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    Quantification of PFAS in Oyster Tissue Using a Rapid QuEChERS Extraction Followed by UPLC-MS/MS Analysis
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    Abstract:
    Per- and poly-fluoroalkyl substances (PFAS) are a large group of man-made chemicals that repel oil, stains, grease, and water and are fire resistant. PFAS are known to be persistent in the environment and bioaccumulate in human and animal tissue, soil, and water. To mitigate human exposure to these chemicals, PFAS analysis by ultra-performance liquid chromatography coupled with tandem mass spectrometry (UPLC-MS/MS) was used to monitor their presence in the environment. This study focused on analyzing oysters harvested from coastal New England for 14 PFAS. The validated method addressed in this study utilized a quick, easy, cheap, effective, rugged, and safe (QuEChERS) approach using various sorbents and showed that the combination of primary secondary amine/graphitized carbon black (PSA/GCB) provided the most effective sample clean-up prior to analysis. The recoveries for the targeted analysis ranged from 61% to 116.3% with relative standard deviations from 2.4% to 13.3% at the 125.0 ng mL−1 analyte level. The method detection limits were from 0.33 ng g−1 to 6.75 ng g−1. In a targeted analysis of five unknown samples, two samples had a detectable level of the legacy compound, perfluorooctanesulfonic acid (PFOS).
    Keywords:
    QuEChERS
    Perfluorooctanoic acid
    Solid phase extraction
    Sample Preparation
    Clean-up
    Surveys of pesticide residues in fruit are important to demonstrate conformity with strict regulations of newly open markets for export of exotic fruit. Multi-residue methods are tools to ensure compliance with regulations and both the CEN and the AOAC have versions of QuEChERS that are used effectively as mainstream methods. The aim of this study was to assess their performance and pick the optimum one for this particular application using GC-MS. The use of graphitised carbon black (GCB) to improve clean-up was assessed. Optimisation of large volume injection (LVI) and implementation of concurrent back-flushing was needed in order to improve sensitivity at a low concentration levels for 33 pesticides (0.01 mg kg−1). Cleaner total ion current (TIC) profiles were obtained with the CEN method. Recoveries of most of the pesticides showed statistical differences (α = 0.05) when GCB was used in the AOAC method, unlike the CEN method. In general, GCB/no GCB use for CEN clean-up gave good, very similar results for all fruit, though some pesticides showed some adsorption on the GCB surface. The CEN general method was preferred since acceptable recoveries (> 80%) and RSD (< 20%) can be achieved for all analytes.
    QuEChERS
    Clean-up
    This manuscript describes a detailed evaluation of the different procedures of the modified QuEChERS method for pesticide residues in strawberries using UHPLC-DAD.
    QuEChERS
    Cartridge
    Clean-up
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