Artículos (Química Analítica)

URI permanente para esta colecciónhttps://hdl.handle.net/11441/10909

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Potential Application of a Synthetic Organo-funtionalized High Load Expandable Mica as Drug Carrier for Controlled Release.
(Bentham Science Publishers, 2021) Orta Cuevas, María del Mar; Maisanaba Hernández, Sara; Medina Carrasco, Santiago; Jos Gallego, Ángeles Mencía; Química Analítica; Nutrición y Bromatología, Toxicología y Medicina Legal
Background: In this work the cytotoxicity and gastric and gastrointestinal resistance of a high-load synthetic expandable mica, Na-mica-4, is studied for the first time. The hydrophilic character of this clay mineral can be modified by ion exchange reaction between Na+ inorganic cations housed in the interlayer space, and surfactant molecules, resulting in the formation of an organophilic material. This adsorption capability of organic compounds makes them very useful for a wide range of applications, such as their use as drug carriers. Previous studies have shown the high adsorption capacity of organofunctionalized Na-mica-4 of different types of drugs. Objetive: To carry out initial trials aimed at testing the cytotoxicity of a synthetic organofunctional expandable mica and evaluating its resistance to gastric and gastrointestinal digestion. Methods: A highly charged sodium mica (Na-mica-4) was synthesized and organofunctional by cationic exchange with an alkylamine, primary amine of 18 carbon atoms (C18-mica-4). Both were characterized by X-ray diffraction, field transmission electron microscopy, surface-specific analysis, differential scanning calorimetry, and thermal gravimetric analysis. In addition, screening cytotoxicity trials were conducted on the human intestinal cell line Caco-2 with C18-mica-4 (0-125 μg/ml). Results: Only one of the endpoints evaluated (the reduction of tetrazolium MTS salt by dehydrogenase enzymes) showed a significant decrease in cellular viability after 48h at the highest concentration tested. C18-mica-4 shows structural resistance to both, gastric and gastrointestinal, digestion. Conclusion: A successful development of a functionalized mica has been made with a promising potential application as a carrier to the drug.
Dietary freeze-dried beer prevents inflammation in DSS-induced chronic ulcerative colitis in mice
(Royal Society of Chemistry, 2025-07-01) Paredes Sánchez, María; Muñoz García, Rocío; Ávila Román, Francisco Javier; Lobo Prieto, Ana; Orta Cuevas, María del Mar; García González, Diego L.; Vázquez Román, María Victoria; Talero Barrientos, Elena Mª; Sánchez Hidalgo, Marina; Farmacología; Química Analítica; Citología e Histología Normal y Patológica
Inflammatory bowel disease (IBD) is a complex condition that is influenced by numerous factors, including genetic, immune and environmental factors. In the search for new therapies, nutritional interventions including dietary polyphenols are becoming increasingly important in the management of IBD. The present study aimed to investigate the antioxidant and anti-inflammatory effects of commercial freeze-dried beer, an interesting product resulting from the fermentation of cereals, rich in polyphenols, in (I) an in vitro model of inflammation using lipopolysaccharide (LPS)-stimulated THP-1 human derived macrophages and (II) a murine dextran sodium sulfate (DSS)-induced chronic colitis model, for elucidating the action mechanism involved. According to the results, commercial freeze-dried beer exhibits antioxidant, anti-inflammatory and immunomodulatory properties in LPS-stimulated THP-1 human macrophages by reducing reactive oxygen species (ROS), tumor necrosis factor (TNF)-α and interleukin (IL)-6 levels. Moreover, in vivo results showed that preventive treatment with dietary freeze-dried beer improved murine DSS-induced chronic colitis by attenuation of the clinical and histological signs of colonic damage. Colonic cytokine levels in animals fed with commercial freeze-dried beer reached values near basal levels. In addition, pro-inflammatory cyclooxygenase (COX)-2 and microsomal prostaglandin E synthase (mPGES)-1 protein expressions were significantly downregulated via inhibition of nuclear transcription factor kappa B (NF-κB) translocation. This inhibition may be mediated by an induction of the antioxidant nuclear factor (erythroid-derived 2)-like 2 (Nrf2)/heme oxygenase-1 (HO-1) signaling pathway and a reduction of signal transducer and activator of transcription (STAT)-3 phosphorylation orchestrating its potent anti-inflammatory and immunomodulatory effects. Overall, our results suggest that dealcoholized beer may be effective in the management of immune-mediated inflammatory diseases in which macrophages are crucial, including IBD, providing clues for developing useful dietary interventions against inflammation-associated pathologies.
