Abstract

An intercollaborative study was organized to evaluate the performance characteristics of a liquid chromatography tandem mass spectrometry procedure for the simultaneous determination of 12 mycotoxins in food, which were ochratoxin A, aflatoxins B1, B2, G1, G2, and M1, deoxynivalenol, zearalenone, fumonisins B1 and B2, and T-2 and HT-2 toxins. The method combined the simplicity of the QuEChERS (Quick, Easy, Cheap, Efficient, Rugged and Safe) approach with the efficiency of immunoaffinity column cleanup (the step used to enhance sensitivity and sample cleanup for some matrices only). Twenty-three entities were enrolled and were European reference laboratories for mycotoxin analysis, U.S. and European service laboratories, and Nestlé laboratories. Each participant analyzed 28 incurred and/or spiked blind samples composed of spices, nuts, milk powder, dried fruits, cereals, and baby food using the protocol given. Method performances were assessed according to ISO 5725-2. Relative standard deviations of repeatability and reproducibility and trueness values for each of the 115 mycotoxin/sample combinations ranged from 5% to 23%, 7% to 26%, and 85% to 129%, respectively, in line with requirements defined in EC 401/2006. The overall set of data gathered demonstrated that the method offered a unique platform to ensure compliance with EC 1881/2006 and EC 165/2013 regulations setting maximum limits for mycotoxins in food samples, even at low regulated levels for foods intended for infants and young children. The method was applicable regardless of the food, the regulated mycotoxin, and the concentration level, and thus is an excellent candidate for future standardization.

Highlights

  • Mycotoxins are a group of toxic chemical substances produced by filamentous fungi that commonly grow on a number of food commodities such as cereals, nuts, spices, fruits, oil seeds, or coffee.These toxins can be produced before harvest in the crop and even after harvest if climate conditions are favorable for further fungal growth

  • Key Contribution: Validation data gathered through this international collaborative study demonstrated that the analytical method proposed was suitable to ensure full compliance with regards to EC 1881/2006 and EC 165/2013 regulations, even at low regulated levels for foods intended for infants and young children

  • The procedure enables the quantitative LC-MS/MS determination of regulated mycotoxins (OTA, AFB1, AFB2, AFG1, AFG2, AFM1, DON, ZEN, FB1, FB2, and T-2 and HT-2 toxins) in a broad range of food items including cereals and cereal based baby foods, spices, nuts, coffee, tea, cocoa, vegetable oils, dried fruits, infant formula, dairy products, feed/pet food, etc. This routine method has the advantage of offering a unique platform to ensure full compliance with the EC 1881/2006 regulation [3], even at low regulated levels for foods intended for infants and young children

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Summary

Introduction

Mycotoxins are a group of toxic chemical substances produced by filamentous fungi (molds) that commonly grow on a number of food commodities such as cereals, nuts, spices, fruits, oil seeds, or coffee. These toxins can be produced before harvest in the crop and even after harvest if climate conditions are favorable for further fungal growth. The European Union legislation (often considered as the most stringent one) has established MLs for aflatoxins (AFLAs), ochratoxin A (OTA), zearalenone (ZEN), fumonisins (FBs), and deoxynivalenol (DON) (EC 1881:2006 [3]) and recently indicative levels for T-2 and HT-2 toxins (EC 165/2013 [4]) in a broad range of food commodities. Lower MLs have been established for food intended for infants and young children

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