Multiple Mycotoxins Determination in Food by LC-MS/MS: An International Collaborative Study

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.

A Review: Sample Preparation and Chromatographic Technologies for Detection of Aflatoxins in Foods

“…When factoring in EU's regulatory levels of aflatoxin M 1 (0.025-0.05 ppb), more sensitivity is required if samples are diluted prior to LC-MS analysis. While such sensitivity is not possible for the majority of commercial LC-MS instruments, concentration and clean-up steps are necessary to ensure the detection of aflatoxin M 1 at and below the regulatory levels [258,259]. In-depth sample clean-up could be used to eliminate matrix-components/interferences but very often the process is lengthy and laborious.…”

Levels of Alternaria Toxins in Selected Food Commodities Including Green Coffee

“…Applicability of the QuEChERS (Quick, Easy, Cheap, Efficient, Rugged and Safe) approach for the analysis of Alternaria toxins was considered in parallel since already validated elsewhere [8,9,25]. This approach is faster, user friendly, cost efficient, and already used in many laboratories dealing with chemical contaminants analysis, e.g., mycotoxins, veterinary drugs, pesticides [26][27][28][29]. Our protocol encompasses an initial extraction of the analytes with a mixture of water, acetonitrile, and formic acid (50/50/0.1, v/v/v), followed by a liquid-liquid partition using salt mixtures.…”

“…Best results were obtained using Na2SO4/NaCl (4 g + 1 g) salts to induce liquid-liquid partition and hexane to remove co-extracted fat as a subsequent clean-up step. This clean-up procedure is extensively used for mycotoxins and tropane alkaloids analyses in Nestlé laboratories [26,28,32]. To reduce the strong matrix effects observed for ALT and AOH in some Historically, most methods for monitoring Alternaria toxins were devoted to the analysis of high-water content commodities such as tomatoes and tomato-based products and fruit juices [24,25,30,31].…”

The fate of mycotoxins during secondary food processing of maize for human consumption

“…Methods for mycotoxin analyses in research and routine applications are under continuous development. This concerns in particular the analysis of so far less studied mycotoxins, the simultaneous analysis of multiple mycotoxins including efficient detection of EU‐regulated mycotoxins, and the detection and quantification of mycotoxin degradation products, potentially toxic modified forms, and bound toxins in different feed and food matrices (see, e.g., Bertuzzi, Mulazzi, Rastelli, & Pietri, 2016; Bessaire, Mujahid, Mottier, & Desmarchelier, 2019; Rausch, Brockmeyer, & Schwerdtle, 2020; Stadler, Berthiller, Suman, Schuhmacher, & Krska, 2020; Tittlemier et al., 2020). In silico approaches can broaden the understanding of toxicological impacts (Dellafiora, Dall'Asta, & Galaverna, 2018).…”