[Determination of 23 perfluorinated and polyfluoroalkyl substances in eggs by ultra-high performance liquid chromatography-tandem mass spectrometry].

Abstract

OBJECTIVE: To establish a method for the simultaneous determination of 23 perfluorinated and polyfluoroalkyl substances（PFASs）, including perfluoroalkyl carboxylic acids（PFCAs）, perfluoroalkyl sulfonic acids（PFSAs）, and fluorotelomer sulfonic acids（FTSs）, in eggs, using organic solvent extraction, solid-phase extraction（SPE） cleanup, and ultra-high performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS）. METHODS: Chromatographic separation conditions, mass spectrometry detection parameters, SPE sorbents, reconstitution solvent, and syringe filter were optimized to achieve the best recovery and purification efficiency. Egg samples were extracted with acetonitrile, purified using a high-efficiency lipid-removal SPE column（HLB-P/HMR-Lipid）, and separated on a C18（2.1 mm×150 mm, 3 μm） reversed-phase column with a mobile phase consisting of 5 mmol/L ammonium formate in water and methanol. The analytes were detected in negative electrospray ionization（ESI-） mode with multiple reaction monitoring（MRM） and quantified using stable isotope-labeled internal standards. RESULTS: The 23 PFASs exhibited good linearity in the range of 0.20-50.0 ng/mL（r>0.990）. The limits of detection（LOD） and limits of quantification（LOQ） were 0.0022-0.0189 μg/kg and 0.0066-0.0567 μg/kg, respectively. The recoveries ranged from 70.2% to 110.6%, with relative standard deviations of 1.2%-8.9%（n=7）. This method was then applied to determine PFASs in 51 commercially available egg samples collected from Xinjiang. A total of five PFASs were detected, with a detection frequency of 33.3% and concentrations ranging from 0.185 to 1.88 μg/kg. CONCLUSION: This method is simple, sensitive, selective, and reproducible, making it suitable for the rapid determination of 23 PFASs in eggs.

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