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.

In this study, we considered the reaction of (E)-1-[(2-phenylhydrazono)methyl]naphthalen-2-ol with iodobenzene diacetate in dichloromethane-produced novel 3-phenyl-3H-naphtho[1,2-e][1,2,3]oxadiazine in 11% yield. By analogy to previously published work, we suggested that the reaction proceeds via the intermediacy of an o-naphthoquinone azomethide that undergoes conjugated 6π-electrocylization to produce the product. 1D, 2D NMR, HRMS, IR, and UV-VIS spectra provided information that supported the structure of the product.

Flame retardants (FRs) and plasticizers are widely used additives that can accumulate in aquatic sediments, where strong sorption and matrix complexity hinder reliable trace analysis. Because the available literature spans diverse compound classes, extraction strategies, clean-up procedures, and instrumental methods, a focused comparison is needed to clarify how analytical choices relate to method performance. Candidate studies published between 2015 and 2026 were identified primarily through Google Scholar, complemented by PubMed and publisher platforms. These studies were screened for relevance to FR and plasticizer determination in sediments. The resulting evidence base comprised 77 unique primary publications, yielding 80 category-specific analytical entries. The review is restricted to aquatic sediment matrices and focuses on sample pretreatment, extraction, clean-up/preconcentration, and instrumental determination, with occurrence, toxicology, and risk considered only where they provide analytical context. The literature is assessed across the main stages of the analytical workflow, i.e., sample pretreatment, extraction, clean-up, and instrumental analysis, with emphasis on recovery, detection limits, solvent use, extraction time, and procedural complexity. The reviewed evidence shows distinct extraction patterns between the two analyte classes: Soxhlet extraction and pressurized liquid extraction (PLE/ASE) are strongly represented among FR workflows, whereas ultrasound-assisted extraction predominates among plasticizer studies, with microwave-assisted extraction and other approaches employed to a lesser extent. The influence of solvent selection and clean-up requirements on compatibility with GC- and LC-based determination is also considered. Particular attention is given to the trade-offs between analytical performance and the environmental and operational cost of the complete pipeline, rather than assigning intrinsic greenness to individual extraction techniques. The reviewed studies reveal current methodological trends, recurring limitations in reporting and comparability, and priorities for more efficient, reproducible, and environmentally responsible monitoring of FRs and plasticizers in aquatic sediments.