Chemical Engineering, Catalysis, Environmental Chemistry, Waste Management and Disposal
17
Scopus Publications
Scopus Publications
Rapid carbamazepine detection by means of a disposable electrochemical sensor based on a molecularly imprinted polymer Verónica Poza-Nogueiras, Antón Puga, João G. Pacheco, Cristina Delerue-Matos Talanta, 2026 The presence of pharmaceuticals such as carbamazepine (CBZ) in water environments poses a threat, highlighting the importance of developing analytical tools for the detection and quantification of these compounds. In this work, for the first time a molecularly imprinted polymer (MIP) sensor was obtained on a screen-printed carbon electrode (SPCE) for the rapid detection of CBZ. This simple and portable voltammetric sensor was obtained by electropolymerization of 3,4-ethylenedioxythiophene (EDOT) as the functional monomer in the presence of CBZ as the template molecule. Using differential pulse voltammetry (DPV) as the detection method, the construction parameters were assessed and optimized. As a result, the optimal sensor was obtained performing the following steps: i) an activation with 50 mM of H 2 SO 4 , ii) an electropolymerization performing 20 cycles of cyclic voltammetry using 4.5 mM of EDOT and 1mM of CBZ, iii) an extraction with HCl 0.1 M during 30 min, and iv) an incubation in PBS pH 10 during 15 min. A linear analytical response was obtained in the range of 1-50 μM, with a LOD of 0.58 μM. The prepared sensor showed high selectivity towards CBZ over pharmaceuticals with similar chemical structures (CBZ 10,11-epoxide, diclofenac and diltiazem), with a response under 5% of that for CBZ. Additionally, its performance in real water samples was assessed, yielding good recoveries. Hence, an easy-to-use MIP-based sensor was successfully developed with potential applications for on-site monitoring of CBZ in the environment. • First reported MIP-based sensor on SPCE for carbamazepine (CBZ) was developed. • The MIP film was obtained through electrochemical polymerization of EDOT. • High sensitivity and selectivity towards CBZ obtained after optimization. • It successfully detected CBZ in tap, river and sea water samples. • The proposed MIP-sensor provides simple, low cost and rapid CBZ detection in water.
Electro-Fenton Degradation of Pirimicarb Using Basil Waste-Derived Catalyst Support Antón Puga, Ana Rita Alves, Cristina Soares, Sónia Figueiredo, Cristina Delerue-Matos Proceedings of the 2025 IEEE 15th International Conference Nanomaterials Applications and Properties Nap 2025, 2025 In this work, basil (Ocimum basilicum) residues were valorized through controlled pyrolysis to produce a functional biochar, used as a catalytic support in an electro-Fenton (EF) process for the degradation of the pesticide pirimicarb. The system was optimized in batch mode and adapted to continuous flow under simulated conditions of a wastewater treatment plant. The biochar exhibited favorable properties for hydroxyl radical generation, achieving over 100% removal in batch and more than 65% in continuous mode. This approach offers a sustainable alternative for tertiary treatment within circular economy frameworks.
Pineapple Waste Utilization: Generating Wealth from Waste in a Circular Economy Tanara Motta, Maria Fernanda Nogueira, Francisca Santos, Antón Puga, Filipe Fernandes, Manuela Correia, Clara Grosso, Cristina Soares, Cristina Delerue‐Matos Biorefining Fruit Waste Technological Advances in A Circular Bioeconomy, 2025 Pineapple ( Ananas comosus (L.) Merr.), a widely cultivated tropical fruit, generates significant amounts of agricultural and industrial waste, including peels, crowns, leaves, and cores. These by-products, often discarded, present an opportunity for sustainable valorization within a circular economy framework. This chapter explores diverse biovalorization pathways for pineapple waste, including its application in food, cosmetics, pharmaceuticals, and bioenergy production. Nutrient-rich residues can be repurposed into compost, biochar, and animal feed, promoting sustainable agriculture. Rich in cellulose, pineapple leaves can be processed into biodegradable textiles, pots, and packaging materials, offering alternatives to synthetic products. The production of bioethanol, biochar, and bioactive compounds like bromelain highlights the potential of pineapple residues for renewable energy and high-value products. Additionally, pineapple waste demonstrates promise in wastewater treatment and soil remediation, addressing environmental challenges. The chapter evaluates the feasibility and industrial prospects of pineapple waste utilization through a techno-economic analysis. These valorization strategies emphasize sustainability, economic efficiency, and waste minimization, aligning with global sustainability goals.
