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<p>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&amp;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&#xa0;µm) and uniform (<i>C</i><sub>v</sub> = 5.5%), and where the shells are thin (~0.5&#xa0;µm, which improves mass transfer and reduces eddy diffusion) and have high specific surface area (&gt;1300 m<sup>2</sup>/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&#xa0;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&#xa0;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.</p> Graphical abstract <p></p>

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

  • 期刊论文

  • 出版模式：

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  • 发表日期：

    2026年5月28日

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  • Abril Trullàs,
  • Judit Sánchez,
  • Alan Corrigan,
  • Francesc Borrull,
  • Peter A. G. Cormack,
  • Núria Fontanals,
  • Rosa Maria Marcé

摘要

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.

Graphical abstract