front of 9, matrix effect<20% for 31 compounds against 21, and LOQs <25ngg-1 for 38 compounds against 22) indicates that the proposed method is more efficient than QuEChERS, The method was applied to monitoring these compounds along the Turia River. In river waters, Paracetamol (175ngL-1), ibuprofen (153ngL-1) and bisphenol A (41ngL-1) were the compounds most frequently detected while in sediments were vildagliptin (7ngg-1) and metoprolol (31ngg-1) and in fish, bisphenol A (33ngg-1) or sulfamethoxazole (13ngg-1).

Pesticide occurrence in the waters of Júcar River, Spain from different farming landscapes.

A combined methodology to identify and quantify farming chemicals in the entire Júcar River basin has been developed. The procedure consisted of the application of environmental forensic criteria associating laboratory analytical samples, cartographic analysis using Geographical Information Systems (GIS) and synthetic statistical analysis. Sampling involved the collection of 15 samples in surface waters distributed alongside the Júcar River and its two main tributaries (Cabriel and Magro Rivers). The analytical procedure involves generic sample extraction and selective determination of up to 50 target pesticides by liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS). Geographical analysis was performed by mixing both sampling points with analytical results and land use-cover layers for the year 2011. PCA and descriptive statistical analysis was further performed combining land use/cover information and pesticides results to determine correlation between dominant agricultural practices (irrigation and rain fed farming) and location of sampling points. Out of 50 pesticides, 20 were identified and 18 presented concentrations higher than the limits of quantification in surface waters, with a large dispersion in concentrations: from 0.05ng/L (terbuthylazine-2 hydroxy) to 222.45ng/L (imazalil). Statistical analyses reveals that there is a correlation between the percentage of land devoted to irrigation farming, whereas correlations are weaker when analysing the relationship of pesticides in rain fed dominated areas.

Assessing drugs of abuse distribution in Turia River based on geographic information system and liquid chromatography mass spectrometry.

Drugs of abuse are continuously discharged into wastewaters as part of their elimination process. Pollution at very low concentrations appears to be broad in environmental compartments near populated areas. A total of 42 drugs of abuse and metabolites were analysed in surface water samples collected in 2012 and 2013 by solid phase extraction and liquid chromatography coupled to mass spectrometry. Analytical results of target compounds were georeferenced and integrated into a geographical information systems (GIS). Ecotoxicological risk of drugs of abuse detected in the Turia River was evaluated in this study by calculating risk quotient (RQ). In 2012, 6 compounds were detected in a total of 22 points. In 2013, 7 compounds were found in a total of 31 sampling sites, 4 of them also detected in 2012. The most frequent compound was benzoylecgonine, detected in 9 sampling points in 2012 and 8 in 2013, at an average concentration of 25.4ng/L and 14.02ng/L. Codeine reached the maximum concentration of detected compounds (101ng/L) in 2013. GIS provided the spatial incidence of drugs of abuse along the Turia River basin. The distribution of these compounds in 2012 and 2013 shows that the highest concentrations and frequency of drugs of abuse run into places with the highest population density. The RQ obtained from measured concentrations of detected drugs predict that no short-term environmental risk might be expected. Further research including multi-stressors studies with more potentially persistent or pseudo-persistent organic pollutants in surface waters is needed to establish relationships with human pressure in a river basin.

Emerging contaminants related to the occurrence of forest fires in the Spanish Mediterranean.

