Hypercrosslinked core‑shell polymer microspheres with amphipathic and amphoteric character for the solid‑phase extraction of acidic and basic pharmaceuticals from environmental waters

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Trullàs, Abril and Sànchez, Judit and Corrigan, Alan and Borrull, Francesc and Cormack, Peter A. G. and Fontanals, Núria and Marcé, Rosa Maria (2026) Hypercrosslinked core‑shell polymer microspheres with amphipathic and amphoteric character for the solid‑phase extraction of acidic and basic pharmaceuticals from environmental waters. Analytical and Bioanalytical Chemistry. ISSN 1618-2642 (https://doi.org/10.1007/s00216-026-06578-z)

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Abstract

Solid-phase extraction (SPE) is used extensively in analytical chemistry for the preconcentration and fractionation of analytes prior to chemical analysis, with enhancements in sorbent efficiency and selectivity being important R&D topics. Although core-shell particles are increasingly used as alternatives to traditional high-performance liquid chromatography (HPLC) stationary phases, their value as SPE sorbents is under-explored. Herein, we describe the design, synthesis and exploitation of core-shell polymer microspheres, where the microspheres are small (3.7 µm) and uniform (Cv = 5.5%), and where the shells are thin (~0.5 µm, which improves mass transfer and reduces eddy diffusion) and have high specific surface area (>1300 m2/g) and amphoteric character. The latter feature means that these microspheres offer both anion-exchange and cation-exchange interactions, which makes the SPE of anions and cations possible. Following synthesis, an SPE protocol using these microspheres as sorbent was optimized and validated using liquid chromatography-tandem mass spectrometry (LC–MS/MS) for the simultaneous retention of acidic and basic pharmaceuticals present in complex water samples. The inclusion of a clean-up step reduced matrix interferences. The method developed achieved satisfactory apparent recoveries (23–75% for river water, 20–88% for effluent wastewater, and 19–56% for influent wastewater), low matrix effects, detection limits within 0.05–2 ng/L for most compounds, and good repeatability and reproducibility across all sample matrices. Application of the SPE method to real environmental samples confirmed the presence of several target pharmaceuticals at ng/L concentration levels, demonstrating the applicability of the hypercrosslinked core-shell sorbent.

ORCID iDs

Trullàs, Abril, Sànchez, Judit, Corrigan, Alan, Borrull, Francesc, Cormack, Peter A. G. ORCID logoORCID: https://orcid.org/0000-0002-3390-8176, Fontanals, Núria and Marcé, Rosa Maria;
CORE (COnnecting REpositories)