Antidepressants and COVID-19: Increased use, occurrence in water and effects and consequences on aquatic environment. A review Antón Puga, Manuela M. Moreira, M. Angeles Sanromán, Marta M. Pazos, Cristina Delerue-Matos Science of the Total Environment, 2024 The COVID-19 pandemic changed the consumption of many drugs, among which antidepressants stand out. This review evaluated the frequency of antidepressant use before and after COVID-19. Once the most consumed antidepressants were identified, detecting a variation in the frequency of consumption on the different continents, an overview of their life cycle was carried out, specifying which antidepressants are mostly detected and the places where there is a greater concentration. In addition, the main metabolites of the most used antidepressants were also investigated. A correlation between the most consumed drugs and the most detected was made, emphasizing the lack of information on the occurrence of some of the most consumed antidepressants. Subsequently, studies on the effects on aquatic life were also reviewed, evaluated through different living beings (fish, crustaceans, molluscs, planktonic crustaceans and algae). Likewise, many of the most used antidepressants lack studies on potential adverse effects on aquatic living beings. This review underscores the need for further research, particularly focusing on the life cycle of the most prescribed antidepressants. In particular, it is a priority to know the occurrence and adverse effects in the aquatic environment of the most used antidepressants after the pandemic.
Novel 3D electro-Fenton reactor based on a catalytic packed bed reactor of perovskite/carbon microelectrodes for the removal of carbamazepine in wastewater A. Cruz del Álamo, A. Puga, C.M. Dias Soares, M.I. Pariente, M. Pazos, R. Molina, M.A. Sanromán, F. Martínez, C. Delerue-Matos Journal of Environmental Chemical Engineering, 2024 This presents the efficacy of a 3D-ElectroFenton (3D-EF) reactor with active perovskite/carbon black/PTFE microelectrodes for the removal of carbamazepine (CZP) present in wastewater. Incorporating particle microelectrodes in the reactor enhanced the electron transfer and improved the electrocatalytic efficiency, leading to a more effective CZP removal. The optimal operational conditions were meticulously determined, including current intensity (0.05 – 0.3 A) and particle loading (0 – 1.5 g), to optimize the process and minimize energy consumption. The findings reveal that a current intensity of 0.2 A was the most effective, achieving 90% of CZP removal in 60 min and 3.86 kWh/mg of CZP. A higher current intensity of 0.3 A significantly increased the energy consumption (6.02 kWh/mg of CZP) for a total and faster CZP removal. The 3D-EF reactor was also operated continuously with ultrapure water and real urban wastewater fortified with CZP. A remarkable 62% CZP removal after 96 h on continuous operation was achieved with urban wastewater. Physicochemical and electrochemical characterization of microelectrodes demonstrated their high mechanical integrity and chemical stability. Our study underscores the potential of a 3D-EF system as a promising advanced oxidation process to address the continuous removal of antidepressant carbamazepine as one of the more resistant micropollutants of emerging concern in wastewater treatment, offering hope for a more efficient and sustainable future.
Efficient carbamazepine removal from wastewater using a continuous three-dimensional electro-Fenton system at natural pH Antón Puga, Cristina Soares, Ana Cruz del Álamo, M. Isabel Pariente, Raúl Molina, Fernando Martínez, M. Angeles Sanromán, Marta M. Pazos, Cristina Delerue-Matos Journal of Water Process Engineering, 2024 This research presents an innovative approach for removing carbamazepine (CBZ), a persistent pharmaceutical contaminant, using a three-dimensional electro-Fenton (TDEF) system. The preliminary phase involved validating the configuration of the TDEF reactor. First, commercial electrodes, metal-mixed oxide as the anode, and stainless steel as the cathode were selected. After that, a third particulate electrode was introduced, working with two options: vineyard biochar and a lab-made conglomerate of perovskite and carbon black. Additionally, two collector systems were evaluated for easy recovery and reuse of this three-dimensional particulate electrode: a thermoplastic tube and a silicone bag. Among the tested configurations, the perovskite conglomerate retained within a silicone bag proved the most effective, achieving a 91 % CBZ removal efficiency at a natural pH (6.5) during a 5-hour batch operation. Considering excellent results, the system's efficacy was confirmed working on fortified tertiary wastewater (FTW) in continuous mode, emphasizing the adaptability to real-world conditions. Moreover, the reusability of microparticles was confirmed for three consecutive cycles, as well as through the characterization study using FTIR, without important modifications in the material after use. Results confirmed the technology's potential for removing CBZ operating with real conditions. Thus, the proposed process represents an alternative treatment to remove CBZ efficiently in a wide range of concentrations from real wastewater in a continuous treatment with a reasonable energy cost (ca. 27 kW/h·gCZP). This novel system represents a cost-effective, straightforward experimental setup suitable for future scaling and industrial applications.
