Development and validation of modified QuEChERS method combined with LC-MS/MS for high-throughput analysis of per- and polyfluoroalkyl substances in fish samples

A rapid and accurate integrated QuEChERS method was developed for analyzing 26 of per- and polyfluoroalkyl substances (PFAS) in fish samples. The magnetic Fe3O4-TiO2 material was used as magnetic separation medium and purification adsorbent to remove proteins. This facilitated rapid phase separation and enabled the extraction and purification processes to be completed in a single step within 5 min. Key factors of the integrated QuEChERS method, including the extraction solution, salting-out and dehydrating reagents, and purification adsorbents, were optimized to ensure effective recovery of PFAS and the elimination of matrix interferences. Under these optimized conditions, systematic method validation exhibited good linearity (R-2 > 0.9931). The method limit of detection ranged from 0.010 to 0.048 mu g/kg, and the method limit of quantitation ranged from 0.025 to 0.050 mu g/kg. The PFAS recoveries varied from 71.3 % to 116.3 % at spiked concentrations of 0.025, 0.05, 10 and 100 mu g/kg, with intra-day RSDs and inter-day RSDs below 11.8 % and 9.0 %, respectively. Compared to the reported QuEChERS and SPE methods, the integrated QuEChERS approach presents distinct advantages in operating procedure, organic solvent usage, pre-treatment time, and offers comparable recoveries and RSDs. When this method was applied to real sample analyses, PFAS were detected in all fish samples with total concentrations ranging from 0.813 mu g/kg to 4.015 mu g/kg. Consequently, the developed method showcases its significant value for the rapid and high-throughput analysis of multiple PFAS in diverse fish samples.