Persona: Garcinuño Martínez, Rosa Mª
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Garcinuño Martínez
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Publicación On-line flow injection molecularly imprinted solid phase extraction for the preconcentration and determination of 1-hydroxypyrene in urine samples(Elsevier, 2017-05-01) Serrano, Montserrat; Bartolomé, Mónica; Gañán Aceituno, Judith; Gallego Picó, Alejandrina; Bravo Yagüe, Juan Carlos; Paniagua González, Gema; Garcinuño Martínez, Rosa MªNew analytical strategies tend to automation of sample pre-treatment and flow analysis techniques provided a number of enhanced analytical methods allowing high throughput. Flow techniques are usually faster, more robust and more flexible than their batch equivalents. In addition, flow methods use less sample and reagent amounts and reduce analytical costs and waste. A flow injection solid-phase extraction pre-concentration system using a molecularly imprinted polymer (MIP) packed micro-column was developed for the determination of 1-hydroxypyrene in human urine with fluorescence detection. The pre-concentration of 1-hydroxypyrene on the MIP was carried out based on the specific retention of analyte by on-line introducing the sample into the micro-column system. Methanol and dichloromethane mixture was used to elute the retained analyte for fluorometric analysis. Important influencing factors were studied in detail, in batch and in flow (MISPE procedure optimisation, sample and eluent volumes, flow rate, dimensions of MIP micro-column and amounts of packing material, etc). To the best of our knowledge, this is the first on-line flow injection molecularly imprinted solid phase extraction for the pre-concentration and determination of hydroxylate PAH metabolite in urine samples. The optimised method was successfully applied to the determination of 1-Hydroxypyrene in spiked urine samples, with recoveries in the range of 74–85% and RSD<4.6%. Under optimum experimental conditions, the linearity concentration range used was 10–400 μg L−1, R2>0.996. We obtained limit of detection and quantification of 3.1 μg L−1 and 10.5 μg L−1, respectivelyPublicación 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 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 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 Methacrylic acid-ethylene glycol dimethacrylate polymeric sorbent for the removal of estrogens from water(['Estrogens', 'Removal', 'Polymer', 'Sorbent', 'Waters', 'Balaban Publishers – Desalination Publications'], 2018-11) Gallego, Alejandrina; Bravo Yagüe, Juan Carlos; Paniagua González, Gema; Fernández Hernando, Pilar; Garcinuño Martínez, Rosa MªThe presence of estrogens in environmental waters can cause adverse effects to aquatic organisms. In the last years, diverse researches have been focussed on the development of cost-effective methods for the removal of these compounds in water. In this paper, a series of methacrylic acid-ethylene glycol dimethacrylate polymers with different monomers ratio were synthesised by photochemical (UV irradiation at 365 nm) or thermal (oven at 60°C) initiation. Batch and continuous flow experiments were carried out to evaluate the capacity of these polymers to adsorb estradiol (E2), ethinylestradiol (EE2) and dienestrol (DEN). Adsorption isotherm studies revealed that Langmuir isotherm model was fitted with a better correlation than Freundlich isotherm. Finally, continuous flow experiments were carried out by microcolumn studies to check the suitability of the polymeric sorbent for the removal of estrogens from real water samples. When continuous removal experiments at 8 mL min–1 flow rate were carried out, breakthrough adsorption capacities of 28.5, 38 and 69.7 mg g–1 for E2, EE2 and DEN, respectively, were achieved.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 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.