Hypercrosslinked strong anion-exchange polymers for selective extraction of fluoroquinolones in milk samples

In this work, hypercrosslinked strong anion-exchange polymer resins (HXLPP-SAX) were synthesized and evaluated as solid-phase extraction (SPE) sorbents for extracting fluoroquinolones (FQs) in milk samples. These particles were prepared using a protocol that was facile and cost-effective by combining hypercrosslinking reactions and quaternisation reactions in one step. After the synthesis, the morphological properties and anion-exchange, adsorption, and selectivity performances of the HXLPP-SAX resins were characterized and evaluated. It was shown that the polymers were monodisperse microspheres, with the mean diameters of 2-4 μm, ion-exchange capacity (IEC) of 0.311 meq/g, and specific surface area more than 1000 m²/g. The resins applied as SPE sorbents possessed high selectivity in the extraction of amphoteric compounds (enoxacin and enrofloxacin as the representatives) followed by HPLC-UV analysis, as compared to commercially available strong anion-exchange sorbents (Oasis MAX). The SPE-HPLC-UV method was fully validated and exhibited good linearity (10-2000 ng/g, R² ≥ 0.997), low limits of detection (2.8-5.1 ng/g), good recoveries (85.8%-117.9%, RSDs ≤ 7.1%) and precisions (intra-day RSDs ≤ 7.7% and inter-day RSDs ≤ 9.4%). Then the method was performed the selective enrichment of six FQs (enoxacin, norfloxacin, ciprofloxacin, lomefloxacin, enrofloxacin, and sparfloxacin) in milk samples. The present results demonstrated that the proposed resins exhibited a promising potential for the enrichment and determination of FQ residues in milk samples as well as in other samples with complex matrices.