A simple and rapid method was developed for evaluating 16 phthalic acid esters (PAEs) at the μg/kg level in a complex milk matrix using directly suspended droplet microextraction-gas chromatography mass spectrometry (DSDME-GC-MS). The different parameters for extraction and for the DSDME experiment were optimized, including You are free to submit the revised manuscript at a later date as a new submission. 10 g/L trichloroacetic acid concentration, 100 μL cyclohexane micro-droplet organic solvent, 1100 rpm stirring speed, 10 min extraction time and no salt amount. Validation experiments showed good linearity (γ>0.9878, 0.002-0.4 μg/mL), satisfactory precision (RSD<11%), and good accuracy (relative recovery of 70.2-108%) when analyzing milk samples using the optimized method. The limits of detection (LODs) ranged between 0.001 and 0.2 μg/L, and the limits of quantification (LOQs) ranged between 0.003 and 0.7 μg/L for 15 PAEs. Dinonyl phthalate (DINP) had a low response and did not have good linearity. The proposed method was successfully applied for the analysis of PAEs in real milk samples.
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