Abstract: | A new silver‐functionalized silica‐based material with a core–shell structure based on silver nanoparticle‐coated silica spheres was synthesized, and silver nanoparticles were modified using strongly bound l‐ cysteine. l‐ Cysteine‐silver@silica was characterized by scanning electron microscopy and FTIR spectroscopy. Then, a solid‐phase extraction method based on l‐ cysteine‐silver@silica was developed and successfully used for bisphenol A determination prior to HPLC analysis. The results showed that the l‐ cysteine‐silver@silica as an adsorbent exhibited good enrichment capability for bisphenol A, and the maximum adsorption saturation was 20.93 mg/g. Moreover, a short adsorption equilibrium time was obtained due to the presence of silver nanoparticles on the surface of the silica. The extraction efficiencies were then optimized by varying the eluents and pH. Under the optimized conditions, good linearity for bisphenol A was obtained in the range from 0.4 to 4.0 μM (R2 > 0.99) with a low limit of detection (1.15 ng/mL). The spiked recoveries from tap water and milk samples were satisfactory (85–102%) with relative standard deviations below 5.2% (n = 3), which indicated that the method was suitable for the analysis of bisphenol A in complex samples. |