Feasibility Assessment on the Use of Near Infrared Hyperspectral Imaging for the Screening of Vitamin C Content and Total Soluble Solids in Strawberries
(Elsevier, 2025) Baca Bocanegra, Berta; Espinar García, Ana Isabel; Hernández Hierro, José Miguel; Escudero Gilete, María Luisa; Nogales Bueno, Julio; Universidad de Sevilla. Departamento de Química Analítica; Universidad de Sevilla. Departamento de Nutrición y Bromatología, Toxicología y Medicina Legal
At market, strawberries are usually picked based on their external attributes, basically surface color. However, internal parameters are also important for the final quality of the fruit and, therefore, can strongly influence acceptance by consumers. The development of analytical methods that allow the evaluation of the strawberry internal quality in a rapid, cost-effective and environmentally friendly way will improve competitiveness in the fruit industry and profitability at markets. In this study, a feasibility assessment on the use of near infrared hyperspectral imaging for the control of the internal quality of strawberries from Huelva (an important strawberry exporting region) has been carried out. For it, modified partial least square regressions have been performed for the screening of vitamin C and total soluble solids. The standard errors of prediction in external validation (4.71 mg/100 g and 1.28 °Brix respectively) demonstrate the potential of the analyzed technique for the proposed objective.
Chemical Society y Pharmaceutical Society of Great Britain: vidas paralelas
(Real Academia Nacional de Farmacia, 2024-06-30) García Asuero, Agustín; Universidad de Sevilla. Departamento de Química Analítica
En esta memoria se pasa revista a la creación e inicios de dos importantes,Sociedades científicas, la “Chemical Society of London”, y la “Pharmaceutical,Society of Great Britain”. Se advierte la semejanza en cuanto a su punto de partida,y establecimiento de objetivos concretos, e.g., la práctica de la química. Se,observan las diferencias en los criterios de admisión, más restrictivos por parte,de la “Chemical Society”. Ambas sociedades son fruto del proceso de,diferenciación de la ciencia, y de la reafirmación del sentir profesional y de los,derechos asociados a la práctica del oficio. Se pasa revista a personajes clave, en,los dos casos, resaltando en el de la “Chemical Society” la influencia alemana en,la química británica. La búsqueda de una sede que satisfaga las necesidades,materiales y el cumplimiento de las misiones encomendadas supone un largo,peregrinaje. La “Chemical Society of London” pasa a convertirse pronto en la,“Chemical Society” y más tarde pasa a formar la “Royal Society of Chemistry”. La,“Pharmaceutical Society of Great Britain” pasa a convertirse en el transcurso de,los años en la “Royal Pharmaceutical Society”.
Novel Bacterial Strains for Nonylphenol Removal in Water and Sewage Sludge: Insights from Gene Expression and Toxicity
(MDPI, 2025-06-06) Lara Moreno, Alba; Aguilar Romero, Inés; Madrid, Fernando; Villaverde, Jaime; Carlier, Jorge D.; Santos Morcillo, Juan Luis; Alonso Álvarez, Esteban; Morillo, Esmeralda; Universidad de Sevilla. Departamento de Microbiología y Parasitología; Universidad de Sevilla. Departamento de Química Analítica; Junta de Andalucía; European Union (UE); Fundação para a Ciência e a Tecnologia. Portugal
4-Nonylphenols (4-NPs) are persistent endocrine disruptors frequently found in wastewater treatment plant (WWTP) effluents and sewage sludge. This study evaluated the ability of eight bacterial strains that were isolated from sewage sludge to degrade 4-n-NP in an aqueous solution. Bacillus safensis CN12, Shewanella putrefaciens CN17, and Alcaligenes faecalis CN8 showed the highest degradation rates, removing 100%, 75%, and 74% of 4-n-NP (10 mg L⁻1), with DT50 values of 0.90, 8.9, and 10.4 days, respectively. Despite the reduction in 4-n-NP concentrations, ecotoxicity assays revealed that the resulting transformation products (TPs) were more toxic than the parent compound. To investigate the potential degradation mechanisms, in silico and gene expression analyses were conducted on B. safensis CN12, revealing a significant upregulation of the multicopper oxidase gene, cotA (7.25-fold), and the ring-cleaving dioxygenase gene, mhqO (13.9-fold). Although the CN12 strain showed potential for mineralization based on gene expression studies, this was not observed in the aqueous solution. However, when 4-n-NP was adsorbed on sludge and treated with CN12 in the presence of hydroxypropyl-β-cyclodextrin (HPBCD) as a bioavailability enhancer, mineralization reached up to 33%, indicating a synergistic effect with the native sludge microbiota.
