LC-MS/MS 单实验室验证法测定咖啡、谷物、婴儿食品、可可、干宠物食品、土豆制品、蔬菜脆片、饼干、茶、坚果和香料中的丙烯酰胺：2023.01 年首次行动

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.

机构信息

Nestlé Research, Orbe, Route de Chavornay, 1350 Orbe, Switzerland.

Société des Produits Nestlé S.A., Nestlé Research, Vers-chez-les-Blancs, 1000 Lausanne 26, Switzerland.

出版信息

J AOAC Int. 2024 May 2;107(3):453-463. doi: 10.1093/jaoacint/qsae007.

DOI:10.1093/jaoacint/qsae007

PMID:38273660

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.

摘要

背景

丙烯酰胺（AA）是一种在高温下烹饪淀粉类食物时自然形成的过程污染物。考虑到 AA 分析中存在固有定量不准确的现有风险，AOAC 发起了一项倡议，要求制定一个共识标准，以确定各种食品中的 AA。

目的

在单实验室研究中验证了一种用于食品中 AA 测定的定量 LC-MS/MS 方法。根据标准方法性能要求（SMPR®）2022.006，针对目标基质、定量限、回收率和精密度等方面，定义了有针对性的性能要求。

方法

该方法源自 EN 16618：2015 标准，对（1）样品制备（简化，可能自动化）；（2）应用范围（显著扩展）；和（3）LC 条件（改进选择性）进行了修改。AA 的确认检测通过 LC-MS/MS 在选择反应监测模式（SRM）下进行，同位素稀释法用于使用 2,3,3-d3-丙烯酰胺（d3-AA）或 13C3-2,3,3-d3-丙烯酰胺（13C3-d3-AA）作为标记内标进行定量分析。

结果

共有来自九个基质类别的 16 个实验室样品纳入验证过程。对咖啡（速溶、烘焙）、婴儿谷物、可可粉、宠物食品（小馅饼）、茶（绿茶）、香料（黑胡椒）和坚果（烤杏仁）进行了全面验证，在回收率（97-108%）和精密度（RSDr 和 RSDiR<12%）方面均表现良好。通过对包括法式炸薯条、薯片、蔬菜薯片、速溶咖啡、婴儿食品和饼干（曲奇）在内的质控材料和参考材料的分析，进一步证明了该方法的适用性，准确度值在 94-107%范围内。