A novel analytical method based on nanofiber-packed solid-phase extraction (PFSPE) combined with HPLC-FLD has been successfully developed and applied to determine aflatoxin B1, B2, G1, G2 in foods. In order to effectively adsorb analytes from complex food matrices, four types of nanofibers based on skeleton of polystyrene–polyvinyl pyrrolidone were prepared by electrospinning and applied as adsorbent to home-made solid-phase extraction device. The effects of type of nanofibers, pH of sample, type and concentration of salt ion, type of activation solvent, type and volume of eluent, amount of nanofibers, and extraction time on the adsorption/desorption were investigated and optimized. Under optimal conditions, the method showed satisfactory linear relationship, with limits of detection (LODs) of 0.07–0.17 ng g−1, intra-day and inter-day RSDs for spiked samples of 1.3–8.0 % and 1.9–5.8 %, and absolute recoveries in the range of 60.1–98.4 %. The results presented the great potential to be utilized to determine AFs in foodstuffs.
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