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Automated solid-phase extraction coupled online with HPLC-FLD for the quantification of zearalenone in edible oil

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Abstract

Established maximum levels for the mycotoxin zearalenone (ZEN) in edible oil require monitoring by reliable analytical methods. Therefore, an automated SPE-HPLC online system based on dynamic covalent hydrazine chemistry has been developed. The SPE step comprises a reversible hydrazone formation by ZEN and a hydrazine moiety covalently attached to a solid phase. Seven hydrazine materials with different properties regarding the resin backbone, pore size, particle size, specific surface area, and loading have been evaluated. As a result, a hydrazine-functionalized silica gel was chosen. The final automated online method was validated and applied to the analysis of three maize germ oil samples including a provisionally certified reference material. Important performance criteria for the recovery (70–120 %) and precision (RSDr <25 %) as set by the Commission Regulation EC 401/2006 were fulfilled: The mean recovery was 78 % and RSDr did not exceed 8 %. The results of the SPE-HPLC online method were further compared to results obtained by liquid–liquid extraction with stable isotope dilution analysis LC-MS/MS and found to be in good agreement. The developed SPE-HPLC online system with fluorescence detection allows a reliable, accurate, and sensitive quantification (limit of quantification, 30 μg/kg) of ZEN in edible oils while significantly reducing the workload. To our knowledge, this is the first report on an automated SPE-HPLC method based on a covalent SPE approach.

SPE-HPLC online method for automatic analysis of the mycotoxin zearalenone in edible oils.

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Acknowledgments

The authors would like to thank the ZIM program (Zentrales Innovationsprogramm Mittelstand) of the Federal Ministry for Economic Affairs and Energy for funding (no. KF2201035SB1).

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    Authors and Affiliations

    1. Department 1 Analytical Chemistry, Reference Materials, Federal Institute for Materials Research and Testing (BAM), Richard-Willstätter-Str. 11, 12489, Berlin, Germany

      Sarah S. Drzymala, Carsten Prinz, Annett Zimathies & Matthias Koch

    2. KNAUER Wissenschaftliche Geräte GmbH, Hegauer Weg 38, 14163, Berlin, Germany

      Stefan Weiz, Julia Heinze & Silvia Marten

    3. Department of Biotechnology, Institute of Bioanalytics, Technische Universität Berlin, 13353, Berlin, Germany

      Leif-Alexander Garbe

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    1. Sarah S. Drzymala
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    2. Stefan Weiz
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    Correspondence to Matthias Koch.

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    Sarah S. Drzymala and Stefan Weiz should be considered co-first authors.

    Sarah S. Drzymala and Stefan Weiz contributed equally to this work.

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    Drzymala, S.S., Weiz, S., Heinze, J. et al. Automated solid-phase extraction coupled online with HPLC-FLD for the quantification of zearalenone in edible oil. Anal Bioanal Chem 407, 3489–3497 (2015). https://doi.org/10.1007/s00216-015-8541-5

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    • DOI: https://doi.org/10.1007/s00216-015-8541-5

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