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Development of multi-residue extraction procedures using QuEChERS and liquid chromatography tandem mass spectrometry for the determination of different types of organic pollutants in mussel

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Abstract

This study aimed to develop multi-residue methods for the extraction of organic pollutants in mussels (Mytilus galloprovincialis), including 11 pharmaceuticals, 5 pesticides, 5 perfluoroalkyl substances (PFASs) and 2 illicit drugs. The combination of 4 different QuEChERS methods and 12 clean-ups (a total of 44 combinations) was tested. QuEChERS included acidified (AQ), non-acidified (SQ) and their miniaturized versions. The clean-ups included 6 different conventional dispersive solid phase extraction (dSPE) plus 2 enhanced matrix removal (EMR-Lipid) and 4 SPE procedures (including sorbents focused on phospholipid removal and polymer-based). After sample analysis via HPLC-MS/MS, the three methods that provided the best results were validated in terms of linearity, accuracy, precision, sensitivity and matrix effect. The methods selected were the combination of (i) SQ and EMR-Lipid, (ii) AQ and Z-sep+ bulk-based dSPE and (iii) AQ and graphitized carbon black (GCB)-based dSPE. Recoveries at two concentration levels (50 and 500 ng/g) ranged 54–124%, 59–124% and 60–127%, respectively, and limits of quantification (LOQs) were < 30 ng/g for most analytes using any of the methods. The three methods were tested in non-spiked mussel samples purchased in local markets, but organic pollutants were not detected in any sample. However, the methods probed to successfully extract a wide range of organic pollutants families in mussel samples from the market and from bioaccumulation trials.

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Acknowledgements

We thank the mass spectrometry section of the Central Services of Support to the Experimental Research (SCSIE) of the Universitat de València for providing us access to QTRAP 6500 (Applied Biosciences), and to Dr. Sales Galletero for her help. We also thank Phenomenex® and especially Noemi Fillol for providing the SPE cartridges employed for the extraction procedures.

Funding

The research that led to these results received funding from the Spanish Ministry of Science, Innovation and Universities and the ERDF (European Regional Development Fund) through the project WETANDPAC (RTI2018-097158-B-C31) and from the Generalitat Valenciana through the project ANTROPOCEN@ (PROMETEO/2018/155). R. Álvarez-Ruiz acknowledges the Spanish Ministry of Science, Innovation and Universities and the ERDF for his FPI grant BES-2016-078612.

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Authors and Affiliations

  1. Environmental and Food Safety Research Group (SAMA-UV), Desertification Research Centre (CIDE), Universitat de València-CSIC-GV, Moncada-Naquera Road km 4.5, 46113, Moncada, Valencia, Spain

    Rodrigo Álvarez-Ruiz, Yolanda Picó, Daniele Sadutto & Julián Campo

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  1. Rodrigo Álvarez-Ruiz
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  2. Yolanda Picó
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  3. Daniele Sadutto
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  4. Julián Campo
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Contributions

Conceptualization: Rodrigo Álvarez-Ruiz, Yolanda Picó; methodology: Rodrigo Álvarez-Ruiz, Daniele Sadutto; formal analysis and investigation: Rodrigo Álvarez-Ruiz, Daniele Sadutto; writing—original draft preparation: Rodrigo Álvarez-Ruiz, Julián Campo; writing—review and editing: Yolanda Picó, Julián Campo, Rodrigo Álvarez-Ruiz, Daniele Sadutto; funding acquisition: Yolanda Picó; resources: Yolanda Picó; supervision: Julián Campo.

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Correspondence to Rodrigo Álvarez-Ruiz.

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Local supermarkets from the city of Valencia, Spain.

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Álvarez-Ruiz, R., Picó, Y., Sadutto, D. et al. Development of multi-residue extraction procedures using QuEChERS and liquid chromatography tandem mass spectrometry for the determination of different types of organic pollutants in mussel. Anal Bioanal Chem 413, 4063–4076 (2021). https://doi.org/10.1007/s00216-021-03363-y

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