Publications by authors named "Marina Campos-Mañas"

6 Publications

  • Page 1 of 1

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

Environ Int 2021 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

Enhanced activated persulfate oxidation of ciprofloxacin using a low-grade titanium ore under sunlight: influence of the irradiation source on its transformation products.

Environ Sci Pollut Res Int 2021 Jan 7. Epub 2021 Jan 7.

Instituto de Ingeniería, Universidad Nacional Autónoma de México (UNAM), Alcaldía Coyoacán, 04510, México City, Mexico.

In this work, the activated persulfate oxidation of ciprofloxacin (CIP) using a low-grade titanium ore under sunlight or simulated sunlight were conducted to analyze the CIP degradation efficiency and to identify the transformation products (TPs) generated during oxidation under both types of irradiation sources by using liquid chromatography-quadrupole time-of-flight mass spectrometry (LC-QTOF-MS). All advance oxidation process experiments were performed in a 2700-mL raceway reactor at a pH value of ~ 6.5 and an initial CIP concentration of 1 mg/L, during 90 min of reaction time. The control experiments carried out under simulated sunlight achieved a 97.7 ± 0.6% degradation efficiency, using 385 W/m of irradiation with an average temperature increase of 11.7 ± 0.6 °C. While, the experiments under sunlight reached a 91.2 ± 1.3% degradation efficiency, under an average irradiation value of 19.2 ± 0.3 W/m in October-November 2019 at hours between 11:00 am and 3:00 pm with an average temperature increase of 1.4 ± 0.8 °C. Mass spectrometry results indicated that 14 of the 108 possible TPs reported in the literature were detected. The calculated exact mass, measured accurate mass, and its characteristic diagnostic fragment ions were listed, and two new TPs were tentative identified. The TP generation analysis showed that some specific compounds were detected in different time intervals with kinetic variations depending on the irradiation used. Consequently, two CIP degradation pathways were proposed, since the type of irradiation determines the CIP degradation mechanism. Graphical abstract.
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http://dx.doi.org/10.1007/s11356-020-11564-8DOI Listing
January 2021

Determination of dextromethorphan and dextrorphan solar photo-transformation products by LC/Q-TOF-MS: Laboratory scale experiments and real water samples analysis.

Environ Pollut 2020 Oct 10;265(Pt A):114722. Epub 2020 May 10.

Solar Energy Research Centre (CIESOL), Joint Centre University of Almería-CIEMAT, Ctra de Sacramento s/n. 04120, Almería, Spain; Department of Chemistry and Physics, University of Almería, Spain. Electronic address:

This work discusses the identification of the transformation products (TPs) generated during the photolytic degradation of dextromethorphan (DXM) and its metabolite dextrorphan (DXO), under simulated solar radiation in aqueous solutions (Milli-Q water and river water) in order to determinate its behavior into the aquatic environment. Tentative identification of the TPs was performed by liquid chromatography/quadrupole time-of-flight mass spectrometry (LC/QTOF-MS), following a suspect screening approach. The use of high resolution-mass spectrometry (HRMS) allowed the tentative identification of DXM and DXO photoproducts based on the structure proposed by an in silico software, the accurate mass measurement, the MS/MS fragmentation pattern and the molecular formula finding. A total of 19 TPs were found to match some of the accurate masses included in a suspect list, and they were all tentatively identified by their characteristic MS-MS fragments. Most of the TPs identified showed a minor modified molecular structure like the introduction of hydroxyl groups, or demethylation. The time-evolution of precursors and TPs were monitored throughout the experiments, and degradation kinetics were presented for each analyte. Finally, the occurrence of DXM, DXO, and their tentatively proposed photodegradation TPs was evaluated in both surface and wastewater. In all real matrices, the results showed that the highest concentration was detected for DXO, followed by TP-244 (N-desmethyldextrorphan) and DXM.
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http://dx.doi.org/10.1016/j.envpol.2020.114722DOI Listing
October 2020

Determination of pesticide levels in wastewater from an agro-food industry: Target, suspect and transformation product analysis.

Chemosphere 2019 Oct 23;232:152-163. Epub 2019 May 23.

Solar Energy Research Centre (CIESOL), Joint Centre University of Almeria-CIEMAT, Carretera de Sacramento s/n, 04120, Almeria, Spain; Department of Chemistry and Physics, University of Almeria, Spain.

Agriculture is considered as the main source of water contamination by pesticides. However, food packaging or processing industries are also recognised as relevant point sources of contamination by these compounds, not yet investigated in depth. The objective of this work has been to improve current knowledge about the presence and concentration of pesticides in the effluent of a food processing industry, as well as to investigate their main transformation products (TPs). An analytical strategy combining target and suspect analysis has been applied to provide an evaluation of the effluents. The methodology involves solid-phase extraction (SPE) of wastewater samples followed by (i) liquid chromatography quadrupole-linear ion trap tandem mass spectrometry (LC-QqLIT-MS/MS) for quantitative target analysis and (ii) liquid chromatography coupled to quadrupole-time-of-flight high resolution mass spectrometry (LC-QTOF-HRMS) to identify non-target pesticides and possible TPs. The results revealed the presence of 17 of the target pesticides analysed and 3 additional ones as a result of the suspect screening performed by HRMS. The TPs were investigated for the pesticides found at the highest concentrations: imazalil (7038-19802 ng/L), pyrimethanil (744-9591 ng/L) and thiabendazole (341-926 ng/L). Up to 14 TPs could be tentatively identified, demonstrating the relevance of this type of studies. These data provide a better understanding of the occurrence of pesticides and their TPs in agro-food industrial effluents.
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http://dx.doi.org/10.1016/j.chemosphere.2019.05.147DOI Listing
October 2019

Identification of opioids in surface and wastewaters by LC/QTOF-MS using retrospective data analysis.

