Analysis of 36 mycotoxins in different agricultural and food/feed matrices using LC-MS/MS

In this report a multi-mycotoxin method, based on solid-liquid extraction (SLE} for analysis of 36 mycotoxins using Agilent 6460c UHPLC-MS/MS is described.

The 36 mycotoxins included were:

European Union (EU) regulated and related mycotoxins

• Aflatoxins (AFB1, AFB2, AFG1, AFG2)
  Deoxynivalenol (DON)
• Fumonisins (FB1, FB2, FB3, FB4)
• HT-2 toxin (HT-2)
• Ochratoxin A (OTA)
• T-2 toxin (T-2)
• Zearalenone (ZEN)

Emerging mycotoxins

• Beauvericin (BEA)
• Enniatins (ENNA, ENNA1, ENNB, ENNB1)
• Fusaric acid (FA)
• Moniliformin (MON)

Other mycotoxins

• 15-acetyl deoxynivalenol (15-ADON)
• 3-acetyl deoxinyvalenol (3-ADON)
• Deoxynivalenol-3-glucoside (D3G)
• Citrinin (CIT)
• Alternariol (AOH)
• Diacetoxyscirpenol (DAS)
• Ergosine (ES)
• Ergocryptine (ECR)
• Neosolaniol (NEO)
• Nivalenol (NIV)
• Patulin (PAT)
• Tenuazonic acid (TeA)
• Fusarenon-X (FX)
• Zearalanone (ZAN)
• α-zearalenol (α-ZEL)
• β-zearalenol (β-ZEL)

The method follows the dilute and shoot principle, in which samples are extracted with an organic solvent and the resulting extracts centrifuged.

To minimize matrix effects during electrospray ionization, the centrifuged extracts are combined with isotopically labelled internal standards (ISTDs) specific to each group of mycotoxins.

⇰ This addition is carried out directly in the autosampler needle, immediately before injection into the UHPLC-MS/MS system, ensuring accurate quantification.

The recoveries of 36 mycotoxins in spiked food, feed, and cereal matrices ranged from 67.4 % to 121.1 % after internal standard correction, with relative standard deviations (RSDs) below 14.9 %.