Integrated QuEChERS combined with LC-MS/MS for high-throughput analysis of per- and polyfluoroalkyl substances in milk

Abstract

In this study, an integrated QuEChERS method was developed for the rapid determination of 22 per- and polyfluoroalkyl substances (PFASs) in milk by liquid chromatography-tandem mass spectrometry (LC-MS/MS). The extraction and purification processes were combined into one step with this method. Meanwhile, the solid-liquid separation was carried out by magnetic suction (Fe₃O₄-SiO₂) instead of the centrifugal process. The primary experimental parameters were optimized, including the type of extraction solvent, the amounts of magnetic nanomaterials (Fe₃O₄-SiO₂), and the purification materials (ZrO₂ and C₁₈). The developed method exhibits high precision (RSDs < 9.9%), low limits of detection (0.004-0.079 μg/kg) and limits of quantitation (0.01-0.26 μg/kg), and acceptable recovery (71.7-116%) under optimized conditions. The developed integrated QuEChERS method had clear superiority in terms of sample pretreatment time, operating procedures, reagent amount, and recovery. This makes it an excellent alternative analytical technique for PFAS residue measurement at low micrograms-per-kilogram ranges with desirable sensitivity.

Keywords: LC–MS/MS; Magnetic nanoparticles; Milk; Per- and polyfluoroalkyl substances; QuEChERS.