Persona: Garcinuño Martínez, Rosa Mª
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rmgarcinuno@ccia.uned.es
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Garcinuño Martínez
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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 Evaluation of total phenol pollution in water of San Martin Canal from Santiago del Estero, Argentina.(Elsevier, 2018-05) Acosta Rosales, Carina Andrea; López, Clara; Paniagua González, Gema; Garcinuño Martínez, Rosa Mª; Fernández Hernando, PilarSantiago del Estero is a province located in northwestern Argentina. The Dulce River is used for irrigation through a vast network of channels and ditches, including the San Martin Canal (SMC), which crosses the capital city of Santiago del Estero. This canal's water is used for drinking, as well as recreational use for the general population. However, this river has been seriously polluted for several decades. The present study focuses on the identification and the quantification of the water pollution levels of total phenols in the SMC according to the seasonal periods. Water samples from various areas of the canal in different months of the year, extending from December to September, were collected for analysis. Additionally, the concentration of total dissolved solids (TDS), chlorides, sulphates, nitrites and organic matter, as well as water hardness and alkalinity, were analysed in order to conduct a more complete study of the contamination of this area. The results showed a worrying total phenol concentration that exceeded the limit set by Argentine legislation for drinking water, as well as water for recreational use (5 μg/L). The total phenol (TP) concentration was directly determined by a molecular absorption spectroscopy method based on a new flow injection analysis system (FIA). Under the selected experimental conditions, the detection and quantification limits were 0.0490 and 0.1633 μg/mL, respectively. The developed method provides a number of improvements related to the speed of analysis, the restricted consumption of the reagents and sample volumes and the unnecessary sample treatment that contribute to environmentally friendly analytical chemistry. The results showed that TP make a significant contribution in the SMC pollution, especially during the months of April (400 ± 110 μg/L) and September (240 ± 20 μg/L). A high sulphate concentration that was higher than the limit allowed by the legislation was also found.Publicación A systematic review of methods of analysis for plastic additives in fisheries and aquaculture products(Taylor & Francis, 2025-02-06) Esther Garrido Gamarro; Garcinuño Martínez, Rosa Mª; Paniagua González, Gema; Fernández Hernando, Pilar; Organización de las Naciones Unidas para la Alimentación y la Agricultura (FAO); Universidad Nacional de Educación a DistanciaMicroplastic particles have been found in a variety of food commodities, and fisheries and aquaculture products seem to be one of the main contributors to the dietary exposure of microplastics, which are complex mixes of chemicals, containing polymers, plastics additivities, and environmental contaminants. The implications for food safety are not well understood. The lack of simple and efficient analytical techniques for the determination of microplastics as well as their additives in food are some of the challenges. To improve the understanding of the methods available for the determination of plastic additives, a systematic literature review was conducted focusing on methods to determine those plastic additives known for their possible endocrine disruption and/or carcinogenic activity, such as bisphenol A (BPA), bisphenol F (BPF), bisphenol S (BPS), 4- nonylphenol (NP-4), nonylphenol (NP), diethyl phthalate (DEP), di-n-butyl phthalate (DBP), di(2-ethylhexyl)phthalate (DEHP), and polybrominated diphenyl ether (PBDE) in fisheries and aquaculture products. The review aimed to identify the most common extraction and determination methods used for these analytes and assess their efficiency. The findings of this review shed light on the current state of analytical methodologies in this field and provide insights that could inform and guide further research.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 Characterization of Plastics Ingested by the Bioindicator Cory’s Shearwater from Tenerife Island (Canary Islands): Implications for Marine Environmental Monitoring(MDPI, 2025-11-03) Baena, Natalia; Paniagua González, Gema; Bravo Yagüe, Juan Carlos; Garcinuño Martínez, Rosa Mª; Rodríguez, Beneharo; Jiménez, Begoña; Fernández Hernando, Pilar; Muñoz Arnanz, Juan; Agencia Estatal de Investigación (España); Universidad Nacional de Educación a Distancia (UNED)Plastic pollution is a pressing environmental concern globally, especially in marine ecosystems. In this study, the evaluation of the potential ingestion of plastic, mostly in the form of microplastics (MPs), by fledglings of Cory’s shearwaters (Calonectris borealis) from the Canary Islands (Spain) was conducted. The total number of plastics found in the stomach samples was 674, primarily comprising large MPs (1–5 mm: 82%), followed by mesoplastics (>5–25 mm: 18%). The predominant morphology was threadlike (31.6%), followed by hard, irregularly shaped fragments (28.3%), microspheres (22.4%), and sheets (15.7%). Loads were found to overlap with those described for the same species in highly populated areas such as the Mediterranean Sea. Plastic counts above Cory’s threshold value may suggest poor environmental status for the Canary Current region. FTIR-ATR analysis evidenced the predominance of polyethylene (PE) (46.7%), polypropylene (PP) (24.6%) and polyamide (PA) (20.4%). This is likely linked not only to the fact that PE is the most produced plastic worldwide, but also the fact that, along with PP, it makes up the highest amount of single-use plastic products. Overall, findings provide a contamination-controlled, FTIR-verified baseline for fledglings from Tenerife; however, given the limited, single-season sample (n = 33) and opportunistic design, results are descriptive and not intended for population-level inference. Yet, the potential of Cory’s shearwater as a sentinel species to monitor plastic pollution is highlighted, emphasizing the urgent need for effective mitigation strategies to address plastic pollution in marine environments.Publicación Red RIEQA. EBSQA, un entorno para el aprendizaje autónomo y su evaluación continua(2009-09) Durand Alegría, Jesús Senén; Sánchez Muñoz, Pedro Jesús; Fernández Hernando, Pilar; Garcinuño Martínez, Rosa Mª; García Mayor, M AsunciónPublicación Synthesis and characterization of a molecularly imprinted polymer for the determination of spiramycin in sheep milk(Elsevier, 2017-04-15) Durand Alegría, Jesús Senén; García Mayor, M Asunción; Paniagua González, Gema; Fernández Hernando, Pilar; Garcinuño Martínez, Rosa MªA series of molecularly imprinted polymers (MIPs) comprising reactionary sites which are complementary to macrolide antibiotic spiramycin (SPI) were synthetized by noncovalent bulk polymerization technique. MIPs were synthesized under different polymerization process and their recognition efficiency was evaluated in binding studies in comparison with non-imprinted polymers. The best MIP was morphologically characterized and equilibrium assays were carried out. The MIP was evaluated as a sorbent for extraction and preconcentration of SPI from aqueous and sheep milk samples, and an off-line MISPE method followed by high-performance liquid chromatography with UV diode-array detection was established. Good linearity were obtained for SPI in a range of 24–965 μg kg−1 and the average recoveries at three spiked levels in milk samples were higher than 90% (RSD < 5%). Limit of quantification was 24.1 μg kg−1. Cross-reactivity studies from other macrolides with similar structure were tested. The optimum imprinted polymer showed a good selectivity and affinity for SPI, demonstrating the potential of the proposed MISPE for rapid, sensitive and effective sample pretreatment for selective determination of SPI in sheep milk samples.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 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 Mª; https://orcid.org/0000-0002-4031-1407New 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 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 Fiol, Xavier; Silva, Mónica; Solé, Montserrat; Freitas, Rosa; Deudero, Salud; Paniagua González, Gema; Soliz Rojas, Dulce Lucy; Fernández Hernando, Pilar; Garcinuño Martínez, Rosa Mª; https://orcid.org/0000-0002-3499-5494The 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.
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