| 1. |
- Celma, Alberto, et al.
(författare)
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Analysis of polycyclic aromatic hydrocarbons (PAHs) and their derivatives in biochar treated stormwater
- 2023
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Ingår i: MethodsX. - 2215-0161. ; 10
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Tidskriftsartikel (refereegranskat)abstract
- Polycyclic aromatic hydrocarbons (PAHs), oxygenated PAHs (oxy-PAHs) and nitrogen heterocyclic polycyclic aromatic compounds (N-PACs) are persistent and semi-volatile organic compounds primarily formed due to incomplete combustion of organic material or, in the case of the derivatives, through transformation reactions of PAHs. Their presence in the environment is ubiquitous and many of them have been proven carcinogenic, teratogenic, and mutagenic. These toxic pollutants can therefore pose a threat to both ecosystem and human health and urges for remediation strategies for PAHs and derivatives from water bodies. Biochar is a carbon-rich material resulting from the pyrolysis of biomass resulting in a very porous matter with high surface area for an enhanced interaction with chemicals. This makes biochar a promising alternative for filtering micropollutants from contaminated aquatic bodies. In this work, a previously developed and validated methodology for the analysis of PAHs, oxy-PAHs and N-PACs in surface water samples was adapted for its utilization in biochar treated stormwater with special emphasis on scaling down the solid-phase extraction as well as including an additional filtering step for the removal of particulate matter in the media. & BULL; Optimized extraction method for PAHs, oxy-PAHs and N-PACs from stormwater treated with biochar. & BULL; Biochar strongly impacts the stormwater matrix and, therefore, additional steps are required in the extraction methodology. & BULL; Solid-phase extraction combined with GC-MS have been used to analyse PAHs, oxy-PAHs and N-PACs in stormwater treated with biochar.
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| 2. |
- Celma, Alberto
(författare)
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Screening for new psychoactive substances in wastewater from educational institutions
- 2023
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Ingår i: Environmental Research. - 0013-9351 .- 1096-0953. ; 237
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Tidskriftsartikel (refereegranskat)abstract
- Drug (ab)use among young people is a serious issue, negatively impacting their well-being and prospects. The emergence of new psychoactive substances (NPS) further complicates the situation as they are easily accessible (e.g., online), but users are at high risk of intoxication as their chemical identity is often unknown and toxicity poorly understood. While surveys and drug testing are traditionally used in educational institutions to comprehend drug use trends and establish effective prevention programs, they are not without their limitations. Accordingly, we investigated the occurrence of NPS in educational institutions through wastewater analysis and critically evaluated the viability of the approach. The study included eight wastewater samples from primary schools (ages 6-15 years), six from secondary schools (ages 15-19 years), three from institutions for both secondary and higher education (ages 15+), and six from higher educational institutions (ages 19+). Samples were obtained mid-week and evaluated in two Slovenian municipalities; the capital Ljubljana and a smaller one (M1). Samples were screened using liquid chromatography-ion mobility-high-resolution mass spectrometry (LC-IMSHRMS), and NPS identified at three levels of confidence (Level 1: unequivocal, Level 2: probable, Level 3: tentative) from a suspect list containing over 5600 entries. NPS were identified in all types of educational institutions. Most were synthetic stimulants, with 3-MMC, ephedrine, 4-chloro-alpha-PPP, and ethcathinone being unequivocally identified. Also, NPS were present in wastewater from all educational institution types revealing potential spatial but no inter-institutional trends. Although specific groups cannot be targeted, the study, as a proof-of-concept, demonstrates that a suspect screening of wastewater employing LC-IMS-HRMS can be used as a radar for NPS in educational institutions and potentially replace invasive drug testing.