Sci Total Environ 2019 May 30;664:874-884. Epub 2019 Jan 30.

Solar Energy Research Centre (CIESOL), Joint Centre University of Almería-CIEMAT, Ctra de Sacramento s/n, 04120 Almería, Spain.

Opioids, both as prescription drugs and abuse substances, have been a hot topic and a focus of discussion in the media for the last few years. Although the literature published shows the occurrence of opioids and some of their metabolites in the aquatic environment, there are scarce data in the application of high resolution mass spectrometry (HRMS) for the analysis of these compounds in the environment. The use of HRMS allows increasing the number of opioids that can be studied as well as the detection of unknown opioids, their metabolites and potential transformation products. In this work, a retrospective analysis for the identification of opioids and their metabolites using a curated database was applied to surface water and wastewater samples taken in the state of Minnesota (U.S.) in 2009, which were previously analyzed by liquid chromatography/time-of-flight mass spectrometry (LC/TOF-MS) for antidepressants. The database comprised >200 opioids including natural opiates (e.g. morphine and codeine), their semi-synthetic derivatives (e.g. heroin, hydromorphone, hydrocodone, oxycodone, oxymorphone, meperidine and buprenorphine), fully synthetic opioids (e.g. fentanyl, methadone, tramadol, dextromethorphan and propoxyphene), as well as some of their metabolites (e.g. 6-monoacetylcodeine, dextrorphan, EDDP, normorphine and O-desmethyltramadol). Moreover, additional MS-MS experiments were performed to confirm their identification, as well as to recognize fragmentation patterns and diagnostic ions for several opioids. These data provide a better understanding of the historical occurrence of opioids and their metabolites in surface waters impacted by wastewater sources. The concentrations of individual opioids in surface water and wastewater effluent varied from 8.8 (EDDP) to 1640 (tramadol) ngL and from 12 (dihydrocodeine) to 1288 (tramadol) ngL, respectively. The opioids with higher overall frequency detections were tramadol, dextromethorphan and its metabolite, dextrorphan.
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http://dx.doi.org/10.1016/j.scitotenv.2019.01.389DOI Listing
May 2019

Fast determination of pesticides and other contaminants of emerging concern in treated wastewater using direct injection coupled to highly sensitive ultra-high performance liquid chromatography-tandem mass spectrometry.

J Chromatogr A 2017 Jul 26;1507:84-94. Epub 2017 May 26.

Solar Energy Research Centre (CIESOL), Joint Centre University of Almería-CIEMAT, 04120, Almería, Spain. Electronic address:

It is well known that wastewater treatment plant (WWTP) effluents usually contain micropollutants such as pharmaceuticals (or their transformation products, TPs) or pesticides, which is a major issue when evaluating their possible reuse (e.g. for irrigation in agriculture). In search for an improved accuracy and simplicity, methods based on the direct injection of the sample (DI) represent a recent trend taking advantage of the increasing sensitivity of new mass spectrometry (MS) instruments. Thus, the present study shows the development and validation of a DI-based method by ultra-high-performance liquid chromatography quadrupole-linear ion trap analyser (UHPLC-QqLIT-MS/MS). The proposed method was applied to the monitoring of 115 organic microcontaminants (including pharmaceuticals, TPs and pesticides) at the ngL/μgL level in wastewater effluents from urban WWTPs. Sample pre-treatment was reduced to acetonitrile addition and filtration of the mixture previous to LC-MS analysis. Total analysis time was <15min. A subsequent validation protocol was carried out in treated WW (TWW), following indications of SANTE and Eurachem Guidelines. Linearity and matrix effect were evaluated in the range of 10-1000ngL. 70% of the analytes showed a moderate matrix effect (≤25%). Trueness (expressed as recovery) and precision (calculated as relative standard deviation, RSD) were evaluated at four concentration levels (20, 50, 500 and 1000ngL) in TWW samples. The LODs ranged from 1 to 357ngL and the LOQs from 10 to 500ngL. 92% of the compounds showed limits of quantification ≤100ngL. In most cases, mean recoveries were in the range 70-120%, and RSD values were ≤20%. The validated method was successfully applied to the analysis of 10 TWW samples, demonstrating the occurrence of 67 target compounds at concentration levels from 26705ngL (4-aminoantipyrine) to 10ngL (tebuconazole and bezafibrate).
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http://dx.doi.org/10.1016/j.chroma.2017.05.053DOI Listing
July 2017