Novel Fe-Ti nanoparticles synthesized in deep eutectic solvents for enhanced photo-electro-Fenton processes: Synergistic effects and environmental applications A. Puga, J. Meijide, M. Pazos, M.A. Sanromán, E. Rosales Journal of Molecular Liquids, 2024 An innovative titanium-magnetite (Fe-Ti) catalyst was developed using a production strategy based on water-free solvents such as deep eutectic solvents (DES) for the removal of persistent pollutants. The prepared catalyst was applied in electro-Fenton and photo-electro-Fenton processes. To this end, a new cell design with electrodes based on conductive materials was developed using 3D printing in two different electrochemical cells configurations: vertical electrode configuration (VEC) and horizontal electrode configuration (HEC). The HEC showed good performance attaining a yield hydrogen peroxide production of 20 mg·L−1 and being able to operate in electro-Fenton degradation batch assays for the removal of the drugs (Antipyrine and Lissamine Green B). Then, the heterogeneous bimetallic catalyst (BC-FeTi) was tested and compared with the monometallic Fe catalyst (MC-Fe). The results with both catalysts showed a synergistic effect combining electrochemical oxidation and Fenton reaction, promoting the best removal of the target pollutants. Subsequently, the contribution of UV radiation was evaluated with BC-FeTi, achieving that more than 80 % of both pollutants were removed in 80 min by the photo-Fenton process, confirming the high affinity of oxidizing free radicals for high molecular weight organic molecules. Finally, the simultaneous application of electro- and photo-oxidation (photo-electro-Fenton) significantly improved the removal of the target contaminants from the aqueous solution, achieving complete removal in 50 and 80 min for Lissamine Green B and Antipyrine, respectively. The stability and reusability of BC-FeTi and 3D-printed electrodes were achieved in five successive working cycles, with negligible loss of activity compared to new catalysts, which achieved greater than 99 % removal after five consecutive runs. Leaching of iron and titanium from the catalyst evaluated throughout the cycles, was low, totalling 2.7 and 4.5 % at the end of the fifth cycle.
Activity and stability of bifunctional perovskite/carbon-based electrodes for the removal of antipyrine by electro-Fenton process A. Cruz del Álamo, A. Puga, M.I. Pariente, E. Rosales, R. Molina, M. Pazos, F. Martínez, M.A. Sanromán Chemosphere, 2023 Bifunctional perovskite/carbon-black(CB)/polytetrafluoroethylene(PTFE) electrodes for electro-generation and catalytic decomposition of hydrogen peroxide to oxidizing hydroxyl radicals have been fabricated. These electrodes were tested for electroFenton (EF) removal of antipyrine (ANT) as a model antipyretic and analgesic drug. The influence of the binder loading (20 and 40 wt % PTFE) and type of solvent (1,3-dipropanediol and water) was studied for the preparation of CB/PTFE electrodes. The electrode prepared with 20 wt % PTFE and water exhibited a low impedance and remarkable H2O2 electro-generation (about 1 g/L after 240 min, a production rate of ca. 6.5 mg/h·cm2). The incorporation of perovskite on CB/PTFE electrodes was also studied following two different methods: i) direct deposition on the CB/PTFE electrode surface and ii) addition in the own CB/PTFE/water paste used for the fabrication. Physicochemical and electrochemical characterization techniques were used for the electrode's characterization. The dispersion of perovskite particles in the own electrode matrix (method ii) exhibited a higher EF performance than the immobilisation onto the electrode surface (method i). EF experiments at 40 mA/cm2 and pH 7 (non-acidified conditions) showed ANT and TOC removals of 30% and 17%, respectively. The increase of current intensity up to 120 mA/cm2 achieved the complete removal of ANT and 92% of TOC mineralisation in 240 min. The bifunctional electrode also proved high stability and durability after 15 h of operation.
Application of Deep Eutectic Solvents (DES) for the Synthesis of Iron Heterogeneous Catalyst: Application to Sulfamethoxazole Degradation by Advanced Oxidation Processes Antón Puga, Emilio Rosales, Marta Pazos, María Angeles Sanromán Catalysts, 2023 The development of novel approaches to the remotion of pharmaceuticals in wastewater is a subject of concern due to their effect on living beings and the environment. Advanced oxidation processes and the use of relevant catalysts are feasible treatment alternatives that require further development. The development of suitable heterogeneous catalysts is a necessity. This work proposes the synthesis of an iron catalyst in a deep eutectic solvent (Fe-DES) composed of choline chloride and citric acid, which was physically and chemically characterized using SEM-EDS and TEM, FTIR, RAMAN, XRD and XPS. The characterisation confirmed the presence of iron in the form of hematite. Fe-DES was shown to be a multipurpose catalyst that can be applied in the removal of sulfamethoxazole as a reagent in the Fenton and electro-Fenton processes and as an activator of peroxymonosulfate (PMS) processes. After testing the catalyst with the aforementioned techniques, the best result was achieved by combining these processes in an electro-PMS, with great efficiency achieved by dual activation of the PMS with the catalyst and electric field, attaining total elimination at natural pH in 90 min. Furthermore, the degradation was confirmed by the detection of short-chain carboxylic acids (oxalic, succinic, and acetic) and reduction in toxicity values. These results confirm the suitability of Fe-DES to degrade high-priority pharmaceutical compounds.
