Simultaneous Determination of Aflatoxins and Benzo(a)pyrene in Vegetable Oils Using Humic Acid-Bonded Silica SPE HPLC–PHRED–FLD

In the present work, a rapid, accurate, and cost-effective method was developed for the simultaneous quantification of aflatoxins and benzo(a)pyrene in lipid matrices, using solid-phase extraction (SPE) via humic acid-bonded silica (HAS) sorbents, followed by high-performance liquid chromatography coupled with photochemical post-column reactor fluorescence spectroscopy (HPLC–PHRED–FLD) analysis. The major parameters of extraction efficiency and HPLC–PHRED–FLD analysis were investigated and this method was fully validated. The limits of quantification and the limits of detection were 0.05–0.30 and 0.01–0.09 µg kg(−1), respectively. The recoveries were 66.9%–118.4% with intra-day and inter-day precision less than 7.2%. The results of 80 oil samples from supermarkets indicated a high occurrence of BaP, and most of concentrations were within the requirements of EU and China food safety regulations. This is the first utilization of HAS–SPE HPLC–PHRED–FLD to simultaneously analyze the occurrence of aflatoxins and benzo(a)pyrene in vegetable oils.