Persona: Garcinuño Martínez, Rosa Mª
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Publicación Assessing matrix solid phase dispersion extraction strategies for determining bisphenols and phthalates in gilthead sea bream samples(MDPI, 2024-01) Soliz Rojas, Dulce Lucy; Paniagua González, Gema; Bravo Yagüe, Juan Carlos; Fernández Hernando, Pilar; Garcinuño Martínez, Rosa MªMicroplastics (MPs) and nanoplastics (NPs) are widely spread in the environment, generating significant concern due to their potential impact on environmental health. Marine species usually ingest plastic fragments, mistaking them for food. Many toxic compounds, such as plastic additives that are not chemically bound to the plastic matrix, can be released from MPs and NPs and reach humans via the food chain. This paper highlights the development and validation of a straightforward solid–liquid extraction clean-up procedure in combination with a matrix solid-phase dispersion method using high-performance liquid chromatography coupled with mass spectrometry (HPLC-MS) detection, enabling facile, precise, and reliable identification and quantitation of a total of six bisphenols and phthalates in gilthead sea breams. Under the optimized conditions, the developed method showed good linearity (R2 > 0.993) for all target compounds. The recoveries obtained were between 70 and 92%. The relative standard deviations (RSDs) for reproducibility (inter-day) and repeatability (intra-day) were less than 9% and 10%, respectively. The limit of detection (LOD) and limit of quantification (LOQ) for the target compounds ranged from 0.11 to 0.68 µg/kg and from 0.37 to 2.28 µg/kg, respectively. A new, efficient extraction methodology for the determination of BPA, BPS, BPF, DBP, DEP, and DHEP in gilthead seabream has been optimized and validated.Publicación Development of a molecularly imprinted polymeric membrane for determination of macrolide antibiotics from cow milk(Elsevier, 2022-05-17) Cañadas Soler, Raquel; Paniagua González, Gema; Fernández Hernando, Pilar; Garcinuño Martínez, Rosa MªA molecular imprinted membrane (MIM) was prepared for the selective binding of macrolide antibiotics by UV-initiated non-covalent imprinting approach . The membrane was modified by a UV - photographting technique in the presence of molecule templates of erythromycin (ERY) and spiramycin (SPI) with methacrylic acid (MAA) as functional monomer and ethylene glycol dimethacrylate (EGDMA) as crosslinker. The nanofunctionalized MIM obtained was characterized by a morphological study using scanning electron microscopy (SEM), as well as by a study of its adsorption capacity by online solid phase extraction (SPE) procedure. Variables affecting the MIM-SPE method were optimized to maximize the extraction of macrolide antibiotics of interest and a high-performance liquid chromatography (HPLC) method was used for the analysis. Good linearity and precision were obtained for ERY and SPI, with average recoveries up to 86.14 % and 34.73 %, respectively, with a relative standard deviation (RSD) lower than 6 %. In addition, selectivity was studied for other macrolides with similar structure to the templates, such as roxithromycin (ROX), josamycin (JOS), ivermectin (IVER) and tylosin (TYL). The proposed MIM-SPE-HPLC methodology was effectively applied to ERY and SPI determination in commercial doped semi-skimmed cow’s milk samples.Publicación Assessing microplastic ingestion and occurrence of bisphenols and phthalates in bivalves, fish and holothurians from a Mediterranean marine protected area(Elsevier, 2022-08-07) Rios Fuster, Beatriz; Alomar, Carme; Deudero, Salud; Paniagua González, Gema; Soliz Rojas, Dulce Lucy; Fernández Hernando, Pilar; Garcinuño Martínez, Rosa MªMicroplastic (MP) ingestion, along with accumulated plasticizers such as bisphenol A (BPA), bisphenol F (BPF), and bisphenol S (BPS), and phthalates represented by diethyl phthalate (DEP), dibutyl phthalate (DBP) and bis (2-ethylhexyl) phthalate (DEHP), were quantified in bivalves, fish, and holothurians collected from a coastal pristine area at the western Mediterranean Sea. MP ingestion in sediment-feeders holothurians (mean value 12.67 ± 7.31 MPs/individual) was statistically higher than ingestion in bivalves and fish (mean 4.83 ± 5.35 and 3 ± 4.44 MPs/individual, respectively). The