Curcumin-Loaded High-Charge Swelling Synthetic Mica: Characterization Studies and Stability under Stress Conditions
(American Chemical Society (ACS), 2025-05-23) Orta Cuevas, María del Mar; Fernández Romero, Ana María; Rabasco Álvarez, Antonio María; Medina Carrasco, Santiago; González Rodríguez, María Luisa; Universidad de Sevilla. Departamento de Química Analítica; Universidad de Sevilla. Departamento de Farmacia y Tecnología Farmacéutica; Universidad de Sevilla
Curcumin (Cur) is a bioactive compound with various pharmacotherapeutic effects. However, its limited solubility and stability pose challenges for therapeutic applications. Clay minerals, such as montmorillonite (MMT) and high-charge swelling synthetic micas, show promise as drug carriers due to their properties. This study aimed to obtain complexes with clay minerals that could enhance the stability of Cur. MMT, Na-Mica-4, and the latter organofunctionalized with 18-carbon alkylamines (C18-Mica-4) were used as support for Cur. Adsorption studies showed that Na-Mica-4 exhibited the highest percentage of adsorption (60%). Cur-Mica-4 complexes were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), thermal analysis (DSC and TGA), specific surface area (BET), pore size and volume determinations, and surface charge determination by zeta potential measurement. The effect of light on Cur and Cur-Mica-4 complexes was also evaluated. Forced degradation studies were performed under hydrolytic, oxidative, photolytic, and thermal conditions to assess the stability and degradation pathways. The FTIR spectra indicated that the enol tautomer mainly formed part of the complexes. BET analysis showed a reduced pore size after adsorption, indicating Cur immobilization. TGA and scanning electron microscopy (SEM) suggested degradation primarily occurring under exposure to sunlight, heat, and ultraviolet light. The effect of acidic and basic conditions on the Cur-Mica-4 complex was evaluated. Under acidic conditions, a decrease in the specific surface area of the complex was observed, suggesting the formation of larger configurational structures. An increase in the specific surface area with a smaller pore size was observed in the basic medium, possibly due to the formation of new structures in the clay minerals, supported by XRD results. These findings indicate that the pH of the medium can significantly influence the structure and stability of the Cur-Mica-4 complex, which could have important implications for its application in specific environments, such as drug delivery systems.
Enantioselective toxicity of propranolol on marine diatoms: Assessing growth, energy metabolism and oxidative damage in Phaeodactylum tricornutum
(Elsevier , 2025) Arenas, Marina; Feijão, Eduardo; Duarte, Irina A; Fonseca, Vanessa F.; Aparicio Gómez, Irene; Alonso Álvarez, Esteban; Universidad de Sevilla. Departamento de Química Analítica; Fundação para a Ciência e a Tecnologia (FCT). Portugal
Concern about the presence of pharmaceuticals in aquatic systems has increased in recent years owing to their continued release and the impact they may have on non-target organisms. Over half of these pharmaceuticals are chiral, with enantiomers that may have different pharmacokinetics and effects. However, most studies on their toxicity in marine biota have used racemic mixtures, ignoring the effects of isolated enantiomers. This work examines the potential enantioselective toxic effects of the chiral β-blocker propranolol, widely prescribed for cardiovascular diseases and migraines, and increasingly concerning due to its long-term use and raising consumption. This study used the diatom Phaeodactylum tricornutum as a model organism to assess the effect of each enantiomer on growth, photosynthesis, energy metabolism, and oxidative damage. The results showed that exposure of diatoms to R-propranolol induced growth inhibition due to deficiencies in photochemical metabolism, which was reflected in changes in the photosynthetic pigment profile. Oxidative stress also occurred in cells, resulting in lipid oxidation and DNA damage. In contrast, such effects were not observed for the S-enantiomer at the tested concentrations. This work shows the importance of considering enantiomer-specific effects in ecotoxicological assessments, as the two PRO enantiomers exhibit different toxicities in marine diatoms.
Rapid determination of phenylalanine and tyrosine in volumetrically collected dried blood spots using fully automated processing and analysis by capillary electrophoresis
(Elsevier, 2025-03-01) Aranda Merino, Noemí; Dvořák, Miloš; Kubáň, Pavel; Universidad de Sevilla. Departamento de Química Analítica; Czech Science Foundation; Czech Academy of Sciences
An off-the-shelf Agilent 7100 capillary electrophoresis (CE) instrument was employed for the automated processing and analysis of dried blood spots (DBSs) collected by Capitainer®B volumetric devices. Solutions for DBS elutions were transferred directly into CE vials through a separation capillary by the application of an auxiliary nitrogen gas connected to the external pressure line of the CE instrument. This allowed for liquid handling at pressures up to 15 bar and enabled the use of a single capillary for rapid DBS processing and efficient CE separations. The resulting DBS eluates were at-line injected into a short capillary end, which served for improved instrumental simplicity and short CE analysis times. The current set-up necessitated neither hardware nor software adjustments of the CE instrument, except for the connection of a gas cylinder to an in-built connector. The novel features presented in this study (DBSs with exact blood volumes, high external pressures, and short-end injections) were used for the automated determination of clinically relevant markers, phenylalanine (Phe) and tyrosine (Tyr), in DBS samples. Sensitive and selective Phe and Tyr quantification was achieved by CE-UV in 375 mM formic acid and 0.01 % (v/v) Tween 20 (pH 2.09) as a background electrolyte. The total processing and analysis times per one DBS were <1.5 and 4.5 min, respectively, in a sequence of 36 DBSs, and resulted in a sample throughput of >10 DBSs per hour. The intra- and inter-day repeatability values were better than 5.9 and 1.1 % RSD for peak areas and migration times, respectively, and calibration curves were linear in the 20–3000 μM (Phe) and 20–250 μM (Tyr) range (R2 ≥ 0.9973). The limits of detection were ≤2 μM and enabled the determination of endogenous Phe and Tyr concentrations as well as elevated Phe concentrations and Phe/Tyr ratios, which are the typical markers for neonatal phenylketonuria screening.
