Instituto de Investigación en Análises Químicas e Biolóxicas (IIAQBUS)

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An Analysis of the Use of Systemic Antifungals (Fluconazole, Itraconazole, and Terbinafine) in Galicia, Spain, between 2019 and 2022
(MDPI, 2024) Vázquez Prieto, Severo; Vaamonde, Antonio; Paniagua Crespo, Esperanza; Universidade de Santiago de Compostela. Departamento de Microbioloxía e Parasitoloxía
In the present work, we examined the consumption of systemic antifungals (fluconazole, itraconazole, and terbinafine) in outpatients in the four provinces of Galicia, Spain, between 2019 and 2022. We also described the variability in the use of these types of drugs between these provinces. In addition, we detected any deviation in consumption at a seasonal level and analyzed possible changes during the study period. A descriptive, cross-sectional, and retrospective study of the use of antifungals, expressed in terms of a defined daily dose per 1000 inhabitants per day, was carried out. The results obtained revealed statistically significant differences between provinces and by the active principle consumed in the four Galician provinces (p < 0.001), which can be explained by multiple factors. This study also revealed that there was stable consumption during the study period, with no significant seasonal differences observed. This study represents a contribution to the knowledge about the consumption of antifungals for systemic use in Galicia and serves as a basis for subsequent studies. This will allow us to understand the consumption patterns of these types of drugs and, ultimately, will help to establish stewardship strategies and prevent the development of resistance.
Study of the Use of Permethrin 5% Cream in Galicia (Spain) between 2018 and 2021
(MDPI, 2023) Vázquez Prieto, Severo; Vaamonde, Antonio; Paniagua Crespo, Esperanza; Universidade de Santiago de Compostela. Departamento de Microbioloxía e Parasitoloxía
Drug utilization studies can provide direct insights into how a drug is used in real-world conditions and can give a rough estimate of the proportion of the study population treated with it. In the present work, we examined the consumption of permethrin 5% cream in the four provinces of Galicia (a Spanish autonomous community) and described the seasonal variability and the annual evolution of its consumption between 2018 and 2021. A descriptive, cross-sectional, and retrospective study of the consumption of this drug, expressed in defined daily dose per 1000 inhabitants per day (DID), was carried out. The results obtained revealed differences between the amounts consumed in the four Galician provinces (p < 0.001). No specific geographical pattern was observed; however, the results suggested a marked seasonality and a slightly increasing global trend in the consumption of permethrin 5% cream throughout the study period. Since the only authorized indication of this drug in the study area is the treatment of scabies, this work may give an idea of the epidemiological situation of the disease in Galicia and serve to establish public health strategies against this parasitosis.
Study of the Use of Antinematode Drugs, Mebendazole and Pyrantel, in Galicia (Spain) from 2016 to 2020
(Wiley, 2022) Sánchez Prieto, Severo; Vaamonde, Antonio; Paniagua Crespo, Esperanza; Universidade de Santiago de Compostela. Departamento de Microbioloxía e Parasitoloxía
To the best of our knowledge, there is no study on the use of drugs focused on the consumption of antinematode drugs in any region of the world. In the present study, we analyzed and evaluated the use of mebendazole and pyrantel in the provinces of Galicia (Spain), as well as described the variability of the consumption of both drugs between these provinces from 2016 to 2020. A descriptive, cross-sectional, and retrospective study of the consumption of these drugs, expressed in defined daily dose per 1000 inhabitants per day (DHD), was carried out. The DHD values for both drugs were small, although clearly higher, both on average and in variability, in the case of mebendazole. The difference in the mean DHD between both drugs and the geographical differences observed was statistically significant. The seasonal differences were statistically significant for both active principles, with lower values in summer. The active principle most consumed in all the provinces and years was mebendazole. The main consequence of the excessive use of this drug compared to pyrantel may be the increased risk of the development of resistance and of therapeutic failure, as well as the consequent limitation of pharmacological options in the future.
