Determination of Acrylamide in Coffee, Cereals, Baby Food, Cocoa, Dry Pet Food, Potato Products, Vegetable Crisps, Biscuits, Tea, Nuts, and Spices by LC-MS/MS in a Single-Laboratory Validation: First Action 2023.01.

BACKGROUND: Acrylamide (AA) is a process contaminant naturally formed during the cooking of starchy food at high temperatures. Considering existing risks of misquantification inherent to the analysis of AA, an AOAC initiative raised the need for a consensus standard to determine AA in a broad variety of food. OBJECTIVE: A quantitative LC-MS/MS method for AA determination in food was validated in a single-laboratory study. Targeted performance requirements in terms of target matrixes, limit of quantification, recovery, and precision were as defined per Standard Method Performance Requirement (SMPR®) 2022.006. METHOD: The proposed method derives from EN 16618:2015 standard pending modifications brought to the (1) sample preparation (simplified, potentially automated); (2) scope of application (significantly extended); and (3) LC conditions (improved selectivity). Confirmatory detection of AA is conducted by LC-MS/MS in the Selected Reaction Monitoring mode (SRM), and isotopic dilution was applied for quantification approach using either 2,3,3-d3-acrylamide (d3-AA), or 13C3-2,3,3-d3-acrylamide (13C3-d3-AA) as labeled internal standard. RESULTS: A total of 16 laboratory samples from nine matrix categories were included in the validation process. A full validation was conducted on coffee (instant, roast), infant cereal, cocoa powder, pet food (croquettes), tea (green tea), spices (black pepper), and nuts (roasted almonds) with satisfactory performances both in terms of recovery (97-108%) and precision (RSDr and RSDiR <12%). The method applicability was further demonstrated through the analysis of quality control materials and reference materials including French fries, potato crisps, vegetable crisps, instant coffee, infant food, and biscuits (cookies), with accuracy values determined within a 94-107% range. CONCLUSIONS: The performances of the presented method are in agreement with the acceptance criteria stipulated in SMPR 2022.006. HIGHLIGHTS: The Expert Review Panel for acrylamide approved the present method as AOAC Official First Action 2023.01.

Degradation of glyphosate along coffee roasting: Do residue levels in green beans mirror exposure derived from coffee consumption?

Robusta and Arabica green beans were supplemented with carbon 14-glyphosate labelled on each carbon position alternatively prior to roasting, up to 220 °C for Robusta and 200 °C for Arabica (2, 5 and 10 min). The results of the study point a significant decomposition of glyphosate that happens during roasting, from at least 42 % to > 74 % depending on roasting conditions (time, temperature) and coffee variety. The data obtained with 14C-labelled glyphosate materials suggest that the carboxymethyl branch of the compound degrades more effectively than the phosphonomethyl moiety. The degradation of glyphosate does not lead to the formation of aminomethylphosphonic acid (AMPA). The results of the study indicate that carbon dioxide, methylamine and dimethylamine are major degradation products of glyphosate formed along coffee roasting, likely released with the roasting gas. Ultimately, the results of the study show that levels of glyphosate in green beans do not mirror those in coffee beverages.

Traces of 2-phenylphenol in roasted coffee are not related to agrochemical residue in green coffee beans, but to generation during roasting.

Traces of the phytosanitary agent 2-phenylphenol in roasted coffee are not necessarily related to residues of agrochemicals. This study shows that roasting of coffee generates 2-phenylphenol at low level. Green coffee samples (approx. 1500) were found negative for 2-phenylphenol and the levels of 2-phenylphenol increased as a function of roasting degree. Packaging materials as a source of contamination can be excluded. The exposure to 2-phenylphenol by coffee consumption is negligible and contributes to less than 0.004% of the ADI. The presence of 2-phenylphenol residues in roasted coffee above the regulatory limits for green coffee must not necessarily lead to the conclusion that the green coffee, either conventional or organic, was non-compliant.

Furan and Methylfurans in Foods: An Update on Occurrence, Mitigation, and Risk Assessment.

The acceptance of many foods is related to traditional cooking practices, which create taste and texture and are important to digestibility, preservation, and the reduction of foodborne illnesses. A wide range of compounds are formed during the cooking of foods, a number of these have been shown to lead to adverse effects in classical toxicological models and are known as food processing contaminants (FPC). It is essential that the presence and effects of such compounds alone and in combination within the diet are understood such that proportionate risk management measures can be developed, while taking a holistic view across the whole value chain. Furan and alkylfurans (principally 2- and 3-methylfuran) are highly volatile FPC, which are formed in a wide range of foods at low amounts. The focus of research to-date has been on those foods, which have been identified to be most consequential in terms of being sources of exposure, namely jarred and canned foods for infants and young children (meals and drinks) and coffee (roast and ground, soluble). This report presents (i) new industry data on the occurrence of furan and methylfurans in selected food categories following previous coffee studies, (ii) the most salient parameters that impact furan formation, and (iii) aspects of importance for the risk assessment.

Mepiquat: A Process-Induced Byproduct in Roasted Cereal-Based Foodstuffs.

Mepiquat, a growth regulator widely used in agriculture, is also known as a process-induced byproduct formed in coffee from natural constituents during heat treatments such as roasting. This study examines mepiquat formation in cereal-based foodstuffs treated at sufficiently high temperature to trigger methyl transfer reactions that involve glycine betaine and choline naturally present in cereals. Color measurements of roasted barley grains revealed a correlation between thermal treatment and mepiquat content. Trials at industrial scale on instant beverages composed of roasted cereals demonstrated significant increases in mepiquat during the thermal process (in the range of 140-205 µg/kg in final products). A targeted survey of commercial products showed mepiquat in the range 69-381 µg/kg in powdered cereal instant drinks and 42-168 µg/kg in mugicha tea, a roasted barley infusion. These findings will not significantly affect the exposure of consumers to mepiquat due to the low amounts detected.

N,N-dimethylpiperidinium (mepiquat) Part 2. Formation in roasted coffee and barley during thermal processing.

Previous work in model systems has demonstrated that mepiquat can be formed under typical roasting conditions from the amino acid lysine via the Maillard reaction and trigonelline, the latter alkaloid serving as a methyl donor. This study shows for the first time that mepiquat is formed in low mg kg(-1) amounts during the coffee roasting process and consequently can be detected in roast and ground as well as soluble coffee up to levels of 1.4 mg kg(-1). Darker roast coffees contain relatively higher amounts of mepiquat versus light roasted beans, with an excellent correlation of mepiquat formation to roast colour (r(2) = 0.99) in robusta beans. A survey of 20 of the major green coffee origins (robusta and arabica coffees) showed the absence of mepiquat (<0.005 mg kg(-1)). Preliminary studies indicate that mepiquat is not formed during processing (thermal treatment) in most of the cereal-based foods such as pizza and ready-to-eat cereals, but was detected in barley after roasting (0.64 mg kg(-1)). Mepiquat can therefore be considered a process-induced compound formed from natural constituents during the roasting process. Even considering a high intake of seven cups per day of soluble coffee containing 1.4 mg kg(-1) mepiquat in the coffee powder (the highest amount measured in this study), the resulting intake would exhaust less than 0.2% of the ADI of mepiquat.