main ingested polymers were polyethylene, polypropylene, and polystyrene. The levels of BPS, BPF, and DEHP were highest in bivalves' soft tissue; BPA and DBP had the highest levels in the holothurians’ muscle. In addition, the levels of all plasticizers assessed were lowest in fish muscle; only BPA levels in fish were higher than in bivalves, with intermediate values between those of bivalves and holothurians. This study provides data on exposure to MPs and plasticizers of different species inhabiting Cabrera Marine Protected Area (MPA) and highlights the differences in MP ingestion and levels of plasticizers between species with different ecological characteristics and feeding strategies.Publicación Assessment of molecularly imprinted polymers as selective solid-phase extraction sorbents for the detection of cloxacillin in drinking and river water(MDPI, 2023-11-03) Collado, Eduardo José; Paniagua González, Gema; Bravo Yagüe, Juan Carlos; Fernández Hernando, Pilar; Garcinuño Martínez, Rosa MªThis paper describes a new methodology for carrying out quantitative extraction of cloxacillin from drinking and river water samples using a molecularly imprinted polymer (MIP) as a selective sorbent for solid-phase extraction (MISPE). Several polymers were synthesized via thermal polymerization using cloxacillin as a template, methacrylic acid (MAA) as a functional monomer, ethyleneglycoldimethacrylate (EGDMA) as a cross-linker and different solvents as porogens. Binding characteristics of the adequate molecularly imprinted and non-imprinted (NIP) polymers were evaluated via batch adsorption assays following the Langmuir and Freundlich isotherms and Scatchard assays. The parameters related to the extraction approach were studied to select the most appropriate polymer for cloxacillin determination. Using the optimized MIP as the SPE sorbent, a simple sample treatment methodology was combined with high-performance liquid chromatography (HPLC) to analyze cloxacillin residues in drinking and river water. Under the optimum experimental conditions, the MISPE methodology was validated using spiked samples. The linearity for cloxacillin was assessed within the limits of 0.05–1.5 g L1 and the recovery percentage was higher than 98% (RSD < 4%). The limits of detection and limits of quantification were 0.29 and 0.37 g L1 and 0.8 and 0.98 g L1 for drinking and river water, respectively. The selectivity of MIP against other ß-lactam antibiotics with similar structures (oxacillin, cefazoline, amoxicillin and penicillin V) was studied, obtaining a good recovery higher than 85% for all except cefazoline. The proposed MISPE-HPLC methodology was successfully applied for the detection of cloxacillin in drinking water from Canal de Isabel II (Madrid) and river water from the Manzanares River (Madrid).Publicación Selective extraction of diazepam and its metabolites from urine samples by a molecularly imprinted solid phase extraction (MISPE) method(MDPI, 2024-02) Gil Tejedor, Ana María; Bravo Yagüe, Juan Carlos; Paniagua González, Gema; Fernández Hernando, Pilar; Garcinuño Martínez, Rosa MªIn this research, a molecularly imprinted polymer (MIP) was synthesized by precipitation polymerization using oxazepam (OZ) as a template molecule and was subsequently applied as a selective sorbent for the extraction of diazepam (DZP) and its metabolites in urine samples using an SPE cartridge. OZ, temazepam (TZ), nordiazepam (NZ) and DZP were analyzed in the final extracts by high-performance liquid chromatography with diode array detection (HPLC-DAD). The SPE extraction steps were optimized, and the evaluation of an imprinting factor was carried out. The selectivity of the method for OZ versus structurally related benzodiazepines (BZDs), such as bromazepam (BRZ), tetrazepam (TTZ) and halazepam (HZ), was investigated. Under the optimum conditions, the proposed methodology provided good linearity in the range of 10–1500 ng/mL, with limit of detection values between 13.5 and 21.1 ng/mL and recovery levels for DZP and its metabolites from 89.0 to 93.9% (RSD ≤ 8%) at a concentration level of 1000 ng/mL. The proposed method exhibited good selectivity, precision and accuracy and was applied to the analysis of urine samples from a real case of DZP intake.Publicación Occurrence of common plastic additives and contaminants