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| 3. |
- Celma, Alberto
(författare)
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Wastewater monitoring of a community COVID-19 outbreak in a Spanish municipality
- 2023
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Ingår i: Journal of Environmental Exposure Assessment. - 2771-5949. ; 2
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Tidskriftsartikel (refereegranskat)abstract
- Severe acute respiratory syndrome coronavirus 2 (SARS-CoV-2) wastewater surveillance has become an increasingly important tool since the initial moments of the coronavirus disease (COVID-19) pandemic, mainly conducted at a large population scale. However, the large-sized sewersheds may not provide suitable information for monitoring localized outbreaks. After the declaration of a community COVID-19 outbreak in two neighborhoods of Castellón (Spain), SARS-CoV-2 RNA levels were monitored in wastewater samples. Moreover, genomic sequencing was performed. Thirty-three samples were collected in 2020, distributed over three points of the sewage network, two of which were close to the areas where the cases were declared. The third point was located at the inlet of the municipal wastewater treatment plant (WWTP). The samples were analyzed by RT-qPCR, using specific N1 and N2 target regions. The sum of confirmed cases, with the date of symptoms onset within the 3 weeks before each sampling day, was calculated. SARS-CoV-2 RNA was detected on most days in the two sampling points at neighborhood level, and the detection became negative when the number of cases with symptoms onset during the last 21 days in the study areas decreased to 0 or 1 case. The genomic sequencing performed for RNA from wastewater and clinical samples showed the same variant. The detection of SARS-CoV-2 and the subsequent non-detection provided the epidemiologists in charge of controlling the outbreak with useful information to confirm its closure, complementing the clinical and epidemiological data. Our findings illustrate the value of wastewater surveillance for localized outbreaks, especially in situations of low incidence of COVID-19 at the broader community level.
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| 4. |
- Celma Tirado, Alberto, et al.
(författare)
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Are preserved coastal water bodies in Spanish Mediterranean basin impacted by human activity? Water quality evaluation using chemical and biological analyses
- 2022
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Ingår i: Environment International. - : Elsevier BV. - 0160-4120 .- 1873-6750. ; 165
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Tidskriftsartikel (refereegranskat)abstract
- The Spanish Mediterranean basin is particularly susceptible to climate change and human activities, making it vulnerable to the influence of anthropogenic contaminants. Therefore, conducting comprehensive and exhaustive water quality assessment in relevant water bodies of this basin is pivotal. In this work, surface water samples from coastal lagoons or estuaries were collected across the Spanish Mediterranean coastline and subjected to target and suspect screening of 1,585 organic micropollutants by liquid chromatography coupled to ion mobility separation and high resolution mass spectrometry. In total, 91 organic micropollutants could be confirmed and 5 were tentatively identified, with pharmaceuticals and pesticides being the most prevalent groups of chemicals. Chemical analysis data was compared with data on bioanalysis of those samples (recurrent aryl hydrocarbon receptor (AhR) activation, and estrogenic receptor (ER) inhibition in wetland samples affected by wastewater streams). The number of identified organic contaminants containing aromatic rings could explain the AhR activation observed. For the ER antagonistic effects, predictions on estrogenic inhibition potency for the detected compounds were used to explain the activities observed. The integration of chemical analysis with bioanalytical observations allowed a comprehensive overview of the quality of the water bodies under study.
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| 5. |
- Celma Tirado, Alberto
(författare)
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Effects of structural characteristics of (un)conjugated steroid metabolites in their collision cross section value
- 2023
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Ingår i: Analytica Chimica Acta. - : Elsevier BV. - 0003-2670 .- 1873-4324. ; 1254
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Tidskriftsartikel (refereegranskat)abstract
- In this work, the collision cross section (CCS) value of 103 steroids (including unconjugated metabolites and phase II metabolites conjugated with sulfate and glucuronide groups) was determined by liquid chromatography coupled to traveling wave ion mobility spectrometry (LC-TWIMS). A time of flight (QTOF) mass analyzer was used to perform the analytes determination at high-resolution mass spectrometry. An electrospray ionization source (ESI) was used to generate [M+H]+, [M + NH4]+ and/or [M − H]- ions. High reproducibility was observed for the CCS determination in both urine and standard solutions, obtaining RSD lower than 0.3% and 0.5% in all cases respectively. CCS determination in matrix was in accordance with the CCS measured in standards solution showing deviations below 2%. In general, CCS values were directly correlated with the ion mass and allowed differentiating between glucuronides, sulfates and free steroids although differences among steroids of the same group were less significant. However, more specific information was obtained for phase II metabolites observing differences in the CCS value of isomeric pairs concerning the conjugation position or the α/β configuration, which could be useful in the structural elucidation of new steroid metabolites in the anti-doping field. Finally, the potential of IMS reducing interferences from the sample matrix was also tested for the analysis of a glucuronide metabolite of bolasterone (5β-androstan-7α,17α-dimethyl-3α,17β-diol-3-glucuronide) in urine samples.
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| 6. |
- Celma Tirado, Alberto, et al.