Functionalization of a clay mineral with Sn species for anti-inflammatory removal
(Elsevier, 2025-04-19) Gomes Oliveira, Lucilane; França, Denise B.; Oliveira, Luís H. de; Osajima, Josy A.; Silva-Filho, Edson C.; Sainz-Díaz, Ignacio; Medina-Carrasco, Santiago; Orta Cuevas, María del Mar; Fonseca, Maria G.; Universidad de Sevilla. Departamento de Química Analítica; Universidad de Sevilla
Diclofenac is one of the most detected drugs in aquatic environments, however, it can be removed through adsorption. In the present study, sodium bentonite (Na-Bent) was functionalized with an Sn species by reaction between the clay and aqueous SnCl2 solutions (0.01, 0.05 and 0.10 mol L-1), and used as new adsorbents for diclofenac. X-ray diffraction patterns with Rietveld refinement analysis indicated the presence of hydrated SnO2 or Sn(OH)4 nanoparticles in the samples. SnO2 content in the samples were 12.8, 32.4, and 45.0 % for Sn0.01-, Sn0.05- and Sn0.10-Bent, respectively. The specific surface area of the samples increased, reaching 194 m2 g−1 for Sn0.1-Bent. X-ray photoelectron spectroscopy (XPS) suggested the presence of Sn (IV) species in Sn-Bent. The adsorption isotherms indicated high drug adsorption, reaching 106.1 and 105.5 mg g−1 for Sn0.05- and Sn0.10-Bent samples, respectively. Fourier transform infrared (FT-IR) spectroscopy and XPS analyses showed an interaction between the carboxylate group of diclofenac sodium and the Sn species in the Sn-Bent samples. Artemia salina tests indicated that Sn0.10-Bent was not toxic, and all samples showed good stability during diclofenac adsorption at pH 6. Therefore, Sn-Bent samples behaved as environmentally friendly adsorbents for the removal of diclofenac.
Chemically Modified Polysaccharide Cryogels and their Performance in Ibuprofen Release
(Elsevier, 2025) da Silva Santos, Ariane María; Dias, Érico Rego; Osajima, Josy Antevelli; Orta Cuevas, María del Mar; da Silva Barud, Hernane; da Silva Filho, Edson Cavalcanti; Universidad de Sevilla. Departamento de Química Analítica; Consejo Nacional de Desarrollo Científico y Tecnológico (CNPq). Brasil; Research Support Foundation of the State of Piauí (FAPEPI). Brasil; São Paulo Research Foundation (FAPESP). Brasil
Alternative disease treatment methods, such as controlled drug release systems, provide the administration of specific medications at controlled rates over the long term, minimizing side effects resulting from toxicity and increasing the effectiveness of therapy. The main objective of the present work was to prepare cryogels based on babassu mesocarp and bacterial cellulose that was chemically modified through a copolymerization reaction with acrylamide for use in the controlled release of the drug Ibuprofen. The cryogels was characterized by different techniques, when presented a band around 1700 cm−1 referring to Cdouble bondO, which can be attributed to N, N’-methylene-bis-acrylamide, being an indication of the formation of the large, in addition, they presented indications of an amorphous polymeric matrix. The X-ray tomography images showed two-dimensional images and three-dimensional reconstructions, which could not be seen in the SEM. The results of cryogels loaded with the drug Ibuprofen showed that the samples showed toxicity only at a concentration of 5 mg mL−1. All other cryogel samples were considered non-cytotoxic. Regarding the release of Ibuprofen, there was aelease of the drug in the first 12 h in PBS, and the release in the gastric fluid was slower, but all cryogels tended to release 100 %; these cryogels were promising in the drug release model.
