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

Anal Bioanal Chem. 2015 May;407(12):3489-97. doi: 10.1007/s00216-015-8541-5. Epub 2015 Feb 24.

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.

Publication types

  • Research Support, Non-U.S. Gov't

MeSH terms

  • Automation
  • Chromatography, High Pressure Liquid / instrumentation
  • Chromatography, High Pressure Liquid / methods*
  • Chromatography, Liquid
  • Equipment Design
  • Food Analysis / methods*
  • Hydrazines / chemistry
  • Plant Oils / analysis*
  • Plant Oils / chemistry
  • Reproducibility of Results
  • Solid Phase Extraction / instrumentation
  • Solid Phase Extraction / methods*
  • Tandem Mass Spectrometry / methods
  • Zearalenone / analysis*

Substances

  • Hydrazines
  • Plant Oils
  • hydrazine
  • Zearalenone