Background: Monochloropropanediol (MCPD) and its fatty acid esters as well as glycidyl fatty acid esters are substances generated during oil refining or food processing. The free form released during digestion, 3-MCPD and glycidol, have shown adverse effects in animal studies. Objective: So far, the available analytical methods have not been validated in a collaborative study for infant and adult nutritional formulas. This manuscript describes a single-laboratory validation method in view of a future multilaboratory validation trial. Methods: The method described is for the direct determination of 2- and 3-MCPD and indirect determination of 2- and 3-MCPD esters and glycidyl esters in infant and adult/pediatric nutritional formulas by GC coupled to MS. Results: The analytical range was found to be 4–2000 μg/kg powder formula and 0.7–333 μg/kg liquid formula for fatty acid esters of MCPD and glycidol, and 2.5–750 μg/kg samples for free MCPD. The recovery rates were within 91–124% for all samples. Repeatability precision was <20% at levels close to the LOQ. Conclusions: The results met the Standard Method Performance Requirements® (SMPR) set by the AOAC Stakeholder Panel on Infant Formula and Adult Nutritionals. Highlights: The AOAC Expert Review Panel approved the present method as AOAC Official First Action 2018.03.

Alternaria toxins are emerging mycotoxins, candidates for regulation by European Authorities. Therefore, highly sensitive, confirmatory, and reliable analytical methodologies are required for their monitoring in food. In that context, an isotope dilution LC-MS/MS method was developed for the analysis of five Alternaria toxins (Altenuene, Alternariol, Alternariol monomethylether, Tentoxin, and Tenuazonic Acid) in a broad range of commodities including cereals and cereal-based products, tomato-based products, tree nuts, vegetable oils, dried fruits, cocoa, green coffee, spices, herbs, and tea. Validation data collected in two different laboratories demonstrated the robustness of the method. Underestimation of Tenuazonic Acid level in dry samples such as cereals was reported when inappropriate extraction solvent mixtures were used as currently done in several published methodologies. An investigation survey performed on 216 food items evidenced large variations of Alternaria toxins levels, in line with data reported in the last EFSA safety assessment. The analysis of 78 green coffee samples collected from 21 producing countries demonstrated that coffee is a negligible source of exposure to Alternaria toxins. Its wide scope of application, adequate sample throughput, and high sensitivity make this method fit for purpose for the regular monitoring of Alternaria toxins in foods.

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