in raw, steamed and canned mussel samples from different harvesting areas using MSPDHPLC methodology(Elsevier, 2024-04) Garrido Gamarro, Esther; Soliz Rojas, Dulce Lucy; Paniagua González, Gema; Fernández Hernando, Pilar; Garcinuño Martínez, Rosa MªMicroplastics are a complex mix of chemicals containing polymers and certain plastic additives such as bisphenols and phthalates. These particles are porous materials that can also sorb contaminants from their surroundings, and leach chemicals from the particle under certain circumstances. Aquatic animals can ingest microplastic particles, which mostly bioaccumulate in the gastrointestinal tract of animals. In terms of dietary exposure, small animals consumed whole such as mussels, contribute more to the dietary intake of microplastic particles. Plastic additives and contaminants are not chemically bound to the polymers, and certain processing methods or cooking processes result in the release of these chemicals that leach from the plastic particles, leaving them more available for absorption when ingested. Analytical methods are crucial for a better understanding of the occurrence of plastic additives and contaminants in aquatic products, and to know certain circumstances and treatments that influence human exposure. This study uses an MSPD-HPLC methodology for the simultaneous determination of 9 analytes (BPA, BPF, BPS, DEP, DBP, DEHP, DDD, DDT, and DDE) analyzing, for the first time, the occurrence of these chemicals in raw, steamed and canned mussels of two different harvesting areas (Atlantic and the Mediterranean), becoming one of the most efficient methodologies for determining the presence of these analytes in very complex food matrices, able to define the changes in cooking and processing activities. The results showed that the heat and pressure treatment could influence the migration of plastic additives from microplastic particles present in mussels to the cooking liquids.Publicación Statistical evaluation of fluoride contamination in groundwater resources of Santiago del Estero Province , Argentina(Elsevier, 2020-11) Rondano Gómez, Karina del Valle; López Pasquali, C. E.; Paniagua González, Gema; Fernández Hernando, Pilar; Garcinuño Martínez, Rosa MªThis study investigates the suitability of statistical techniques for evaluating the fluoride content and the groundwater quality from Robles Department (RD) and Banda Department (BD) areas in Santiago del Estero (Argentina). Groundwater mineralization is driven by many processes such as, weathering of volcanic products, geothermal activity and human activities. The original matrix consisted of 9 parameters estimated (fluoride content, pH, conductivity, environmental and water temperatures, total dissolved solids, chloride concentration, hardness and alkalinity) from 110 groundwater samples collected of 23 selected scattered rural areas. Groundwater samples were obtained by sampling in wells at different depths. The fluoride levels were determined by a standard colorimetric method in two seasonal periods, dry (from April to September) and rainy (from October to March). Parameters such as pH and total dissolved solids (TDS) reached their highest values in the rainy season; while the temperature, alkalinity, chloride concentration and hardness did it in the dry season. In both seasons, the environmental temperature average was 22 °C. Regarding the fluoride content, approximately the fifty percent of the analyzed groundwater samples exceeded the upper limit (1.0 mg/L) established by the current legislation, obtaining concentration levels between 0.01-2.80 mg/L. This study demonstrates the usefulness of univariate (quartiles calculation, interquartile range IQR) and multivariate statistical method of principal component analysis (PCA) and clusters to establish a better understanding of the environmental status of the region studied and the degree of pollution.Publicación Occurrence of common plastic additives and contaminants in mussel samples: Validation of analytical method based on matrix solid-phase dispersion(Elsevier, 2021-07) Cañadas Soler, Raquel; Garrido Gamarro, Esther; Paniagua González, Gema; Fernández Hernando, Pilar; Garcinuño Martínez, Rosa MªA new matrix solid-phase dispersion (MSPD) extraction methodology, combined with high-performance liquid chromatography