Ozone injection system based on NETmix technology for quaternary treatment of urban wastewater
(Elsevier, 2025-04) Pituco, Mateus Mestriner; Marrocos, Paulo H.; Méndez, Sandra; Montes Goyanes, Rosa; Rodil Rodríguez, María del Rosario; Moreira, Francisca C.; Vilar, Vítor J. P.; Universidade de Santiago de Compostela. Departamento de Química Analítica, Nutrición e Bromatoloxía
An innovative high-intensity static mixer technology, known as NETmix, was applied as an ozone (O3) gas injection system to promote the quaternary treatment of urban wastewater (UWW), focusing on the elimination of contaminants of emerging concern (CECs). The NETmix network with an exclusive geometry boosts mass transfer rates and rapidly develops an O3-rich stream to react with CECs. The mixer operated in continuous mode promotes a rapid gas (O3)–liquid (water) dissolution. The ozonation process’ performance was evaluated for the abatement of 19 CECs spiked (10 μg dm−3 each) in demineralized water and two tertiary-treated UWW matrices, coming from (i) a secondary settler tank after a conventional activated sludge and (ii) the outlet of a membrane biological reactor (MBR). In addition, the ozonation system was tested for removing a broad range of CECs at natural trace levels from the UWW matrix coming from the MBR. In the realistic wastewater contamination scenario, a maximum transferred O3 dose of 1.28 and 0.76 resulted in removal values ≥80% for 12 out of the 19 spiked CECs from the secondary settler tank, and 9 out of the 19 spiked CECs from the post-MBR treatment, respectively, at a very short hydraulic residence time (55 s). Moreover, removals ≥80% were attained for 22 out of 25 CECs detected in the effluent from the MBR, applying a specific O3 dose of 0.6 . The enhanced ozone-water mass transfer provided by the NETmix technology enabled high removal efficiencies for CECs.
Redox cell signalling triggered by black carbon and/or radiofrequency electromagnetic fields: Influence on cell death
(Elsevier, 2024-09-05) López Martín, María Elena; Sueiro-Benavides, Rosana; Leiro Vidal, José Manuel; Rodríguez González, Juan Antonio; Ares Pena, Francisco José; Universidade de Santiago de Compostela. Departamento de Ciencias Morfolóxicas; Universidade de Santiago de Compostela. Departamento de Física Aplicada
The capacity of environmental pollutants to generate oxidative stress is known to affect the development and progression of chronic diseases. This scientific review identifies previously published experimental studies using preclinical models of exposure to environmental stress agents, such as black carbon and/or RF-EMF, which produce cellular oxidative damage and can lead to different types of cell death. We summarize in vivo and in vitro studies, which are grouped according to the mechanisms and pathways of redox activation triggered by exposure to BC and/or EMF and leading to apoptosis, necrosis, necroptosis, pyroptosis, autophagy, ferroptosis and cuproptosis. The possible mechanisms are considered in relation to the organ, cell type and cellular-subcellular interaction with the oxidative toxicity caused by BC and/or EMF at the molecular level. The actions of these environmental pollutants, which affect everyday life, are considered separately and together in experimental preclinical models. However, for overall interpretation of the data, toxicological studies must first be conducted in humans, to enable possible risks to human health to be established in relation to the progression of chronic diseases. Further actions should take pollution levels into account, focusing on the most vulnerable populations and future generations.
Identification of hazardous organic compounds in e-waste plastic using non-target and suspect screening approaches
(Elsevier, 2024-04-09) Castro Varela, Gabriela; Cobo Golpe, Miguel; Rodríguez Pereiro, Isaac; Universidade de Santiago de Compostela. Departamento de Química Analítica, Nutrición e Bromatoloxía
End-of-life electric and electronic devices stand as one of the fastest growing wastes in the world and, therefore, a rapidly escalating global concern. A relevant fraction of these wastes corresponds to polymeric materials containing a plethora of chemical additives. Some of those additives fall within the category of hazardous organic compounds (HOCs). Despite the significant advances in the capabilities of analytical methods, the comprehensive characterization of WEEE plastic remains as a challenge. This research strives to identify the primary additives within WEEE polymers by implementing a non-target and suspect screening approach. Gas chromatography coupled to time-of-flight mass spectrometry (GC-QTOF-MS), using electron ionization (EI), was applied for the detection and identification of more than 300 substances in this matrix. A preliminary comparison was carried out with nominal resolution EI-MS spectra contained in the NIST17 library. BPA, flame retardants, UV-filters, PAHs, and