Determination of Acrylamide in Coffee, Cereals, Baby Food, Cocoa, Dry Petfood, Potato Products, Vegetable Crisps, Biscuit, 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 matrices, limit of quantification, recovery and precision were as defined per SMPR 2022.06.

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 labelled internal standard.

RESULTS: A total of 16 laboratory samples from 9 matrix categories were included in the validation process. A full validation was conducted in 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 biscuit (cookie), with accuracy values determined within a 94-107% range.

CONCLUSION: The performances of the presented method are in agreement with the acceptance criteria stipulated in SMPR 2022.06.

HIGHLIGHTS: The Expert Review Panel for acrylamide approved the present method as AOAC Official First Action 2023.01.