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Microextraction by Packed Sorbent (MEPS) represents a significant evolution of solid-phase extraction (SPE) that integrates sorbent material directly into a syringe, thereby miniaturizing the extraction process and reducing solvent consumption. This approach maintains the fundamental principles of SPE, selective retention of analytes on a sorbent phase followed by elution, while eliminating the need for traditional cartridge systems and associated handling steps. The syringe-based configuration simplifies workflow, enabling rapid sample processing with minimal solvent requirements, which aligns MEPS with the principles of green chemistry. In MEPS, the sorbent bed is repeatedly conditioned, loaded with the sample, washed to remove matrix interferences, and finally eluted with a small-volume solvent into a receiving vial, making it particularly well-suited for routine analyses and high-throughput applications. A critical consideration in MEPS is the choice of sorbent and its compatibility with the target analytes and the sample matrix. The packed syringe format permits the use of a wide range of sorbent chemistries, from reversed-phase and normal-phase silica to polymeric sorbents and mixed-mode materials that combine hydrophobic interactions with ion-exchange functionality. The selection of sorbent influences extraction efficiency, selectivity, and robustness against matrix effects, with optimization often involving adjustments to conditioning, sample loading volume, wash strength, and elution solvent composition. Polyethylene glycol (PEG) has emerged as a versatile component in adsorption science due to its unique physicochemical properties, including hydrophilicity, biocompatibility, and tunable molecular weight. As an adsorbent modifier or supporting matrix, PEG can impart increased hydrophilicity to surfaces, reduce nonspecific binding, and create flexible, water-rich environments that influence the partitioning behavior of various analytes. The polymer’s ability