Persona: Fernández Hernando, Pilar
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Publicación Corrigendum to “Occurrence of common plastic additives and contaminants in mussel samples: Validation of analytical method based on matrix solid-phase dispersion”(Springer, 2021) Cañadas, Raquel; Garrido Gamarro, Esther; Garcinuño Martínez, Rosa Mª; Paniagua González, Gema; Fernández Hernando, Pilar; https://orcid.org/0000-0002-2935-6655Publicación Enhancement of a Simple, Economic and Eco-Friendly Analytical Approach for the Extraction and Determination of Endocrine Disruptors from Plastics in Shrimp(MDPI, 2024-07-12) Soliz Rojas, Dulce Lucy; García González, Jorge; Paniagua González, Gema; Garcinuño Martínez, Rosa Mª; Bravo Yagüe, Juan Carlos; Fernández Hernando, PilarThe economic significance of the shrimp industry relies heavily on the comprehensive utilization of all of the shrimp’s parts. However, this importance is often threatened by common challenges such as disease and pollution, caused by prominent contaminants that are capable of exerting adverse effects either directly as physical pollutants or indirectly through the incorporation of additives or adsorbed chemicals. Among these substances are endocrine disruptors, which pose risks to both wildlife and human populations. In this study, 11 endocrine-disrupting compounds were determined (3 bisphenols, 3 phthalates, 3 pesticides, and 2 nonylphenols) through the development of a cost-effective, greener and cost-friendly method based on solid-phase matrix dispersion (MSPD) with high-performance liquid chromatography coupled with diode array detection (HPLC-DAD). Determinations were performed on different parts of the shrimp: the cephalothorax, abdomen, intestine and shell. Several variables were optimized in the extraction, separation and detection phases, resulting in average recoveries of about 90%. The limit of detection (LOD) varies depending on the analyte and matrix. At concentrations of 1 mg/kg in the cephalothorax+shells and 1.25 mg/kg in the abdomen+intestine, all compounds were detected, except for nonylphenols. The developed method has allowed the simultaneous determination of 11 endocrine disruptors in different parts of the shrimp samples. Furthermore, the MSPD has been demonstrated to be an efficacious, selective, and streamlined sample extraction method, eliminating the necessity for pretreatment steps such as centrifugation and filtration, as well as the use of large volumes of solvents.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 Statistical evaluation of fluoride contamination in groundwater resources of Santiago del Estero Province , Argentina(Elsevier, 2020-11) Rondano Gómez, Karina del Valle; López Pasquali, Clara Elena; 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 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 Alonso, 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.Publicación Development of a molecularly imprinted polymeric membrane for determination of macrolide antibiotics from cow milk(Elsevier, 2022-05-17) Cañadas, Raquel; Paniagua González, Gema; Fernández Hernando, Pilar; Garcinuño Martínez, Rosa Mª; https://orcid.org/0000-0002-2935-6655A 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 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 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 Identification and morphological characterization of different types of plastic microparticles(Elsevier, 2024-05-15) Soliz Rojas, Dulce Lucy; Paniagua González, Gema; Muñoz Arnanz, Juan; Bravo Yagüe, Juan Carlos; Fernández Hernando, Pilar; Garcinuño Martínez, Rosa MªThe knowledge of the polymeric composition of microplastics (MPs) is interesting because offers useful information on the resistance, durability, and degradability of these materials, also allowing progress in the control of this contamination. However, there is currently a lack of reliable standardized methods for the identification, and characterization of the plastic microparticles. This work uses different techniques in a complementary manner for the identification, and characterization of MPs that more frequently are found in the environment. A total of 10 types of plastics were collected (polystyrene (PS), polyethylene terephthalate (PETE), polyethylene (PE), high- and low-density polyethylene (HDPE and LDPE, respectively), polyvinyl chloride (PVC), polypropylene (PP), polytetrafluoroethylene (PTFE), Polyamide (PA, Nylon 6,6) and poly-carbonate (PC)) and their chemical identification were analyzed by reflectance-attenuated infrared (FTIR-ATR). Furthermore, the samples were observed using light microscopy, and scan-ning electron microscopy (SEM). Also, staining with 12 different dyes was performed to improve the identification of microplastics. The results of this study revealed that PETE, PE, HDPE and LDPE, whose SEM images exhibited smoothness and flat uniformity of their surface, were not (or less) susceptible to adsorb staining solutions while PP, PA, PVC, and PTFE, were capable of adsorbing the dye solutions.Publicación Development and Characterization of SBA-15 Imprinted Polymers for Spiramycin Analysis(MDPI, 2024) González Gómez, Lorena; Morante Zarcero, Sonia; Pérez Quintanilla, Damián; Paniagua González, Gema; Garcinuño Martínez, Rosa Mª; Fernández Hernando, Pilar; Sierra Alonso, Isabel; https://orcid.org/0000-0003-2377-8555; https://orcid.org/0000-0001-6448-2385; https://orcid.org/0000-0002-7150-122X; https://orcid.org/0000-0003-2091-6772This work focuses on the development of a hybrid material based on SBA-15 silica with a molecularly imprinted polymer (MIP), using spiramycin (SPI) as a template, for use as sorbent in solid-phase extraction (SPE). Characterization techniques such as nitrogen gas adsorption–desorption isotherms, infrared spectroscopy and scanning electron microscopy confirmed the structure and properties of the SBA-15@MIP-SPI material. SPE conditions using SBA-15@MIP-SPI as sorbent were optimized, which allowed us to demonstrate the high selectivity and adsorption capacity of SPI on the synthesized material. The best conditions were 50 mg of sorbent, loading with 1 mL of standard solution or sample of cow milk previously extracted in acetonitrile and eluting with 3 mL of methanol with 1% acetic acid. After the optimization process, the material demonstrated recovery percentages of 81 ± 3% in SPI standard solutions and showed its potential in cow milk samples (71 ± 6%). The novelty of the research consists of the combination of MIPs with SBA-15, which could offer important advantages in terms of specific surface area and porous structure, thus improving performance and reducing the amount of sorbent compared to other traditional methods.