Salinity influence on Mytilus galloprovincialis exposed to antineoplastic agents: a transcriptomic, biochemical, and histopathological approach
(Elsevier, 2024-12-15) Queirós, Vanessa; Leite, Carla; Azeiteiro, Ulisses M.; Casado Belloso, Marta; Soares, Amadeu M.V.M.; Santos Morcillo, Juan Luis; Alonso Álvarez, Esteban; Barata, Carlos; Freitas, Rosa; Universidad de Sevilla. Departamento de Química Analítica; Ministerio de Ciencia e Innovación (MICIN). España; Universidad de Sevilla. FQM344: Análisis Químico Industrial y Medioambiental
Nowadays, aquatic species face a variety of environmental risks associated with pharmaceutical consumption. More specifically, the increased number of cancer patients has been accompanied by an increased consumption of antineoplastic drugs, such as ifosfamide (IF) and cyclophosphamide (CP). These drugs have been found in aquatic ecosystems, raising concerns about their impact, especially on estuarine species, as marine waters are the final recipients of continental effluents. Simultaneously, predicted climatic changes, such as salinity shifts, may threaten organisms. Considering this, the present research aims to investigate the combined effects of IF and CP, and salinity shifts. For this, a transcriptomic, biochemical, and histopathological assessment was made using the bivalve species Mytilus galloprovincialis exposed for 28 days to IF and CP (500 ng/L), individually, at different salinity levels (20, 30, and 40). IF and CP up-regulated metabolism-related gene cyp3a1, with CP also affecting abcc gene, showing minimal salinity impact and highlighting the importance of these metabolic routes in mussels. Salinity shifts affected the transcription of genes related to apoptosis and cell cycle growth, such as p53, as well as the aerobic metabolism, the antioxidant and biotransformation mechanisms. These findings indicate mussels' high metabolic adaptability to osmotic stress. Under CP exposure and low salinity, mussels exhibited increased cellular damage and histopathological effects in digestive gland tubules, revealing detrimental effects towards M. galloprovincialis, and suggesting that a metabolic slowdown and activation of antioxidant mechanisms helped prevent oxidative damage at the control and high salinities. Overall, results reinforce the need for antineoplastics ecotoxicological risk assessment, especially under foreseen climate change scenarios.
Removal of Ibuprofen in Water by Bioaugmentation with Labrys neptuniae CSW11 Isolated from Sewage Sludge-Assessment of Biodegradation Pathway Based on Metabolite Formation and Genomic Analysis
(MDPI, 2024-12-31) Aguilar-Romero, I.; Madrid Díaz, Fernando; Villaverde Capellán, Jaime; Alonso Álvarez, Esteban; Santos Morcillo, Juan Luis; Morillo González, Esmeralda; Universidad de Sevilla. Departamento de Química Analítica; Junta de Andalucía; European Commission (EC). Fondo Europeo de Desarrollo Regional (FEDER); Universidad de Sevilla. FQM344: Análisis Químico Industrial y Medioambiental
Ibuprofen (IBP) is one of the most consumed drugs in the world. It is only partially removed in wastewater treatment plants (WWTPs), being present in effluent wastewater and sewage sludge, causing the widespread introduction of IBP as an emergent xenobiotic in different environmental compartments. This study describes the use of Labrys neptuniae CSW11, recently described as an IBP degrader, through bioaugmentation processes for the removal of IBP from water under different conditions (additional carbon sources, various concentrations of glucose and IBP). L. neptuniae CSW11 showed very good results in a wide range of IBP concentrations, with 100% removal in only 4 days for 1 and 5 mg L⁻¹ IBP and 7 days for 10 mg L⁻¹, and up to 48.4% removal in 28 days for IBP 100 mg L⁻¹ when using glucose 3 g L⁻¹ as an additional carbon source. Three IBP metabolites were identified during the biotransformation process: 1-hydroxyibuprofen (1-OH-IBP), 2-hydroxyibuprofen (2-OH-IBP), and carboxyibuprofen (CBX-IBP), whose concentrations declined drastically in the presence of glucose. IBP metabolites maintained a certain degree of toxicity in solution, even when IBP was completely removed. The results indicate that L. neptuniae CSW11 can be quite effective in degrading IBP in water, but the bioaugmentation method should be improved using CSW11 in consortia with other bacterial strains able to degrade the toxic metabolites produced. A genome-based analysis of L. neptuniae CSW11 revealed different enzymes that could be involved in IBP biodegradation, and a potential metabolic pathway was proposed based on the metabolites observed and genome analysis.
Matrix Solid-Phase Dispersion Procedure for Determination of Antibiotics and Metabolites in Mussels: Application in Exposure Bioassays
(MDPI, 2024-11-20) Mejías Padilla, Carmen; Fonseca, Tainá G. da; García-Criado, Noelia; Martín Bueno, Julia; Santos Morcillo, Juan Luis; Aparicio Gómez, Irene; Alonso Álvarez, Esteban; Universidad de Sevilla. Departamento de Química Analítica; Ministerio de Ciencia, Innovación y Universidades (MICIU). España; Universidad de Sevilla; Universidad de Sevilla. FQM344: Análisis Químico Industrial y Medioambiental
The presence of antibiotics in seafood for human consumption may pose a risk for consumers. Furthermore, some marine organisms, such as mussels, can result in appropriate bioindicators of marine contamination. In this work, a multiresidue analytical methodology suitable for the determination of antibiotics and metabolites in mussels is proposed. The target compounds include three sulphonamides and trimethoprim (TMP) and six of their main metabolites. Sample treatment involves extraction and clean-up in a single step using matrix solid-phase dispersion with acetonitrile. Analytical determination was carried out by liquid chromatography–tandem mass spectrometry. Good linearity (R² > 0.99), accuracy (from 80.8 to 118%), and limits of quantification (lower than 5 ng g⁻¹ (dry matter, dm)) were obtained for all selected compounds. The method was applied to the determination of antibiotics in mussel samples from an exposure assay with contaminated seawater with TMP and sulfamethoxazole (SMX). Both antibiotics were detected in the analysed samples with concentrations up to 77.5 ng g⁻¹ dm. TMP was bioconcentrated to a higher extent than SMX, attributable to its higher hydrophobicity. None of the metabolites were detected. These results demonstrate that Mytilus galloprovincialis is a suitable bioindicator to assess marine pollution.