preservatives were among the compounds detected. Fifty-one out of 300 compounds were confirmed by comparison with authentic standards. The study establishes a comprehensive database containing m/z ratios and accurate mass spectra of characteristic compounds, encompassing HOCs. Semi-quantification of the predominant additives was conducted across 48 WEEE samples collected from handling and dismantling facilities in Galicia. ABS plastic demonstrated the highest median concentrations, ranging from 0.154 to 4456 μg g−1, being brominated flame retardants and UV filters, the families presenting the highest concentrations. Internet router devices revealed the highest concentrations, containing a myriad of HOCs, such as tetrabromobisphenol A (TBBPA), tribromophenol (TBrP), triphenylphosphate (TPhP), tinuvin P and bisphenol A (BPA), most of which are restricted in Europe
Predicting concentrations of volatile and semi-volatile compounds in indoor areas through analysis of condensed water samples. A proof of concept
(Elsevier, 2024) Cobo Golpe, María; Ramil Criado, María; Pérez Mayán, Leticia; Rodríguez Pereiro, Isaac; Universidade de Santiago de Compostela. Departamento de Ciencias Forenses, Anatomía Patolóxica, Xinecoloxía e Obstetricia, e Pediatría; Universidade de Santiago de Compostela. Departamento de Química Analítica, Nutrición e Bromatoloxía
Atmospheres from indoor areas contain a range of volatile and semi-volatile compounds to which inhabitants are exposed through breathing. Despite different qualitative approaches have been proposed for the identification of compounds associated to the vapor phase of confined areas, active sampling remains as the preferred technique when quantitative data is required. Herein, we investigate the correlations existing between concentrations in air and water condensates obtained from indoor areas. To this end, samples of both matrices were simultaneously collected and analyzed by gas chromatography mass spectrometry. After validation of sample concentration approaches for a selection of compounds, the effect of different operational conditions, and environmental variables, in their concentrations in condensed water was assessed. Levels in this matrix were hardly affected by sampling time, air flow through the dehumidifier device, and the environmental temperature and humidity. Thus, air water distribution coefficients (Kaw) could be estimated for fourteen out of sixteen pre-selected compounds. These values permitted a semiquantitative evaluation of their concentrations existing in air from different areas. In case of semi-volatile compounds (i.e. phenol, benzothiazole, phthalates), with log Kaw below −4.8, analysis of 50 mL water samples permitted to achieve lower limits of quantification than active air sampling for 3 h at a flowrate of 1 m3 h−1
Multifunctional polymeric guanidine and hydantoin halamines with broad biocidal activity
(Elsevier, 2024) Bromberg, Lev; Magariños Ferro, Beatriz; Torres, Beatriz S.; Santos Rodríguez, Ysabel; Concheiro Nine, Ángel Joaquín; Hatton, T. Alan; Álvarez Lorenzo, Carmen; Universidade de Santiago de Compostela. Departamento de Farmacoloxía, Farmacia e Tecnoloxía Farmacéutica; Universidade de Santiago de Compostela. Departamento de Microbioloxía e Parasitoloxía
Prolonged and excessive use of biocides during the coronavirus disease era calls for incorporating new antiviral polymers that enhance the surface design and functionality for existing and potential future pandemics. Herein, we investigated previously unexplored polyamines with nucleophilic biguanide, guanidine, and hydantoin groups that all can be halogenated leading to high contents of oxidizing halogen that enables enhancement of the biocidal activity. Primary amino groups can be used to attach poly(N-vinylguanidine) (PVG) and poly(allylamine-co-4-aminopyridine-co-5-(4-hydroxybenzylidene)hydantoin) (PAH) as well as a broad-spectrum commercial biocide poly(hexamethylene biguanide) (PHMB) onto a solid support. Halogenation of polymer suspensions was conducted through in situ generation of excess hypobromous acid (HBrO) from bromine and sodium hydroxide or by sodium hypochlorite in aqueous solutions, resulting in N-halamines with high contents of active > N-Br or > N-Cl groups. The virucidal activity of the polymers against human respiratory coronavirus HCoV-229E increased dramatically with their halogenation. Brominated PHMB-Br showed activation activity value > 5 even at 1 mg/L, and complete virus inhibition was observed with either PHMB-Br or PAH-Br at 10 mg/mL. Brominated PVG-Br and PAH-Br possessed fungicidal activity against C. albicans, while PHMB was fungistatic. PHMB, PHMB-Br and PAH polymers demonstrated excellent bactericidal activity against the methicillin-resistant S. aureus and vancomycin-resistant E. faecium. Brominated polymers (PHMB-Br, PVG-Br, PAH-Br) were not toxic to the HeLa monolayers, indicating acceptable biocompatibility to cultured human cells. With these features, the N-halamine polymers of the present study are a worthwhile addition to the arsenal of biocides and are promising candidates for development of non-leaching coatings
