Analytical and Bioanalytical Chemistry

, Volume 407, Issue 12, pp 3489–3497 | Cite as

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

  • Sarah S. Drzymala
  • Stefan Weiz
  • Julia Heinze
  • Silvia Marten
  • Carsten Prinz
  • Annett Zimathies
  • Leif-Alexander Garbe
  • Matthias KochEmail author
Research Paper


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.

Graphical Abstract

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


Dynamic covalent hydrazine chemistry (DCHC) Maize germ oil Food Mycotoxin 



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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Copyright information

© Springer-Verlag Berlin Heidelberg 2015

Authors and Affiliations

  • Sarah S. Drzymala
    • 1
  • Stefan Weiz
    • 2
  • Julia Heinze
    • 2
  • Silvia Marten
    • 2
  • Carsten Prinz
    • 1
  • Annett Zimathies
    • 1
  • Leif-Alexander Garbe
    • 3
  • Matthias Koch
    • 1
    Email author
  1. 1.Department 1 Analytical Chemistry, Reference MaterialsFederal Institute for Materials Research and Testing (BAM)BerlinGermany
  2. 2.KNAUER Wissenschaftliche Geräte GmbHBerlinGermany
  3. 3.Department of Biotechnology, Institute of BioanalyticsTechnische Universität BerlinBerlinGermany

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