Impact of Frozen Storage on Sensory, Physicochemical, and Volatile Compounds Parameters of Different Extra Virgin Olive Oils
(Multidisciplinary Digital Publishing Institute (MDPI), 2024-11-24) Díaz Montaña, Enrique Jacobo; Barbero López, María; Aparicio Ruiz, Ramón; García González, Diego Luis; Morales Millán, María Teresa; Universidad de Sevilla. Departamento de Química Física; Universidad de Sevilla. Departamento de Química Analítica; Ministerio de Ciencia, Innovación y Universidades (MICIU). España
Storage is important for virgin olive oil, a product obtained only during the harvest period, which requires a year-round storage until its best-before date. Low temperatures slow undesirable reactions, though this method is not widely applied. The objective of this paper is to assess the impact of frozen storage on the volatile composition and sensory properties of virgin olive oils. The quality parameters, volatile composition, and sensory profiles were analyzed for samples stored under different conditions (time 0, sixth month supermarket and frozen storage, and long-term-frozen). The physicochemical parameters of the samples stored under supermarket conditions showed significant differences (p < 0.05), with the frozen-storage sample after three months of storage. Additionally, the samples stored under supermarket conditions showed higher volatile concentrations than frozen ones, with increased concentrations of aldehydes and acids producing sensory defects. Thirty-two samples, considered as the long-term-frozen, were divided into three groups depending on the frozen-storage time (1, 6 or 10 years). These long-term-frozen storage samples confirmed the suitability of the proposed oxidation markers (pentanal, hexanal, heptanal, nonanal, acetic, propanoic, butanoic, and hexanoic acids) for differentiating storage conditions and times. This work highlights the oxidation process under different storage conditions and suggests oxidation markers.
Variability of Faecal Microbiota and Antibiotic Resistance Genes in Flocks of Migratory Gulls and Comparison with the Surrounding Environment
(Elsevier, 2024) Jarma, D.; Sacristán Soriano, O.; Borrego, C. M.; Hortas, F.; Peralta Sánchez, Juan Manuel; Balcázar, J. L.; Green, A. J.; Alonso Álvarez, Esteban; Sánchez Melsió, A.; Sánchez Ordóñez, Marta Isabel; Universidad de Sevilla. Departamento de Química Analítica; Universidad de Sevilla. Departamento de Zoología; Gobierno de España; Ministerio de Ciencia, Innovación y Universidades (MICIU). España; Generalitat de Catalunya
Gulls commonly rely on human-generated waste as their primary food source, contributing to the spread of antibiotic-resistant bacteria and their resistance genes, both locally and globally. Our understanding of this process remains incomplete, particularly in relation to its potential interaction with surrounding soil and water. We studied the lesser black-backed gull, Larus fuscus, as a model to examine the spatial variation of faecal bacterial communities, antibiotic resistance genes (ARGs), and mobile genetic elements (MGEs) and its relationship with the surrounding water and soil. We conducted sampling campaigns within a connectivity network of different flocks of gulls moving across functional units (FUs), each of which represents a module of highly interconnected patches of habitats used for roosting and feeding. The FUs vary in habitat use, with some gulls using more polluted sites (notably landfills), while others prefer more natural environments (e.g., wetlands or beaches). Faecal bacterial communities in gulls from flocks that visit and spend more time in landfills exhibited higher richness and diversity. The faecal microbiota showed a high compositional overlap with bacterial communities in soil. The overlap was greater when compared to landfill (11%) than to wetland soils (6%), and much lower when compared to bacterial communities in surrounding water (2% and 1% for landfill and wetland water, respectively). The relative abundance of ARGs and MGEs were similar between FUs, with variations observed only for specific families of ARGs and MGEs. When exploring the faecal carriage of ARGs and MGEs in bird faeces relative to soil and water compartments, gull faeces were enriched in ARGs classified as High-Risk. Our results shed light on the complex dynamics of antibiotic resistance spread in wild bird populations, providing insights into the interactions among gull movement and feeding behavior, habitat characteristics, and the dissemination of antibiotic resistance determinants across environmental reservoirs.
