Removing Disturbing Matrix Constituents from Biota Extracts from Total Extraction and Silicone‐Based Passive Sampling

Abstract

Contaminant analysis in biota extracts can be hampered by matrix interferences caused by, e.g., co-extracted lipids that compromise the quality of the analytical data and require frequent maintenance of the analytical instruments. In this study 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 This article is protected by copyright. All rights reserved. Accepted Articlephysico-chemical properties representative of pollutant screening in biota extracts using gas chromatography coupled to high-resolution mass spectrometry (GC-HRMS). 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). 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 clean-up 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 without clean-up. Hence, EMR-Lipid cartridges were shown to be efficient as a clean-up method in multi-class monitoring of biota samples and open up new possibilities as a suitable clean-up method for silicone extracts in biota passive sampling studies using GC-HRMS.

Exploring the partitioning of hydrophobic organic compounds between water, suspended particulate matter and diverse fish species in a German river ecosystem

“…The extraction process was repeated once without the addition of new IS. The combined extract was reduced under a nitrogen stream, transferred to 1.5 mL acetonitrile and cleaned over 3 mL Captiva EMR-Lipid cartridges (Agilent Technologies, USA) [ 29 ]. The extracts were then blown down to ~5 µL and dissolved in 100 µL ethylacetate for chemical analysis.…”

Chemometers: an integrative tool for chemical assessment in multimedia environments

“…110 Besides those abandoned research lines, some challenges have been addressed and partially overcome: (i) the impact of co-dosed lipids in cell-based bioassays and (ii) background contamination of silicone mono-and oligomers in the chemometer extracts. Those obstacles have been overcome as follows: (i) the effect of the co-dosed lipids has been quantified and modeled in the bioassays, 123 and environmental concentrations can now be corrected for co-extracted lipids; (ii) the coextraction of silicone mono-and oligomers has been evaluated and discussed in Muz et al 4 and it can partially be solved applying the non-destructive cleanup protocol. In addition, using different solvents for extracting the chemicals from the chemometers could minimize the co-extraction of any polymeric matrix.…”

“…Following the sampling, the chemometer is retrieved from the sample, its surface is thoroughly cleaned, and the chemicals from the chemometer are extracted using a suitable solvent or mixture(s) of solvents. Depending on the medium that was sampled and the analytical requirements, a non-destructive 4 or destructive cleanup 5 can be used to remove matrix constituents and enhance the analytical result. However, in general, chemometer extracts require less cleanup compared to traditional exhaustive solvent extraction methods due to lower amounts of co-extracted matrix, such as lipids, which is one of the benefits of this approach.…”

Fatal aspergillosis and evidence of unrelated hearing loss in a harbor porpoise (Phocoena phocoena) from the German Baltic Sea

“…The extracts were then evaporated to dryness, and the residue was redissolved in ethyl acetate, containing 100 ng ml -1 of the following stable isotope-labeled internal standards: 13 C 12 -PCBs 28, 52,101,118,153,138,180 (Wellington Laboratories,Guelph,Ontario,Canada). The extracts were analyzed for PCB congeners 28/31, 52, 101, 118, 153, 138 and 180 by gas chromatography-high-resolution Orbitrap mass spectrometry [GC-HRMS QExactive, Thermo Fisher Scientific, Waltham, MA, United States, Muz et al (2021)], based on method-matched calibrations. The obtained data were processed, and the peak areas of the above-mentioned PCBs were integrated using the software TraceFinder V 5.1.…”