Phthalic acid esters (PAEs) were determined by aromatic hydroxylation fluorimetry. PAEs can react with OH in VMT-BiFeO3/H2O2 to form fluorescent hydroxyl phthalates. Fluorescence intensity is proportional to PAEs concentration. A good linear relationship was obtained in range of 3.8 × 10−7 to 4.8 × 10−5 mol L−1. PAEs in airborne particulates were determined with satisfactory results.