A novel analytical proposal based on nanofiber-packed solid-phase extraction coupled with high performance liquid chromatography-fluorescence detector (HPLC-FLD) has been successfully developed for determining aflatoxin B1 (AFB1) in foods. Four types of nanofibers, including polystyrene (PS) nanofibers, polypyrrole (PPY) nanofibers, polystyrene–acrylic resin (PS–AR) nanofibers, and polystyrene–polyvinyl pyrrolidone (PS–PVP) nanofibers, were fabricated by electrospinning and utilized to prepare a home-made extraction device. In this study, the factors of different fibers, namely, fiber dosage, pH of extraction solution, type of salt ion, concentration of salt ion, and volume of the eluent were optimized. Under optimized conditions, the method showed good linearity in the range of 0.1–40 ng mL⁻¹ with a correlation coefficient greater than 0.999 and good inter-day accuracy (90.8–112.7% recovery) and precision (1.8–3.6% intra-day RSDs, 2.6% inter-day RSD), and the limit of detection (LOD) was 0.05 ng mL⁻¹. Due to its cost-effective, time-saving, environmentally friendly, and simple performance, it has the potential to be utilized to determine aflatoxins in complicated matrices.

A sensitive analytical method based on packed-nanofiber solid phase extraction (PFSPE) and high performance liquid chromatography (HPLC) has been developed for determining chloramphenicol (CAP) in milk. Polystyrene–polyvinylpyrrolidone (PS–PVP) composite nanofibers were fabricated by electrospinning and utilized to prepare a home-made extraction device. With optimal conditions, 12 min of HPLC analysis with isocratic elution was successfully applied to determine CAP in milk. The analyte was separated well and blank milk did not disturb determination, the linearity was good in the range of 0.5–10 μg L⁻¹, and the recoveries were in the range of 97.5–104.0%. The intra-day and inter-day RSDs for spiked samples were respectively 4.6–7.1% and 8.4%, all below 10%. The limit of detection (LOD) was determined to be 0.2 μg L⁻¹. Due to its simplicity, low-cost and time-saving, the method has the potential to be applied to monitor antibiotic residues in dairy products with complex matrices.