(författare)
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In vitro bioanalytical assessment of toxicity of wetland samples from Spanish Mediterranean coastline
- 2021
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Ingår i: Environmental Sciences Europe. - : Springer Science and Business Media LLC. - 2190-4715 .- 2190-4707. ; 33
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Tidskriftsartikel (refereegranskat)abstract
- Background Fresh water bodies represent less than 1% of overall amount of water on earth and ensuring their quality and sustainability is pivotal. Although several campaigns have been performed to monitor the occurrence of micropollutants by means of chemical analysis, this might not cover the whole set of chemicals present in the sample nor the potential toxic effects of mixtures of natural and anthropogenic chemicals. In this sense, by selecting relevant toxicity endpoints when performing in vitro bioanalysis, effect-based methodologies can be of help to perform a comprehensive assessment of water quality and reveal biological activities relevant to adverse health effects. However, no prior bioanalytical study was performed in wetland water samples from the Spanish Mediterranean coastline. Methods Eleven samples from relevant water bodies from the Spanish Mediterranean coastline were collected to monitor water quality on 8 toxicity endpoints. Aryl hydrocarbon receptor (AhR), androgenicity (AR+ and AR-), estrogenicity (ER+ and ER-), oxidative stress response (Nrf2) and vitamin D receptor (VDR+ and VDR-) reporter gene assays were evaluated. Results AhR was the reporter gene assay showing a more frequent response over the set of samples (activated by 9 out of 11 samples), with TCDD-eq in the range 7.7-22.2 pM. For AR, ER and VDR assays sporadic activations were observed. Moreover, no activity was observed on the Nrf2 reporter gene assay. Wastewater and street runaway streams from Valencia could be responsible for enhanced activities in one of the water inputs in the Natural Park 'L'Albufera'. Conclusions Water quality of relevant wetlands from the Spanish Mediterranean coastline has been evaluated. The utilization of a panel of 5 different bioassays to cover for different toxicity endpoints has demonstrated to be a good tool to assess water quality.
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| 7. |
- Celma Tirado, Alberto
(författare)
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Prediction of Retention Time and Collision Cross Section (CCSH plus , CCSH-, and CCSNa plus ) of Emerging Contaminants Using Multiple Adaptive Regression Splines
- 2022
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Ingår i: Journal of Chemical Information and Modeling. - : American Chemical Society (ACS). - 1549-9596 .- 1549-960X. ; 62, s. 5425-5434
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Tidskriftsartikel (refereegranskat)abstract
- Ultra-high performance liquid chromatography coupled to ion mobility separation and high-resolution mass spectrometry instruments have proven very valuable for screening of emerging contaminants in the aquatic environment. However, when applying suspect or nontarget approaches (i.e., when no reference standards are available), there is no information on retention time (RT) and collision cross-section (CCS) values to facilitate identification. In silico prediction tools of RT and CCS can therefore be of great utility to decrease the number of candidates to investigate. In this work, Multiple Adaptive Regression Splines (MARS) were evaluated for the prediction of both RT and CCS. MARS prediction models were developed and validated using a database of 477 protonated molecules, 169 deprotonated molecules, and 249 sodium adducts. Multivariate and univariate models were evaluated showing a better fit for univariate models to the experimental data. The RT model (R2 = 0.855) showed a deviation between predicted and experimental data of +/- 2.32 min (95% confidence intervals). The deviation observed for CCS data of protonated molecules using the CCSH model (R2 = 0.966) was +/- 4.05% with 95% confidence intervals. The CCSH model was also tested for the prediction of deprotonated molecules, resulting in deviations below +/- 5.86% for the 95% of the cases. Finally, a third model was developed for sodium adducts (CCSNa, R2 = 0.954) with deviation below +/- 5.25% for 95% of the cases. The developed models have been incorporated in an open-access and user-friendly online platform which represents a great advantage for third-party research laboratories for predicting both RT and CCS data.
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| 8. |
- Hollender, Juliane, et al.
