Development and Interlaboratory Study of a Liquid Chromatography Tandem Mass Spectrometric Methodfor the Determination of Multiple Mycotoxins inCereals Using Stable Isotope Dilution

J AOAC Int. 2018 May 1;101(3):667-676. doi: 10.5740/jaoacint.17-0340. Epub 2017 Oct 5.


An efficient, rapid, accurate, and cost-effective method based on stable isotope dilution and LC tandem MS was developed for the determination of multimycotoxins in cereals. The samples were extracted using acetonitrile-water-acetic acid (70 + 29 + 1, v/v/v), followed by dilution and centrifugation without any further cleanup. The mycotoxins were separated on a C18 column. Interference due to matrix effects was efficiently compensated for with [13C]-labeled stable isotope internal standards. The method demonstrated excellent linear relations, with regression coefficients above 0.999. Spiked recoveries at three different concentrations ranged from 80.9 to 115.9%, and RSDs were below 14% for all mycotoxins. The trueness of the method was also verified by participating in two proficiency tests, and satisfactory z-scores (|z| < 1.1) were obtained. In addition, an international interlaboratory study was organized to evaluate the methods. Eight laboratories characterized recovery, repeatability, and reproducibility studies in wheat, maize, and barley. The interlaboratory results were analyzed according to ISO 5725-2. Cochran and Grubbs tests were used to remove outliers. The mean recoveries of all 16 mycotoxins ranged from 87 to 111%. Repeatability, reproducibility, and Horwitz ratio values were 3.5-16.2, 5.4-33.6, and 0.16-1.65%, respectively. The results demonstrate that the method is reliable to determine multimycotoxins in cereals.

Publication types

  • Editorial
  • Multicenter Study

MeSH terms

  • Carbon Isotopes
  • Chromatography, Liquid / methods*
  • Edible Grain / chemistry
  • Edible Grain / microbiology
  • Food Contamination / analysis*
  • Hordeum / chemistry
  • Hordeum / microbiology
  • Limit of Detection
  • Mycotoxins / analysis*
  • Mycotoxins / chemistry
  • Reproducibility of Results
  • Tandem Mass Spectrometry / methods*
  • Triticum / chemistry
  • Triticum / microbiology
  • Zea mays / chemistry
  • Zea mays / microbiology


  • Carbon Isotopes
  • Mycotoxins