Abstract

A rapid hybrid solid phase extraction (HybridSPE®) protocol tailored to ultra-performance liquid chromatography–electrospray ionization tandem mass spectrometry (UPLC®–ESI–MS/MS) analysis was developed for the determination of 15 per- and polyfluoroalkyl substances (PFAS) in liver tissue from harbour porpoises (Phocoena phocoena). The HybridSPE® technique has been applied in trace concentration bioanalysis, but it was mainly used for liquid biological media until now. In this study, the protocol was applied on tissue matrix, and it demonstrated acceptable absolute recoveries (%) ranging from 44.4 to 89.4%. The chromatographic separation was carried out using a gradient elution program with a total run time of 4 min. The inter-day method precision ranged from 2.15 to 15.4%, and the method limits of detection (LODs) ranged from 0.003 to 0.30 ng/g wet weight (w.w.). A total of 20 liver samples were analyzed to demonstrate the applicability of the developed method in liver tissue from a wildlife species.

Highlights

  • Per- and polyfluoroalkyl substances (PFAS) are a versatile group of chemicals used in applications where oil and water repellence, and high thermal and chemical stability, are required [1]

  • Several bioanalytical methods are available for the determination of PFAS in a variety of biological matrices, and liquid chromatography–tandem mass spectrometry (LC-MS/MS) is currently the main instrumental technique applied for their analysis, achieving low limits of detection that can reach the picogram range [10]

  • 1% (w/v) ammonium formate, respectively; the results indicated acceptable extraction efficiency

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Summary

Introduction

Per- and polyfluoroalkyl substances (PFAS) are a versatile group of chemicals used in applications where oil and water repellence, and high thermal and chemical stability, are required [1]. The first observations of PFAS toxicity were reported many decades ago, but it was only in the early 2000s when both the widespread environmental occurrence of PFAS and their associated public health effects started to be acknowledged by the scientific community [2,3,4]. This led to restrictions and gradual phasing-out of specific analogues, e.g., perfluorooctanoic acid (PFOA) and perfluorooctane sulfonate (PFOS) [5,6].

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