Physicochemical Properties and Microbiome of Vineyard Soils from DOP Ribeiro (NW Spain) Are Influenced by Agricultural Management
(MDPI, 2024) Blanco Camba, Pilar; Rodríguez Pereiro, Isaac; Fernández Fernández, Victoria; Ramil Criado, María; Alonso Vega, Flora; Universidade de Santiago de Compostela. Departamento de Química Analítica, Nutrición e Bromatoloxía
Agricultural management influences the soil ecosystem by affecting its physicochemical properties, residues of pesticides and microbiome. As vineyards grow crops with the highest incidence of pesticides, the aim of this study was to evaluate the impact of conventional and sustainable management systems of vineyards from DOP Ribeiro on the soil’s condition. Samples from soils under three different management systems were collected, and the main soil physicochemical properties were evaluated. A selection of 50 pesticides were investigated by liquid chromatography with tandem mass spectrometry. The bacterial and fungal microbiomes were characterized through amplicon sequencing. The results show that organic agriculture positively influences soil pH and the concentration of some nutrients compared to conventional management. Our microbiome analysis demonstrated that transitioning from conventional to organic management significantly improves several BeCrop® indexes related to key microbial metabolism and soil bio-sustainability. Such a transition does not affect soil alpha diversity, but leads to a higher interconnected microbial network structure. Moreover, differential core genera and species for each management system are observed. In addition, the correlation of the microbiome with geographical distance is evidence of the existence of different microbial terroirs within DOP Ribeiro. Indeed, sustainable management leads to higher nutrient availability and enhances soil health in the short term, while lowering pesticide usage
Removal of the waterborne parasite Cryptosporidium parvum from drinking water using granular activated carbon
(Elsevier, 2023) Couso Pérez, Seila; Abeledo Lameiro, María Jesús; Vidal Varela, Ana Isabel; Gómez Couso, Hipólito; Universidade de Santiago de Compostela. Departamento de Microbioloxía e Parasitoloxía
Cryptosporidium is a genus of apicomplexan parasites that infect the gastrointestinal tract of a wide range of vertebrate hosts, including humans. These enteropathogens are commonly detected in surface waters and Cryptosporidium is responsible of numerous waterborne outbreaks in industrialised countries. Filters of granular activated carbon (GAC) are mainly used to eliminate emerging micropollutants or control unpleasant odour and taste in drinking water. Recently, GAC has been also employed for removal of microorganisms from different types of water. This work evaluates the capability of GAC in the elimination of the infective forms of Cryptosporidium parvum (oocysts) from drinking water. For this, well water was spiked with oocysts of C. parvum and passed through a chromatographic column filled with fresh GAC at different bed heights (5–50 cm) and a filtration rate of 100 mL/min, approximately. By immunofluorescence microscopy, the number of oocysts in the water samples was determined. The logarithmic reduction (LR) was calculated by comparing the number of oocysts quantified in the filtered samples and the corresponding influent samples. High efficiencies of GAC in removing C. parvum oocysts from water were obtained. Thus, with a bed height of 35 cm, removal efficiencies > 2 LR were achieved. The highest LR (3.47 ± 0.31) was observed when a GAC bed height of 50 cm was used. Taking into account the results obtained, C. parvum oocysts were eliminated remarkably and, therefore, GAC adsorption filters may be considered additional barriers against this waterborne enteropathogen in drinking water at the household level in developing countries.
Occurrence and risk assessment of pesticides and pharmaceuticals in viticulture impacted watersheds from Northwest Spain
(Elsevier, 2023) Fernández Fernández, Victoria; Ramil Criado, María; Cela Torrijos, Rafael; Rodríguez Pereiro, Isaac; Universidade de Santiago de Compostela. Departamento de Química Analítica, Nutrición e Bromatoloxía
