In this study, a highly sensitive and reliable method for the determination of 20 polyfluoroalkane substances (PFASs) in milk was established using the QuEChERS approach and an online interference trapping LC-MS/MS analysis. By a calibration with stable-isotope-labeled internal standards, we showed that the method displayed excellent linear dynamic ranges for 20 PFASs (correlation coefficients ≥0.997). The LOQs for the two types of PFASs, perfluorinated carboxylic acids (PFCAs) and perfluorinated sulfonic acids (PFSAs), were 0.010 and 0.050 μg/L, respectively. At the three spiking levels, the average recoveries for PFCAs ranged from 78.5 to 111% with the RSD (n = 6) within 1.20-13.1%, and those for PFSAs ranged from 72.8 to 105% with the RSD (n = 6) within 3.53-14.9%. By the developed method, 16 PFASs were found to be positive in 46 milk samples, and the levels for the PFASs with longer chains were significantly higher than those reported from other known regions.
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