Quantification of Linear Alkylbenzene Sulphonates in Complex Sludge Samples: Influence of Matrix Effects in Calibration Methods
(Elsevier, 2024) Martín Bueno, Julia; Mejías Padilla, Carmen; Santos Morcillo, Juan Luis; Aparicio Gómez, Irene; Alonso Álvarez, Esteban; Heinze, John; Universidad de Sevilla. Departamento de Química Analítica; Universidad de Sevilla
Linear Alkylbenzene Sulfonates (LAS) are among the priority organic pollutants in sludge owing to their high concentrations, due to its use as a major cleaning agent (surfactant) in laundry detergents and household cleaning products, and to the concentration limits of 2,600 mg/kg outlined in the EU directive draft for land application of sludge. In this work, a method has been optimized and validated for the accurate quantification of LAS homologues C10-C13 in different types of samples in the sludge treatment and disposal process including primary, secondary, and digested sludge, compost, and soil. The type of matrix had a significant impact on the method's validation process, resulting in the need of the use of distinct dilution factors for each matrix. Overall, the procedure propose involves a cost-effective and user-friendly technique that combines both extraction and clean-up in a single step (ultrasound-assisted extraction and dispersive solid phase extraction). Analytical determination is conducted using liquid chromatography-tandem mass spectrometry. The method demonstrated excellent accuracy (relative recoveries exceeding 84.5 % across all types of sludge samples) and the limit of quantification enables the measurement of LAS concentrations up to 1000 times lower than the concentration limits stipulated in the EU directive draft. For an accurate quantification, three calibration approaches were tested (external calibration, standard addition, and matrix-matched calibration). Standard addition was the preferred method for quantitative analysis. It helps mitigate matrix effects that could otherwise distort the accuracy of analyte measurements, making it crucial for quality control, especially in monitoring applications where matrix effects may introduce bias into concentration calculations.
Occurrence, Dissipation Kinetics and Environmental Risk Assessment of Antibiotics and their Metabolites in Agricultural Soils
(Elsevier, 2024) Mejías Padilla, Carmen; Martín-Pozo, Laura; Santos Morcillo, Juan Luis; Martín Bueno, Julia; Aparicio Gómez, Irene; Alonso Álvarez, Esteban; Universidad de Sevilla. Departamento de Química Analítica; Ministerio de Ciencia e Innovación (MICIN). España; Universidad de Sevilla; European Union (UE)
Antibiotics are among the emerging contaminants of greatest concern to the scientific community. However, the occurrence and behaviour of their metabolites in soils have been scarcely studied. To address this research gap, this study investigates the occurrence, sorption, dissipation kinetics, and environmental risk of highly important antibiotics (sulfamethazine, sulfadiazine, sulfamethoxazole, trimethoprim) and their main metabolites in Mediterranean agricultural soils. Batch experiments were conducted under natural conditions for 120 days. Five different dissipation kinetics models were applied to elucidate antibiotics degradation. The sorption isotherms were evaluated by three different models. Most of the antibiotics and metabolites tested showed a good fit with the Linear Isotherm model (R2 >0.96) and biphasic dissipation kinetic models (R2 >0.90). The dissipation and the endpoints values (DT50 and DT90) depended on the soil type properties. A Lixisol soil demonstrated reduced degradation of the investigated compounds. Trimethoprim showed the highest persistence, followed by sulfamethazine, sulfamethoxazole, and sulfadiazine. Parent compounds exhibited lower degradation rates than their metabolites. Remaining antibiotic concentrations were found to be below the predicted no-effect concentration in soil, suggesting that they may not pose a risk to terrestrial biota. This study provides valuable insights into the behaviour of these antibiotics and their metabolites in soil.
Determination of Pesticide Residues in Five Different Corn-based Products Using a Single and Simple Solid–liquid Extraction without Clean-up Steps Followed by Comprehensive Two-dimensional Liquid Chromatography Coupled to Tandem Mass Spectrometry
(Elsevier, 2024) Arena, Katia; Martín-Pozo, Laura; Laganà Vinci, Roberto; Cacciola, Francesco; Dugo, Paola; Mondello, Luigi; Universidad de Sevilla. Departamento de Química Analítica; Ministerio de Ciencia, Innovación y Universidades (MICIU). España; Ministerio de Ciencia e Innovación (MICIN). España
Pesticide residues in food products are a critical issue concerning food safety. Recent studies have increasingly focused on developing selective, rapid, innovative, and environmentally friendly analytical methods for detecting pesticides in foodstuffs. This study presents a novel analytical method utilizing comprehensive two-dimensional liquid chromatography-tandem mass spectrometry for the simultaneous determination of one hundred and thirteen multiclass pesticides in corn products. The method simplifies the process with a single-step solid–liquid extraction and benefits from two-dimensional separation to enhance resolution and minimize matrix effects. The methodology was validated according to European Commission DG-SANTE (SANTE/11312/2021) and European Committee for Standardization (EN 15662, 2018) guidelines, obtaining acceptable analytical parameters. Limits of detection ranged from 0.2 µg/L to 30.2 µg/L and limits of quantification from 0.3 to 91.6 μg/L, all bellow regulatory limits. Accuracy, ranged from 60 to 120 % and precision, estimated by relative standard deviation, was consistently below 15.1 % in all cases. The applicability of the method was demonstrated by analyzing pesticides in five representative corn products (tortilla, corn flakes, corn cake, starch, and polenta). Sixteen pesticides were detected, all within the regulatory residue limits. Three metric tools were applied to assess the analytical process. Environmental sustainability was evaluated using the AGREE metric, while analytical performance and method applicability were assessed with the Red-Green-Blue and Blue Applicability Grade Index models, respectively, yielding promising scores (0.5, ≥ 0.55, and 0.65). These findings and the comparison to previous methods indicated that this approach represents a promising, alternative and user-friendly strategy for pesticide determination, offering effective productivity and reliable analytical performance.