equipped with a diode-array detector, was developed and validated for the simultaneous determination of 10 compounds in mussels from Galician Rias (Spain). These pollutants are compounds commonly used for plastic production as additives, as well as common plastic contaminants. The compounds selected were bisphenol-A, bisphenol-F, bisphenol-S, nonylphenol-9, nonylphenol, diethyl phthalate, dibutyl phthalate, di-2ethylhexyl phthalate, dichlorodiphenyltrichloroethane, dichlorodiphenyldichloroethane, and dichlorodiphenyldichloroethylene. The parameters affecting the MSPD extraction efficiency such as the type of sorbent, mass sample-sorbent ratio, and extraction solvent were optimised . The proposed method provided satisfactory quantitative recoveries (80‒100%), with relative standard deviations lower than 7%. In all cases, the matrix-matched calibration curves were linear in the concentration range of 0.32-120.00 µg/kg, with quantification limits of 0.25‒16.20 µg/kg. The novel developed MSPD-high-performance liquid chromatography methodology provided good sensitivity, accuracy, and repeatability for quality control analysis in mussels.Publicación Assessment of the impact of aquaculture facilities on transplanted mussels (Mytilus galloprovincialis): Integrating plasticizers and physiological analyses as a biomonitoring strategy(Elsevier, 2022-02-15) Rios Fuster, Beatriz; Alomar, Carme; Capó, Xavier; Silva, Mónica; Solé, Montserrat; Freitas, Rosa; Deudero, Salud; Paniagua González, Gema; Soliz Rojas, Dulce Lucy; Fernández Hernando, Pilar; Garcinuño Martínez, Rosa MªThe growing plastic production and its continuous use is a significant problem. In addition, aquaculture practices have experienced a considerable growth and plastic is widely used in these activities, hence plasticizers must be considered due to their potential ecotoxicological impacts on species. Mussels placed inside an Integrated Multi-Trophic Aquaculture (IMTA) system and at two control locations were employed to quantify the ingestion of anthropogenic particles and associated chemical plasticizers, such as bisphenol A (BPA) jointly to bisphenol F (BPF) and bisphenol S (BPS), and phthalates represented by diethyl phthalate (DEP), dibutyl phthalate (DBP) and bis(2-ethylhexyl) phthalate (DEHP). In addition, some metabolism and oxidative stress related parameters were measured in mussels’ whole soft tissue. Anthropogenic particle ingestion of mussels increased over time at the three locations and the following order of abundance of pollutants was observed: BPA> BPF> DEHP> DBP> BPS> DEP. Even though no differences according to location were found for pollutants’ occurrence, time trends were evidenced for BPA and DEHP. On the other hand, a location effect was observed for biomarkers with highest values detected in mussels located at the vicinities of the aquaculture facility. In addition, a reduced detoxification activity was observed over time parallel to BPA decrease.Publicación Determination of atropine and scopolamine in honey using a miniaturized polymer-based solid-phase extraction protocol prior to the analysis by HPLC-MS/MS(Elsevier, 2024-04-09) Fernández Pintor, Begoña; Gañán Aceituno, Judith; Morante Zarcero, Sonia; Sierra, Isabel; Paniagua González, Gema; Fernández Hernando, Pilar; Garcinuño Martínez, Rosa MªTwo homopolymers have been prepared employing methacrylic acid and 4-vynylpiridine as functional monomers (p-MAA, p-4-VP) through an easy and quick precipitation polymerization method for application as sorbents in solid-phase extraction (SPE) to determine atropine and scopolamine in honey. The optimized SPE conditions were as follows: 25 mg of p-MAA, 4 mL of sample loading volume (diluted honey 1:10 with water), 4 mL of elution solvent (methanol/water with 1 % formic acid, 80/20, v/v). The extracts were analyzed by HPLC-MS/MS. The cartridges were reusable for forty cycles demonstrating an environmentally friendly approach. The methodology was validated in terms of linearity, accuracy, precision, selectivity, matrix effect and sensibility, highlighting the absence of matrix effect. The miniaturized polymer-based SPE was successfully applied to fifteen honeys, showing concentrations up to 7.23 ng/g in the most contaminated honey. All quantified honey samples (5 in total) were of multifloral type.