An automated analytical methodology was developed, validated and applied to monitor 73 organic pollutants (pesticides and pharmaceuticals) in surface and groundwater samples obtained in watersheds from an intensive viticulture, rural region, in the Northwest of Spain. Filtered samples were concentrated using a reusable solid-phase extraction sorbent, on-line combined with liquid chromatography tandem mass spectrometry (LC-MS/MS). The analytical procedure achieved limits of quantification between 1 ng L−1 and 10 ng L−1, with a throughput of 2 samples hour−1, providing accurate recoveries for more than 90% of the 73 selected compounds, using calibration solutions prepared in ultrapure water (in presence of methanol and formic acid) as neat solvent. The distribution and the concentrations of pesticides in small streams impacted by discharges of treated municipal wastewaters were different in rural and residential areas. On the other hand, pharmaceuticals showed a similar distribution in both streams. In surface waters from viticulture impacted watersheds, with a limited influence of municipal wastewaters, pulses of pesticides were noticed, with values above 100 ng L−1 for several fungicides. Cardiovascular pharmaceuticals, psychiatric drugs and/or their transformation products were also ubiquitous in these samples, with low, but relatively stable concentrations among sampling campaigns. Within the suite of investigated compounds, maximum pesticide residues remained below their predicted-non effect concentration (PNEC) in all samples. On the other hand, the environmental concentrations of the cardiovascular drug olmesartan stayed systematically above its PNEC in fresh water samples
Assessment of the occurrence and interaction between pesticides and plastic litter from vineyard plots
(Elsevier, 2023) Cobo Golpe, Miguel; Blanco Camba, Pilar; Fernández Fernández, Victoria; Ramil Criado, María; Rodríguez Pereiro, Isaac; Universidade de Santiago de Compostela. Departamento de Química Analítica, Nutrición e Bromatoloxía
In this research, aged plastic fragments collected from vineyards were characterized in terms of composition, residues of pesticides, and their potential to exchange these compounds with the aquatic media. To this end, we employed the qualitative and quantitative information provided by complementary analytical techniques, including chromatography, organic and inorganic mass spectrometry, infrared spectroscopy and electronic microscopy. Debris of weathered plastics were identified as polypropylene and polyethylene, containing different types of additives, from organic UV stabilizers to inorganic fillers, such as calcium salts. Regardless of polymer type, plastic litter collected from vineyards contained residues of pesticides, and particularly of fungicides, with total concentrations in the range of values from 114 ng g 1 to 76.4 μg g 1. Data obtained under different extraction conditions suggested that a fraction of these compounds was absorbed in aged polymers, penetrating inside the material. The parallel analysis of plastic litter and vineyard soils reflected higher pesticide residues in the former matrix. Furthermore, several fungicides, considered as labile in vineyard soils (i.e. zoxamide and folpet), were those showing the highest levels in plastic litter. Simulated sorption-desorption studies, with plastic debris in contact with surface water, demonstrated the higher affinity of aged materials by moderately polar pesticides than their new counterparts. For the first time, the manuscript highlights the presence of plastic litter in vineyards soils, reflecting the accumulation of several fungicides in this matrix, in some cases, with a different stability pattern to that observed in the soil from same vineyards
The HL-60 human promyelocytic cell line constitutes an effective in vitro model for evaluating toxicity, oxidative stress and necrosis/apoptosis after exposure to black carbon particles and 2.45 GHz radio frequency
(Elsevier, 2023-01-09) Benavides, Rosa Ana Sueiro; Leiro Vidal, José Manuel; Rodríguez González, Juan Antonio; Ares Pena, Francisco José; López Martín, María Elena; Universidade de Santiago de Compostela. Departamento de Ciencias Morfolóxicas; Universidade de Santiago de Compostela. Departamento de Física Aplicada; Universidade de Santiago de Compostela. Departamento de Microbioloxía e Parasitoloxía
The cellular and molecular mechanisms by which atmospheric pollution from particulate matter and/or electromagnetic fields (EMFs) may prove harmful to human health have not been extensively researched. We analyzed whether the combined action of EMFs and black carbon (BC) particles induced cell damage and a pro-apoptotic response in the HL-60 promyelocytic cell line when exposed to 2.45 GHz radio frequency (RF) radiation in a gigahertz transverse electromagnetic (GTEM) chamber at sub-thermal specific absorption rate (SAR) levels. RF and BC induced moderately significant levels of cell damage in the first 8 or 24 h for all exposure times/doses and much greater damage after 48 h irradiation and the higher dose of BC. We observed a clear antiproliferative effect that increased with RF exposure time and BC dose. Oxidative stress or ROS production increased with time (24 or 48 h of radiation), BC dose and the combination of both. Significant differences between the proportion of damaged and healthy cells were observed in all groups. Both radiation and BC participated separately and jointly in triggering necrosis and