(författare)
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NORMAN guidance on suspect and non-target screening in environmental monitoring
- 2023
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Ingår i: Environmental Sciences Europe. - : Springer Nature. - 2190-4707 .- 2190-4715. ; 35:1
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Forskningsöversikt (refereegranskat)abstract
- Increasing production and use of chemicals and awareness of their impact on ecosystems and humans has led to large interest for broadening the knowledge on the chemical status of the environment and human health by suspect and non-target screening (NTS). To facilitate effective implementation of NTS in scientific, commercial and governmental laboratories, as well as acceptance by managers, regulators and risk assessors, more harmonisation in NTS is required. To address this, NORMAN Association members involved in NTS activities have prepared this guidance document, based on the current state of knowledge. The document is intended to provide guidance on performing high quality NTS studies and data interpretation while increasing awareness of the promise but also pitfalls and challenges associated with these techniques. Guidance is provided for all steps; from sampling and sample preparation to analysis by chromatography (liquid and gas-LC and GC) coupled via various ionisation techniques to high-resolution tandem mass spectrometry (HRMS/MS), through to data evaluation and reporting in the context of NTS. Although most experience within the NORMAN network still involves water analysis of polar compounds using LC-HRMS/MS, other matrices (sediment, soil, biota, dust, air) and instrumentation (GC, ion mobility) are covered, reflecting the rapid development and extension of the field. Due to the ongoing developments, the different questions addressed with NTS and manifold techniques in use, NORMAN members feel that no standard operation process can be provided at this stage. However, appropriate analytical methods, data processing techniques and databases commonly compiled in NTS workflows are introduced, their limitations are discussed and recommendations for different cases are provided. Proper quality assurance, quantification without reference standards and reporting results with clear confidence of identification assignment complete the guidance together with a glossary of definitions. The NORMAN community greatly supports the sharing of experiences and data via open science and hopes that this guideline supports this effort.
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| 9. |
- Mohammed Taha, Hiba, et al.
(författare)
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The NORMAN Suspect List Exchange (NORMAN-SLE) : facilitating European and worldwide collaboration on suspect screening in high resolution mass spectrometry
- 2022
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Ingår i: Environmental Sciences Europe. - : Springer. - 2190-4707 .- 2190-4715. ; 34:1
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Tidskriftsartikel (refereegranskat)abstract
- Background: The NORMAN Association (https://www.norman-network.com/) initiated the NORMAN Suspect List Exchange (NORMAN-SLE; https://www.norman-network.com/nds/SLE/) in 2015, following the NORMAN collaborative trial on non-target screening of environmental water samples by mass spectrometry. Since then, this exchange of information on chemicals that are expected to occur in the environment, along with the accompanying expert knowledge and references, has become a valuable knowledge base for “suspect screening” lists. The NORMAN-SLE now serves as a FAIR (Findable, Accessible, Interoperable, Reusable) chemical information resource worldwide.Results: The NORMAN-SLE contains 99 separate suspect list collections (as of May 2022) from over 70 contributors around the world, totalling over 100,000 unique substances. The substance classes include per- and polyfluoroalkyl substances (PFAS), pharmaceuticals, pesticides, natural toxins, high production volume substances covered under the European REACH regulation (EC: 1272/2008), priority contaminants of emerging concern (CECs) and regulatory lists from NORMAN partners. Several lists focus on transformation products (TPs) and complex features detected in the environment with various levels of provenance and structural information. Each list is available for separate download. The merged, curated collection is also available as the NORMAN Substance Database (NORMAN SusDat). Both the NORMAN-SLE and NORMAN SusDat are integrated within the NORMAN Database System (NDS). The individual NORMAN-SLE lists receive digital object identifiers (DOIs) and traceable versioning via a Zenodo community (https://zenodo.org/communities/norman-sle), with a total of > 40,000 unique views, > 50,000 unique downloads and 40 citations (May 2022). NORMAN-SLE content is progressively integrated into large open chemical databases such as PubChem (https://pubchem.ncbi.nlm.nih.gov/) and the US EPA’s CompTox Chemicals Dashboard (https://comptox.epa.gov/dashboard/), enabling further access to these lists, along with the additional functionality and calculated properties these resources offer. PubChem has also integrated significant annotation content from the NORMAN-SLE, including a classification browser (https://pubchem.ncbi.nlm.nih.gov/classification/#hid=101).Conclusions: The NORMAN-SLE offers a specialized service for hosting suspect screening lists of relevance for the environmental community in an open, FAIR manner that allows integration with other major chemical resources. These efforts foster the exchange of information between scientists and regulators, supporting the paradigm shift to the “one substance, one assessment” approach. New submissions are welcome via the contacts provided on the NORMAN-SLE website (https://www.norman-network.com/nds/SLE/).
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