A multi-residue method was developed to identify and quantify pharmaceutical drug residues in full-fat milk, using a modified QuEChERS extraction procedure and sonication combined with Ultra-High-Performance Liquid Chromatography–High-Resolution Orbitrap Mass Spectrometry (UHPLC-HR-Orbitrap-MS). Sample preparation involves three different QuEChERS extraction procedures and sorbents for the purification step. The optimized modified extraction method, combined with the clean-up approaches using C18 and the EMR-Lipid sorbent, has been validated in terms of linearity, recovery, precision, LOD and LOQ, matrix effects (ME) and expanded uncertainty. The optimized method showed a linearity >0.9903, recoveries within the range 65.1–120.1%, precision (expressed as %RSD) <17.5%, medium (<39.9%) to low (<16.7%) matrix effects and acceptable expanded uncertainty (<33.1%). Finally, the proposed method was applied to representative real samples of milk (by local markets), revealing the existence of one pharmaceutical drug (imidocarb) in one sample.

The presence of organic pollutants such as pesticides and pharmaceuticals in the aquatic environment, and especially in regions where fish farms are installed, is a matter of major importance due to their possible risks to ecosystems and public health. The necessity of their detection leads to the development of sensitive, reliable, economical and environmentally friendly analytical methods for controlling their residue in various environmental substrates. In the present work, a solid-phase extraction method was developed, optimized and validated for the analysis of 7 pesticides and 25 pharmaceuticals in seawater using LC-HR-LTQ/Orbitrap-MS. The method was then applied in seawater samples collected from an aquaculture farm located in the Ionian Sea, Greece, in order to evaluate environmental pollution levels. None of the pesticides were detected, while paracetamol was the only pharmaceutical compound that was found (at trace levels). At the same time, passive sampling was conducted as an alternative screening technique, showing the presence of contaminants that were not detected with spot sampling. Among them, irgarol was detected and as far as pharmaceuticals is concerned, trimethoprim and sulfadiazine were found; however, all positive findings were at the very low ppt levels posing no threat to the aquatic environment.

Pharmaceuticals and personal care products (PPCPs) are among the most frequently detected emerging pollutants in aquatic sediments, raising increasing concerns due to their persistence, bioaccumulation potential, and ecological impact. As sediments act both as reservoirs and secondary sources of contamination, effective and environmentally responsible analytical methodologies are essential for accurate environmental monitoring and risk assessment. This review presents a critical evaluation of extraction-based workflows for PPCP determination in sediment matrices, covering literature published from 2015 to 2025. We systematically analyze each step of the analytical pipeline, including sample pre-treatment, extraction, clean-up, and instrumental analysis, while emphasizing how method selection and optimization affect recovery rates, sensitivity, and detection limits. Special attention is paid to the physicochemical characteristics of PPCPs that govern extraction behavior, as well as to the trade-offs between analytical efficiency and environmental sustainability, such as solvent type, energy demand, and method greenness. By consolidating current knowledge, this work aims to lay a theoretical foundation for researchers and practitioners in selecting suitable, robust, and sustainable analytical strategies for effective environmental protection.

The widespread presence of pharmaceutical active compounds (PhACs) in aquatic environments raises significant environmental and public health concerns, particularly through their accumulation in marine biota and potential transfer to humans via seafood. In aquaculture, fish feed is essential for production but may also act as a pathway for contaminants in the marine environment. This study aimed to develop and validate an analytical method for the extraction and quantification of 14 antibiotics and ethoxyquin antioxidant in fish tissue and feed. Two QuEChERS-based extraction protocols were compared: the AOAC 2007.01 method (Method A) using Z-Sep⁺ as clean-up, and the original QuEChERS method (Method B) employing Enhanced Matrix Removal (EMR)-lipid. Ultra-performance liquid chromatography coupled with Orbitrap mass spectrometry using electrospray ionization in positive and negative mode was applied for identification and quantification. Validation included assessment of recovery, linearity, precision, limits of detection and quantification, uncertainty, matrix effects, and process efficiency. Both methods showed good linearity (R² > 0.9899) and precision (<19.7%). Method B achieved superior recoveries for most analytes in both fish tissue (70–110%) and feed (69–119%), with lower uncertainties (<18.4%) compared to Method A. Overall, the original QuEChERS method demonstrated better analytical performance, supporting its application as a green, robust tool for monitoring emerging contaminants in aquaculture products.