Quantification of Chlorate and Perchlorate in a Broad Range of Food Commodities, Including Baby Food, Nutritional Formulas, and Ingredients by LC-MS/MS: First Action AOAC 2022.06.

BACKGROUND: Chlorate is an effective herbicide, but also a byproduct of chlorinating agents used to disinfect water, which is one of the reasons why it is regularly found in food. Perchlorate is a ubiquitous contaminant, which is naturally occurring in the environment but also released from anthropogenic sources such as the industrial use of certain natural fertilizers. Chlorate affects the hematological system, and perchlorate the thyroid. OBJECTIVE: Implement and validate a simple and robust analytical method for the accurate determination of chlorate and perchlorate in baby food, infant and adult formulas, and ingredients thereof, which is suited for its application in routine environments where a broad variety of food commodities must be analyzed simultaneously. METHOD: Typically, analytes are extracted with a mixture of water, acidified methanol, and dichloromethane. Optionally, for dairy products and byproducts, extraction can be performed with water, acidified methanol, and EDTA, followed by two steps of cleanup (freezing out and dispersive solid-phase extraction with C18 in acetonitrile). Quantitative determination is carried out by isotopic dilution liquid chromatography tandem mass spectrometry (LC-MS/MS). RESULTS: The method was single-laboratory validated in five Nestlé Quality Assurance Centers (NQACs) in a comprehensive range of representative matrixes of different categories such as baby foods, infant/adult formulas, and ingredients, with results generally in agreement with the acceptance criteria of the Standard Method Performance Requirement (SMPR®) 2021.001 defined by AOAC INTERNATIONAL, in terms of representative matrixes validated, LOQs, trueness, and precision.The data generated during validation show that the method proposed is simple, accurate and robust enough to be implemented and applied in routine environments. CONCLUSION: The data generated during validation show that the method proposed is simple, accurate and robust enough to be implemented and applied in routine environments. HIGHLIGHTS: The AOAC Expert Review Panel approved the present method as AOAC Official First Action 2022.06.

Levels of Alternaria Toxins in Selected Food Commodities Including Green Coffee.

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.

Application of a streamlined LC-MS/MS methodology for the determination of atropine and scopolamine in cereals from Asian and African countries.

Tropane alkaloids are toxic secondary metabolites produced by a wide variety of plants that can be present in edible materials or animal feed. Several human poisoning cases through consumption of cereals were reported over the last years and highlighted the need for reliable and robust analytical methodologies for safety control. To rationalize analyses in high-throughput laboratory environments dealing with shorter and shorter turn-around-around time, the scope of our multi mycotoxins method was extended to the analysis of two regulated tropane alkaloids, namely atropine and scopolamine. Extraction procedure is based on the QuEChERS (Quick, Easy, Cheap, Efficient, Rugged, and Safe) approach followed by liquid chromatography tandem mass spectrometry (LC-MS/MS) detection. Quantification is performed by the isotopic dilution approach using labelled isotopomers as internal standard. The procedure was validated at two fortification levels (0.5 µg/kg and 10 µg/kg) on different cereal-based products according to the European SANTE/12682/2019 document and performance parameters such as precision (RSD(r) ≤ 6%, RSD(iR) ≤ 6%) and recovery (82-114%) fulfilled its requirements. The limit of quantification (0.5 µg/kg) is low enough to ensure compliance with existing regulations. The method was further applied on 95 cereals and cereal-based products collected from Asian and African countries. All samples were found free of the two targeted TAs, with the exception of a rice-based product in which both atropine and scopolamine were quantified at 9.6 µg/kg and 2.6 µg/kg, respectively. A total of 29 cereals samples, shown to be free of both atropine and scopolamine were also analysed for mycotoxins. Aflatoxins, fumonisins, and deoxynivalenol were sporadically detected at levels below the maximum levels defined by the European Union legislation often considered as the most stringent regulation.

Determination of 2- and 3-MCPD as well as 2- and 3-MCPD Esters and Glycidyl Esters (GE) in Infant and Adult/Pediatric Nutritional Formula by Gas Chromatography Coupled to Mass Spectrometry Method, First Action 2018.03.

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.