apoptosis in a programmed way. Oxidative-antioxidant action activated mitochondrial anti-apoptotic BCL2a gene expression after 24 h irradiation and exposure to BC. After irradiation of the cells for 48 h, expression of FASR cell death receptors was activated, precipitating the onset of pro-apoptotic phenomena and expression and intracellular activity of caspase-3 in the mitochondrial pathways, all of which can lead to cell death. Our results indicate that the interaction between BC and RF modifies the immune response in the human promyelocytic cell line and that these cells had two fates mediated by different pathways: necrosis and mitochondria-caspase dependent apoptosis. The findings may be important in regard to antimicrobial, inflammatory and autoimmune responses in humans
Are fish populations at risk? Metformin disrupts zebrafish development and reproductive processes at chronic environmentally relevant concentrations
(ACS, 2022-12-29) Barros, Susana; Alves, Nélson; Pinheiro, Marlene; Ribeiro, Marta; Morais, Hugo; Santos, Miguel M.; Montes Goyanes, Rosa; Coimbra, Ana M.; Neuparth, Teresa; Rodil Rodríguez, María del Rosario; Quintana Álvarez, José Benito; Universidade de Santiago de Compostela. Departamento de Química Analítica, Nutrición e Bromatoloxía; Universidade de Santiago de Compostela. Instituto de Investigación e Análises Alimentarias
The antidiabetic drug Metformin (MET), one of the most prevalent pharmaceuticals in the environment, is currently detected in surface waters in the range of ng/L to low μg/L. As current knowledge regarding the long-term effects of environmentally relevant concentrations of MET in nontarget organisms is limited, the present study aimed at investigating the generational effects of MET, in concentrations ranging from 390 to 14 423 ng/L in the model organism Danio rerio (up to 9 mpf), including the effects on its nonexposed offspring (until 60 dpf). We integrate several apical end points, i.e., embryonic development, survival, growth, and reproduction, with qRT-PCR and RNA-seq analyses to provide additional insights into the mode of action of MET. Reproductive-related parameters in the first generation were particularly sensitive to MET. MET parental exposure impacted critical molecular processes involved in the metabolism of zebrafish males, which in turn affected steroid hormone biosynthesis and upregulated male vtg1 expression by 99.78- to 155.47-fold at 390 and 14 432 MET treatment, respectively, pointing to an estrogenic effect. These findings can potentially explain the significant decrease in the fertilization rate and the increase of unactivated eggs. Nonexposed offspring was also affected by parental MET exposure, impacting its survival and growth. Altogether, these results suggest that MET, at environmentally relevant concentrations, severely affects several biological processes in zebrafish, supporting the urgent need to revise the proposed Predicted No-Effect Concentration (PNEC) and the Environmental Quality Standard (EQS) for MET
A new analytical method to determine trace level concentrations of pharmaceuticals in influent wastewater: a tool to monitor human use patterns
(Elsevier, 2023) Fontanals Torroja, Núria; Pocurull Aixala, Eva; Rodríguez Mozaz, Sara; Montes Goyanes, Rosa; González Mariño, Iria; Santana Vieira, Sergio; Miró Lladó, Manuel; Rico Artero, Andreu; Borrull Ballarín, Francesc; Quintana Álvarez, José Benito; Marcé Recasens, Rosa Maria; Universidade de Santiago de Compostela. Departamento de Química Analítica, Nutrición e Bromatoloxía; Universidade de Santiago de Compostela. Instituto de Investigación e Análises Alimentarias
The occurrence of pharmaceuticals in influent wastewater samples (IWW) is a recurrent issue. The monitoring of their presence is not only valuable from an environmental point of view, but also as a tool to analyze patterns of human use by the so-called wastewater-based epidemiology. The development of an analytical method based on solid-phase extraction followed by liquid chromatography coupled to tandem mass spectrometry to monitor the occurrence of a group of seventeen pharmaceuticals including the most representative for various therapeutic families in IWW samples is described in this work. The samples were collected during a monitoring week in six wastewater treatment plants located in different cities and towns across Spain. The developed method provides acceptable figures of merit with apparent recoveries in IWW ranging from 42% to 139%, and low matrix effect (in general lower than ± 30%), and method quantification limits (MQL) between 1 ng/L and 24 ng/L for all compounds, except atenolol (58 ng/L). All the studied pharmaceuticals were found in all samples with concentrations ranging from < MQL to 10,393 ng/L, being the highest concentrations for tramadol. The population normalized daily loads revealed that the use of pharmaceuticals follows, in general, a similar pattern in all cities monitored.