Forest fires can be a source of contamination because, among others, of the use of chemicals to their extinction (flame retardants, FRs), or by the production of Polycyclic Aromatic Hydrocarbons (PAHs) derived from high temperature alteration of organic matter. Up to our knowledge, this study is the first to assess the direct (PAHs 16 on the USA EPA's priority list), and indirect [tri- to hepta- brominated diphenyl ethers (PBDEs), organophosphorus flame retardants (PFRs) and perfluoroalkyl substances (PFASs)] contamination related to forest fires. The abundance and distribution of these contaminants were monitored on two Mediterranean hillslopes, one burned and one unburned, near Azuébar (SE Spain). Samples were taken in the foot, middle, and top of the slope, at two depths, and in two environments (under canopy and bare soil). Sediments were collected from sediment fences after erosive rainfall events. Most of the screened compounds were found in both, burned and control hillslopes, though significant differences were found between both. In burned soil, low concentrations of PBDEs (maximum ΣPBDEs: 7.3ngg-1), PFRs (664.4ngg-1) and PFASs (56.4ngg-1) were detected in relation to PAHs (Σ16 PAHs=1255.3ngg-1). No significant influence of the hillslope position was observed for any of the contaminants but differences based on depth and vegetation presence tended to be significant, particularly for the PAHs. After the first erosive event, concentrations of PBDEs and PAHs were higher in sediment than in soil (ΣPBDEs: 17.8ngg-1 and Σ16 PAHs=3154.2ngg-1) pointing out the importance of connectivity processes, especially shortly after fire.

Analysis of cannabinoids by liquid chromatography-mass spectrometry in milk, liver and hemp seed to ensure food safety.

A method for determining cannabinoids, Δ9-tetrahidrocannabinol (THC), 11-nor-9-carboxy-Δ9-THC (THC-COOH) and 11-hidroxy-Δ9-THC (THC-OH) in milk, liver and hemp seeds based on liquid chromatography tandem mass spectrometry has been optimized and validated. Analytes were extracted with methanol and the extracts cleaned-up by solid-phase extraction using Oasis HLB (60mg). The developed method was validated according to the Commission Decision 2002/657/EC. The decision limit (CCα) and detection capability (CCß) ranged from 3.10-10.5ngg-1 and 3.52-11.5ngg-1, the recoveries were 76-118% and matrix effect ranged from -17.8% to 19.9% in the three matrices studied. The method was applied to food samples obtaining positive results for THC in hemp seeds (average 0.82µgg-1) and three brands of junior formula milk at concentrations from 4.76 to 56.11ngg-1. The developed method was suitable achieving identification and quantification of cannabinoids in food matrices.

Analysis of psychoactive substances in water by information dependent acquisition on a hybrid quadrupole time-of-flight mass spectrometer.

Emerging drugs of abuse, belonging to many different chemical classes, are attracting users with promises of "legal" highs and easy access via internet. Prevalence of their consumption and abuse through wastewater-based epidemiology can only be realized if a suitable analytical screening procedure exists to detect and quantify them in water. Solid-phase extraction and ultra-high performance liquid chromatography quadrupole time-of-flight-mass spectrometry (UHPLC-QqTOF-MS/MS) was applied for rapid suspect screening as well as for the quantitative determination of 42 illicit drugs and metabolites in water. Using this platform, we were able to identify amphetamines, tryptamines, piperazines, pyrrolidinophenones, arylcyclohexylamines, cocainics, opioids and cannabinoids. Additionally, paracetamol, carbamazepine, ibersartan, valsartan, sulfamethoxazole, terbumeton, diuron, etc. (including degradation products as 3-hydroxy carbamazepine or deethylterbuthylazine) were detected. This method encompasses easy sample preparation and rapid identification of psychoactive drugs against a database that cover more than 2000 compounds that ionized in positive mode, and possibility to identify metabolites and degradation products as well as unknown compounds. The method for river water, influent and effluents samples was fully validated for the target psychoactive substances including assessment of matrix effects (-88-67.8%), recovery (42-115%), precision (<19%) and limits of quantification (1-100ngL(-1)). Method efficiency was thoroughly investigated for a wide range of waste and surface waters. Robust and repeatable functioning of this platform in the screening, identification and quantification of traditional and new psychoactive drugs biomarkers and other water contaminants is demonstrated.

Spatio-temporal patterns of pesticide residues in the Turia and Júcar Rivers (Spain).

A study was conducted on the occurrence of 50 pesticides in water and sediments of Turia and Júcar Rivers (Valencian Community, Eastern Spain) for a period of two consecutive years each, 2010/2011 and 2012/2013, respectively to assess the contribution of agriculture and urban activities on pesticide pollution. The results showed that mean concentrations of pesticides ranged from