Ultrasound-Assisted Extraction (UAE), and UHPLC–MS/MS Methodology for the Pharmaceutical Multiresidue Extraction and Analysis of Agricultural Soil Samples Vanessa Mendoza-Grimón, Javier Pacheco-Juárez, Rayco Guedes-Alonso, Juan Ramón Fernández-Vera, Esmeralda Estevez, Sarah Montesdeoca-Esponda, Zoraida Sosa-Ferrera, María del Pino Palacios-Díaz Agriculture Switzerland, 2026 Using reclaimed water for irrigation is an effective strategy in semi-arid regions facing water scarcity. However, this water may contain pharmaceutical residues, posing potential environmental and health risks. To ensure sustainable reuse, it is essential to study how these substances accumulate in soil and transfer to crops. The aim of this research was to develop and optimise a rapid Ultrasound-Assisted Extraction method combined with Ultra-High-Performance Liquid Chromatography–tandem Mass Spectrometry for quantifying 23 pharmaceuticals in non-cultivated soil. Following optimisation, 18 compounds were successfully extracted using a MeOH:H2O ratio of 75:25. The detection and quantification limits were found to range from 0.52 to 0.5 ng·g−1 and 1.75 to 35 ng·g−1, respectively. The matrix effects and recoveries varied by compounds’ type and concentration, but most results were acceptable. The evidence suggested that some drugs underwent microbial degradation. Soil irrigated with reclaimed water via subsurface drip since 2012 occasionally contained four pharmaceuticals (caffeine, carbamazepine, tamoxifen, and venlafaxine) at low concentrations, while others were absent. This indicates the capacity of soil to act as a barrier, and highlights the importance of proper water management. The study concludes that reclaimed water reuse is safe if supported by efficient treatment and management, offering a promising approach for long-term sustainability in water-scarce regions.
Functionality-Driven Optimization of Green Ultrasound-Assisted Extraction of Antioxidant Compounds from Edible Brown Algae Carolina Padrón-Sanz, Samanta García-Oms, Javier Pacheco-Juárez, Lorena Pasquali, Dolores Cejalvo-Lapeña Marine Drugs, 2025 The extraction of antioxidant compounds from brown macroalgae is of growing industrial interest; however, the weak correlation often observed between polyphenol content and antioxidant activity challenges the conventional strategy of optimizing only extraction yield. This study introduces, for the first time in brown macroalgae, a functionality-driven optimization approach in which ultrasound-assisted extraction (UAE) conditions are optimized based on antioxidant activity as the primary response variable, rather than compound concentration. A green UAE process was developed and optimized for four edible brown algae (Himanthalia elongata, Eisenia bicyclis, Sargassum fusiforme, and Laminaria ochroleuca), considering algae amount, solvent type and concentration, extraction time, ultrasound power, and temperature. The optimized extracts achieved 69.17–94.68% DPPH inhibition, together with high antioxidant capacity supported by ORAC (18.63–491.30 μmol TE g−1 DW) and FRAP (1.24–87.65 µmol Fe+2 g−1 DW) values, identifying E. bicyclis and H. elongata as the most promising species. Chromatographic analyses confirmed the presence of phlorotannins and carotenoid pigments such as fucoxanthin as the main contributors to antioxidant activity. Overall, this work validates a functionality-driven UAE optimization strategy for efficiently maximizing antioxidant activity in brown algal extracts.