Assessing the impact of a major electronic music festival on the consumption patterns of illicit and licit psychoactive substances in a Mediterranean city using wastewater analysis
(Elsevier, 2023) Senta, Ivan; Krizman-Matasic, Ivona; Kostanjevecki, Petra; González Mariño, Iria; Mikac, Iva; Terzic, Senka; Ahel, Marijan; Rodil Rodríguez, María del Rosario; Quintana Álvarez, José Benito; Universidade de Santiago de Compostela. Departamento de Química Analítica, Nutrición e Bromatoloxía; Universidade de Santiago de Compostela. Instituto de Investigación e Análises Alimentarias
The consumption patterns of five categories of psychoactive substances (PS), including “conventional” illicit drugs, new psychoactive substances (NPS), therapeutic opioids, alcohol and nicotine, were studied in the city of Split, Croatia, using wastewater-based epidemiology (WBE), with an emphasis on the impact of a large electronic music festival. The study involved the analysis of 57 urinary biomarkers of PS in raw municipal wastewater samples collected in three characteristic periods, including the festival week in the peak-tourist season (July) and reference weeks in the peak-tourist season (August) and the off-tourist season (November). Such a large number of biomarkers allowed the recognition of distinct patterns of PS use associated with the festival, but also revealed some subtle differences between summer and autumn seasons. The festival week was characterized by markedly increased use of illicit stimulants (MDMA: 30-fold increase; cocaine and amphetamine: 1.7-fold increase) and alcohol (1.7-fold increase), while consumption of other common illicit drugs (cannabis and heroin), major therapeutic opioids (morphine, codeine and tramadol) and nicotine remained rather constant. Interestingly, NPS and methamphetamine clearly contributed to the festival PS signature in wastewater, but their prevalence was rather low compared to that of common illicit drugs. Estimates of cocaine and cannabis use were largely consistent with prevalence data from national surveys, whereas differences were found for typical amphetamine-type recreational drugs, particularly MDMA, and for heroin. The WBE data suggest that the largest proportion of morphine came from heroin consumption and that the percentage of heroin users seeking treatment in Split is probably rather low. The prevalence of smoking calculated in this study (30.6 %) was consistent with national survey data for 2015 (27.5–31.5 %), while the average alcohol consumption per capita >15 years (5.2 L) was lower than sales statistics suggest (8.9 L)
Efficient Validation Strategies in Environmental Analytical Chemistry: A Focus on Organic Micropollutants in Water Samples
(Annual Reviews, 2023) Hernández Hernández, Félix; Fabregat Safont, David; Campos Mañas, Marina Celia; Quintana Álvarez, José Benito; Universidade de Santiago de Compostela. Departamento de Química Analítica, Nutrición e Bromatoloxía; Universidade de Santiago de Compostela. Instituto de Investigación e Análises Alimentarias
This article critically reviews analytical method validation and quality control applied to the environmental chemistry field. The review focuses on the determination of organic micropollutants (OMPs), specifically emerging contaminants and pesticides, in the aquatic environment. The analytical technique considered is (gas and liquid) chromatography coupled to mass spectrometry (MS), including high-resolution MS for wide-scope screening purposes. An analysis of current research practices outlined in the literature has been performed, and key issues and analytical challenges are identified and critically discussed. It is worth emphasizing the lack of specific guidelines applied to environmental analytical chemistry and the minimal regulation of OMPs in waters, which greatly affect method development and performance, requirements for method validation, and the subsequent application to samples. Finally, a proposal is made for method validation and data reporting, which can be understood as starting points for further discussion with specialists in environmental analytical chemistry.
Ozone membrane contactor for tertiary treatment of urban wastewater: Chemical, microbial and toxicological assessment
(Elsevier, 2023) Presumido, Pedro H.; Soares, Sara Ribeirinho; Ribeiro, Marta; Neuparth, Teresa; Santos, Miguel M.; Feliciano, Manuel; Nunes, Olga C.; Gomes, Ana I.; Vilar, Vítor J. P.; Montes Goyanes, Rosa; Quintana Álvarez, José Benito; Rodil Rodríguez, María del Rosario; Universidade de Santiago de Compostela. Departamento de Química Analítica, Nutrición e Bromatoloxía; Universidade de Santiago de Compostela. Instituto de Investigación e Análises Alimentarias
