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.

Aude Bebius, Frédérique Reding, Viviane Theurillat, Leloup Valérie, Erik Konings, Thierry Delatour, Aurélien Desmarchelier
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Abstract

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.

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在单一实验室验证采用 LC-MS/MS 法测定咖啡、谷物、婴儿食品、可可、干宠物食品、马铃薯制品、蔬菜脆片、饼干、茶叶、坚果和香料中的丙烯酰胺:第一次行动 2023.01。
背景:丙烯酰胺(AA)是淀粉类食物在高温烹饪过程中自然形成的一种加工污染物。考虑到 AA 分析中固有的定量错误风险,AOAC 提出需要制定一个共识标准来测定各种食品中的 AA:目标:在一项实验室研究中验证了用于测定食品中 AA 的定量 LC-MS/MS 方法。目标基质、定量限、回收率和精密度等方面的性能要求均按照 SMPR 2022.06 的规定进行:拟议的方法源自 EN 16618:2015 标准,但在以下方面做了修改:(1) 样品制备(简化,可能实现自动化);(2) 适用范围(大幅扩展);(3) LC 条件(提高选择性)。AA 的确认检测采用 LC-MS/MS 的选择反应监测模式 (SRM),并使用 2,3,3-d3-acrylamide (d3-AA) 或 13C3-2,3,3-d3-acrylamide (13C3-d3-AA) 作为标记内标进行同位素稀释定量:共有来自 9 个基质类别的 16 个实验室样品参与了验证过程。在咖啡(速溶咖啡、烘焙咖啡)、婴儿谷物、可可粉、宠物食品(炸丸子)、茶(绿茶)、香料(黑胡椒)和坚果(烤杏仁)中进行了全面验证,回收率(97-108%)和精密度(RSDr 和 RSDiR < 12%)均令人满意。通过分析质量控制材料和参考材料,包括薯条、薯片、蔬菜脆片、速溶咖啡、婴儿食品和饼干(曲奇),进一步证明了该方法的适用性,准确度值在 94-107% 的范围内:结论:该方法的性能符合 SMPR 2022.06.Highlights 中规定的验收标准:丙烯酰胺专家评审小组批准本方法为 AOAC 官方首次行动 2023.01。
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