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Article Abstract

Contaminant analysis in biota extracts can be hampered by matrix interferences caused by, for example, co-extracted lipids that compromise the quality of the analytical data and require frequent maintenance of the analytical instruments. In the present study, using gas chromatography coupled to high resolution mass spectrometry (GC-HRMS), we aimed to develop and validate a straightforward, robust, and reproducible cleanup method with acceptable recoveries for diverse compound classes with a wide range of physicochemical properties representative of pollutant screening in biota extracts. We compared Oasis PRiME HLB cartridges, Agilent Captiva EMR-Lipid cartridges, and "Freeze-Out" with salmon lipids spiked with 113 target chemicals. The EMR-Lipid cartridges provided extracts with low matrix effects at reproducible recoveries of the multi-class target analytes (93 ± 9% and 95 ± 7% for low and high lipid amounts, respectively). The EMR-Lipid cartridges were further tested with spiked pork lipids submitted to total extraction or silicone-based passive sampling. Reproducible recoveries were achieved and matrix residuals were largely removed as demonstrated gravimetrically for both types of extracts. Ion suppression of halogenated compounds was not as efficiently removed by the cleanup of total and silicone-based extracts of pork lipids as for the salmon lipids. However, the samples with clean up provided better instrument robustness than those without cleanup. Hence, EMR-Lipid cartridges were shown to be efficient as a cleanup method in multi-class monitoring of biota samples and open up new possibilities as a suitable cleanup method for silicone extracts in biota passive sampling studies using GC-HRMS analysis. Environ Toxicol Chem 2021;40:2693-2704. © 2021 The Authors. Environmental Toxicology and Chemistry published by Wiley Periodicals LLC on behalf of SETAC.

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http://dx.doi.org/10.1002/etc.5153DOI Listing

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Article Synopsis
  • Biota samples are essential for tracking chemical stressors in ecosystems and understanding dietary chemical exposure but require careful extraction and clean-up to protect sensitive analytical instrumentation.
  • The study tested four different clean-up methods (GPC, EMR, HSO, and PDMS) to effectively remove lipids from hen egg extracts before conducting non-targeted analysis (NTA).
  • Results showed that the sulphuric acid degradation (HSO) method had the least matrix effects, while gel permeation chromatography (GPC) and Captiva EMR-lipid cartridge (EMR) offered good recoveries, highlighting the importance of method selection in sample preparation.
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