A membrane ozone contactor, operated under continuous mode, was applied to promote the tertiary treatment of urban wastewater (UWW), targeting the removal of contaminants of emerging concern (CECs), bacterial disinfection, and toxicity reduction. This system relies on the homogeneous radial distribution of ozone (O3) in the reaction zone by “titration” through a microfiltration borosilicate tubular membrane, while the UWW swirls around the membrane and drags the O3 microbubbles generated in the membrane shell-side. The membrane is coated with titanium dioxide (TiO2-P25) and radiation can be externally supplied via four UV lamps. The ozonation tests were carried out with secondary-treated UWW collected in different seasons (winter and summer) and spiked with a mix of 19 CECs (10 μg L−1 each). For an O3 dose of 18 g m−3, the best performance was obtained by increasing the O3 concentration (maximum [O3]G,inlet of 200 g Nm−3) and decreasing the gas flow rate (minimum QG of 0.15 Ndm3 min−1), providing the highest ozone transfer yield (88 %) and, thus higher specific ozone dose (g O3 per g dissolved organic carbon). Under these conditions, removals >80 % or concentrations below the limit of quantification were obtained for up to 13 of the 19 CECs and reductions up to 5 log units for total heterotrophs and below the limit of detection for enterobacteria and enterococci. Tests including a UVC dose of 0.10 kJ L−1 enhanced disinfection ability but had no impact on CECs oxidation. After ozonation, the abundance of antibiotic resistant bacteria was reduced but not eliminated, and microbial regrowth after 3-day storage was observed. No toxic effect was detected on zebrafish embryos using a dilution factor of 4 for the ozonized UWW and when granular activated carbon adsorption was subsequently applied the dilution factor decreased to 2
Ozone membrane contactor to intensify gas/liquid mass transfer and contaminants of emerging concern oxidation
(Elsevier, 2022) Presumido, Pedro H.; Montes Goyanes, Rosa; Quintana Álvarez, José Benito; Rodil Rodríguez, María del Rosario; Feliciano, Manuel; Li Puma, Gianluca; Gomes, Ana I.; Vilar, Vítor J. P.; Universidade de Santiago de Compostela. Departamento de Química Analítica, Nutrición e Bromatoloxía; Universidade de Santiago de Compostela. Instituto de Investigación e Análises Alimentarias
A tubular porous borosilicate membrane contactor was investigated for ozone gas/water mass transfer and the removal of contaminants of emerging concern (CECs) in water. Ozone gas/water contact occurs on the membrane shell-side, which is coated with a photocatalyst (TiO2-P25), as the ozone gas stream is fed from the lumen side and permeates through the pores generating micro-sized ozone bubbles uniformly delivered to the annular reaction zone where the contaminated water to be treated flows. Under continuous flow, water pH at 3.0 and temperature at 20 ºC, the volumetric mass transfer coefficient (KLa) ranged from 3.5 to 9.0 min−1 and improved with the increase of gas flow rate (QG, 1.5-fold from 0.15 to 1.0 Ndm3 min−1) and liquid flow rate (QL, 2.0-fold from 20 to 50 L h−1), due to enhanced turbulence on the membrane shell-side and annular zone. The mass transfer efficiency was more pronounced as the QG decreased and the QL increased, which is advantageous for large-scale applications. The main resistances to ozone transfer were in the water phase boundary layer (53–76%) and in the membrane (24–47%; kM = (1.14 ± 0.01) × 10−4 m s−1). For an ozone dose of 12 g m−3 and residence time of 3.9 s, removals ≥ 80% were achieved for 13 of 19 CECs spiked in demineralized water (each 10 µg L−1), demonstrating the applicability of this membrane contactor for ozonation treatment. Photocatalytic ozonation (O3/UVC/TiO2) did not significantly improve the treatment performance due to the low residence time inside the contactor.
A real-time quantitative PCR assay using hydrolysis probes for monitoring scuticociliate parasites in seawater
(Elsevier, 2022) Sueiro Benavides, Rosa Ana; Lamas Fernández, Jesús; Palenzuela, Oswaldo; Gulías Otero, Paola; Díez-Vives, Cristina; García Ulloa, Alba; Leiro Vidal, José Manuel; Universidade de Santiago de Compostela. Centro de Investigación en Química Biolóxica e Materiais Moleculares; Universidade de Santiago de Compostela. Departamento de Bioloxía Funcional; Universidade de Santiago de Compostela. Departamento de Microbioloxía e Parasitoloxía
Scuticociliatosis is a serious disease that affects flatfish during culture and against which no effective control measures have yet been developed. Monitoring parasite levels in the water may be a valuable way of establishing the risk of infection and enabling appropriate control measures to be taken, thus representing an advance in controlling the disease. To achieve this objective, we have designed a quantitative real-time PCR (qPCR) assay using primers (f / r ITS2) and a hydrolysis probe that specifically amplify a region of the internal transcribed spacer 2 (ITS2) of the main aetiological agents of scuticociliatosis: Philasterides dicentrarchi and Miamiensis avidus. The slope (m), efficiency (E) and linearity (R2) determined from the standard curves generated are within the optimal values for qPCR. The high analytical sensitivity of the qPCR assay enables quantification of less than 120 pg of DNA per μL of reaction and detection of 1 ciliate per assay. The qPCR assay also exhibits high precision, with intra- and inter-assay coefficients of variation (CV) of respectively 0.27 and 7.57%. The protocol developed for isolating and quantifying ciliates seawater samples it has a recovery efficiency greater than 75% when the ciliate levels are between 103 and 2 × 103 ciliates/L and the turbidity of the water does not exceed one nephelometric turbidity unit (NTU). The real-time qPCR assay developed is a useful and appropriate tool for the specific and sensitive monitoring of scuticociliates in the water used in flatfish farms, enabling the establishment of effective prevention and control programmes

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