Development and Validation of a QuEChERS-Based Liquid Chromatography Tandem Mass Spectrometry Multi-Method for the Determination of 38 Native and Modified Mycotoxins in Cereals

J Agric Food Chem. 2020 Apr 22;68(16):4657-4669. doi: 10.1021/acs.jafc.9b07491. Epub 2020 Apr 13.

Abstract

Here, a reliable and sensitive method for the determination of 38 (modified) mycotoxins was developed. Using a QuEChERS-based extraction method [acetonitrile/water/formic acid (75:20:5, v/v/v)], followed by two runs of high performance liquid chromatography tandem mass spectrometry with different conditions, relevant mycotoxins in cereals were analyzed. The method was validated according to the performance criteria defined by the European Commission (EC) in Commission Decision no. 657/2002. Limits of quantification ranged from 0.05 to 150 μg/kg. Good linearity (R2 > 0.99), recovery (61-120%), repeatability (RSDr < 15%), and reproducibility (RSDR < 20%) were obtained for most mycotoxins. However, validation results for Alternaria toxins and fumonisins were unsatisfying. Matrix effects (-69 to +59%) were compensated for using standard addition. Application on reference materials gave correct results while analysis of samples from local retailers revealed contamination, especially with deoxynivalenol, deoxynivalenol-3-glucoside, fumonisins, and zearalenone, in concentrations up to 369, 58, 1002, and 21 μg/kg, respectively.

Keywords: LC−MS/MS; QuEChERS; cereals; modified mycotoxins; multi-mycotoxin analysis; validation.

Publication types

  • Evaluation Study

MeSH terms

  • Chromatography, High Pressure Liquid / methods*
  • Edible Grain / chemistry*
  • Food Contamination / analysis
  • Limit of Detection
  • Mycotoxins / chemistry*
  • Mycotoxins / isolation & purification*
  • Tandem Mass Spectrometry / methods*

Substances

  • Mycotoxins