Multimycotoxin Analysis by LC-MS/MS in Cereal Food and Feed: Comparison of Different Approaches for Extraction, Purification, and Calibration

Abstract

Twelve different approaches commonly used forthe simultaneous LC tandem MS (MS/MS)determination of mycotoxins (deoxynivalenol,aflatoxins, ochratoxin A, T-2 and HT-2 toxins,fumonisins, and zearalenone) were tested in cerealsand feed materials. They comprised differentextraction solvents, types of cleanup [solid-phaseextraction, QuEChERS, and immunoaffinity (IMA)],and calibration approaches (external or matrixmatched).The percentage of mycotoxins withacceptable recovery, according to Regulation (EC)No. 401/2006, ranged from 9 to 100%. The approachgiving the highest percentage of acceptable resultswas selected and further tested for corn, rice, andfeed spiked at three different mycotoxin levels (low,medium, and high). The method is based onextraction with MeOH-water (70 + 30, v/v) andcleanup with two multiantibody IMA columns. Forcorn and rice spiked at low mycotoxin levels, asignificant matrix effect was observed and wascompensated by using 13C calibration. At highermycotoxin levels (medium and high), matrix effectswere negligible as no significant differences wereobserved for the majority of recovery resultscalculated by 13C calibration and external calibration.Although the proposed method still needsimprovement in terms of accuracy and, to a lesserextent, precision, it was successfully tested with fourproficiency tests in buckwheat, corn, rice, and feed,giving acceptable z-scores for 97% (34 out of 35) ofresults.


Tutti gli autori

  • M. Solfrizzo; L. Gambacorta; R. Bibi; M. Ciriaci ; A. Paoloni; I. Pecorelli

Titolo volume/Rivista

Journal of AOAC International


Anno di pubblicazione

2017

ISSN

1944-7922

ISBN

Non Disponibile


Numero di citazioni Wos

Nessuna citazione

Ultimo Aggiornamento Citazioni

Non Disponibile


Numero di citazioni Scopus

Non Disponibile

Ultimo Aggiornamento Citazioni

Non Disponibile


Settori ERC

Non Disponibile

Codici ASJC

Non Disponibile