Occurrence and assessment of emerging contaminants adsorbed onto microplastic debris in the Macaronesia region Javier Pacheco-Juárez, Zoraida Sosa‐Ferrera, Rayco Guedes-Alonso, Sarah Montesdeoca‐Esponda, María Esther Torres-Padrón, et al. Marine Pollution Bulletin, 2025 The occurrence and accumulation of microplastics in the aquatic environment has becomes a global problem. These microplastics can adsorb on their superficies other hydrophobic organic chemicals surrounding and act as vectors for the transport of these contaminants and transfer to organisms. This study presents the first coordinated comprehensive three-year spatial-temporal assessment of the occurrence and distribution of emerging contaminants adsorbed on microplastic debris collected from 32 beaches across of Macaronesia (Canary Islands, Madeira, Azores, and Cabo Verde). Two types of microplastic debris (pellets and fragments) were analysed for 34 contaminants using previously established analytical procedures. These included twelve UV filters (UVFs) and UV stabilizers (UVSs) commonly added to personal care products; thirteen steroid hormones and nine pharmaceutical compounds. Concentrations were typically in the nanograms per gram range, obtaining highest concentrations for UV compounds, followed by hormones and, in much lower concentration, pharmaceuticals, possibly due to their hydrophilic nature. The most frequently detected compounds of each family were octocrylene (UVFs), levonorgestrel (hormones) and caffeine (pharmaceuticals) found in 69.12 %, 36.65 % and 29.89 % of the samples, respectively. This study presents a unique multi-archipelago dataset revealing unexpected contamination patterns including significant high concentrations of UV compound even on uninhabited and protected beaches such as Achados Beach (Santa Luzia, Cabo Verde), suggesting the influence of long-range oceanic transport. The findings underscore the ecological risks posed by key pollutants like octocrylene associated with plastics in insular ecosystems. This baseline data is crucial to inform mitigation strategies, including the regulation of UV filters in coastal and marine environments. • Microplastics (MPs) can adsorb and transport emerging organic contaminants. • UV compounds, hormones, and pharmaceuticals were analysed in MPs from Macaronesia. • Microplastic debris were collected from 32 beaches from Macaronesia over three years. • A validated UAE-UHPLC-MS/MS method was applied for target compounds analysis. • Findings reveal potential exposure to hazardous chemicals by plastic pollution.
A survey of the presence of pharmaceutical residues in wastewaters. Evaluation of their removal using conventional and natural treatment procedures R. Guedes-Alonso, S. Montesdeoca-Esponda, J. Pacheco-Juárez, Z. Sosa-Ferrera, J. J. Santana-Rodríguez Molecules, 2020 To encourage the reutilization of treated wastewaters as an adaptation strategy to climate change it is necessary to demonstrate their quality. If this is ensured, reclaimed waters could be a valuable resource that produces very little environmental impact and risks to human health. However, wastewaters are one of the main sources of emerging pollutants that are discharged in the environment. For this, it is essential to assess the presence of these pollutants, especially pharmaceutical compounds, in treated wastewaters. Moreover, the different treatment processes must be evaluated in order to know if conventional and natural treatment technologies are efficient in the removal of these types of compounds. This is an important consideration if the treated wastewaters are used in agricultural activities. Owing to the complexity of wastewater matrixes and the low concentrations of pharmaceutical residues in these types of samples, it is necessary to use sensitive analytical methodologies. In this study, the presence of 11 pharmaceutical compounds were assessed in three different wastewater treatment plants (WWTPs) in Gran Canaria (Spain). Two of these WWTPs use conventional purification technologies and they are located in densely populated areas, while the other studied WWTP is based in constructed wetlands which purify the wastewaters of a rural area. The sampling was performed monthly for two years. A solid phase extraction (SPE) coupled to ultra-high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) method was applied for the analysis of the samples, and the 11 pharmaceuticals were detected in all the studied WWTPs. The concentrations were variable and ranged from ng·L−1 in some compounds like diclofenac or carbamazepine to µg·L−1 in common pharmaceutical compounds such as caffeine, naproxen or ibuprofen. In addition, removal efficiencies in both conventional and natural purification systems were evaluated. Similar removal efficiencies were obtained using different purifying treatments, especially for some pharmaceutical families as stimulants or anti-inflammatories. Other compounds like carbamazepine showed a recalcitrant behavior. Secondary treatments presented similar removal efficiencies in both conventional and natural wastewater treatment plants, but conventional treatments showed slightly higher elimination ratios. Regarding tertiary system, the treatment with highest removal efficiencies was reverse osmosis in comparison with microfiltration and electrodialysis reversal.