Clays-based Geopolymers: a Sustainable Application as Adsorbent of Cytostatic Drugs for Water Purification
(Springer Science and Business Media Deutschland GmbH, 2024) Ben Amor, Assia; Arenas Molina, Marina; Martín Bueno, Julia; Ouakouak, Abdelkader; Santos Morcillo, Juan Luis; Aparicio Gómez, Irene; Alonso Álvarez, Esteban; Hamdi, Noureddine; Universidad de Sevilla. Departamento de Química Analítica; Ministerio de Ciencia e Innovación (MICIN). España
The administration of cytostatic drugs in chemotherapy is steadily increasing, triggering thus a risk to the environment. Identifying powerful ways to effectively remove these hazardous pollutants from hospital and effluent wastewater before they discharge into the aquatic environment remains a critical and challenging task. Adsorption is among the most effective ways to treat contaminated water due to the wide availability and selectivity of the adsorbents besides the simplicity and the low start-up costs of the technique. In this work, a geopolymer, elaborated from an illito-kaolinitic clay (Douiret region of Tunisia) and industrial waste (silica fume and phosphogypsum), has been tested as promising decontamination of the cytostatic drugs paclitaxel (PCX) and irinotecan (IRI) from water samples. The foamed geopolymer was characterized using X-ray diffraction, Fourier transform infrared, scanning electron microscopy and thermogravimetric analysis before and after adsorption. Adsorption batch assays were performed using different concentrations of PCX and IRI, contact times and environmental conditions. The geopolymer had an excellent removal efficiency (almost 100% for PCX and 89% for IRI) using 20 mg of adsorbent and 2.5 mg/L of each drug concentration. The characterization results showed that cytostatic drugs were adsorbed to the geopolymer through physical interactions, pore filling, electrostatic attraction and hydrogen bonding. The specific surface area and pore volume of the geopolymer were 82.23 m2/g and 0.19 cm3/g, respectively. In addition to its cost-effective properties, the geopolymer demonstrated excellent efficiency in contaminated natural samples (including influent, effluent wastewater and surface water) denoting a great application for water purification.
Analytical Quality by Design in the Development of a Solvent-modified Micellar Electrokinetic Chromatography Method for the Determination of Sitagliptin and its Related Compounds
(Elsevier, 2021) Pasquini, Benedetta; Gotti, Roberto; Villar Navarro, Mercedes; Douša, Michal; Renai, Lapo; Del Bubba, Massimo; Orlandini, Serena; Furlanetto, Sandra; Universidad de Sevilla. Departamento de Química Analítica; Ministerio de Educación, Cultura y Deporte (MECD). España
A solvent-modified micellar electrokinetic chromatography method was developed following the Quality by Design approach for the simultaneous determination of sitagliptin (SIT), an oral antihyperglycemic drug, and its main impurities derived from the synthesis process. The separation system was identified in the scouting phase and was made by sodium dodecyl sulphate (SDS) micelles with the addition of n-butanol and methanol. The knowledge space was investigated through an asymmetric screening matrix, taking into consideration eight critical method parameters (CMPs) involving the composition of the background electrolyte in terms of buffer concentration and pH, the concentration of surfactants and organic modifiers, and voltage. The critical method attributes (CMAs) were identified as analysis time and the distance between the tail of the electroosmotic flow system peak and the front edge of impurity I1 (sitagliptin triazole hydrochloride). A Box-Behnken Design was used in response surface methodology for calculating the quadratic models relating the CMPs to the CMAs. From the models it was possible to compute the method operable design region (MODR) through Monte-Carlo simulations. The MODR was identified in the probability maps as the multidimensional zone where the risk of failure to achieve the desired values for the CMAs was lower than 10 %. The experimental conditions corresponding to the working point, with the MODR interval, were the following: background electrolyte, 14 (10−18) mM borate buffer pH 9.20, 100 mM SDS, 13.6 (11.1–16.0) %v/v n-butanol, 6.7 (4.5–8.8) %v/v methanol; voltage and temperature were set to 28 kV and 22 °C, respectively. The developed CE method was validated in accordance with International Council for Harmonisation guidelines and was applied to the analysis of SIT tablets. The routine analysis for the quality control of the pharmaceutical product could be conducted in about 11 min.

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