French National Research Institute for Agriculture, Food and Environment (INRAE), MASS Group, UR QuaPA, Saint-Genès-Champanelle, France.
French National Research Institute for Agriculture, Food and Environment (INRAE), MASS Group, UR QuaPA, Saint-Genès-Champanelle, France.
Food Res Int. 2024 Sep;191:114614. doi: 10.1016/j.foodres.2024.114614. Epub 2024 Jun 13.
The aim of the present study was to assess the performance and complementarity of methods capable of both quantifying furan, 2-Methylfuran (2-MF) and 3-Methylfuran (3-MF) in infant foods, but also to comprehensively explore other furan derivatives. It is more particularly a question of validating and comparing the couplings of the two headspace extraction methods most used for the analysis of furan compounds - Headspace Solid Phase Microextraction (HS-SPME) and Static HeadSpace (SHS) - with gas chromatography hyphenated to a high-resolution mass detector (Q Exactive-Orbitrap MS) which allows both targeted quantification and suspect screening. Firstly, the accuracy profile approach was implemented to assess, validate and compare HS-SPME- and SHS-GC-Q Exactive-Orbitrap MS for the quantification of furan in two model infant foods, apple puree and first infant formula. SHS-GC-Q Exactive-Orbitrap MS, showed better accuracy (uncertainty < 17.2 % vs 22.5 % for HS-SPME GC-Q Exactive-Orbitrap MS) and better sensitivity (LOQ < 2.8 vs LOQ < 4.0 µg/kg) over a broader validation range (2-100 µg/kg vs 5-100 µg/kg in apple puree). Secondly, SHS-GC-Q Exactive-Orbitrap MS was assessed and validated by accuracy profile for the quantification of 2-MF and 3-MF, with performance close to those for furan except for 3-MF in apple puree. Thirdly, SHS-GC-Q Exactive-Orbitrap MS was used to quantify the levels of these compounds in 20 commercial samples (n = 3) belonging to the four main categories of infant food (infant formulae, fruit purees, infant cereals, vegetable/fish baby meals). Furan was quantified in 75 % of the samples, with maximum levels in the vegetable/fish-based infant foods (up to 127 µg/kg) while 2-MF and 3-MF were quantified in 45 % and 15 % of products respectively, with maximum levels of 14.1 µg/kg in follow-on formula 3 age and 9.2 µg/kg in apple puree. Finally, SHS- and HS-SPME-GC-Q Exactive-Orbitrap MS data of the 20 infant products were processed in suspect screening mode using Compound Discoverer software. Coupling with HS-SPME, it made it possible to identify 13 additional furan derivatives, i.e. 5 more than with SHS. The relevance and safety status of the compounds identified are discussed.
本研究的目的是评估能够定量测定婴儿食品中呋喃、2-甲基呋喃（2-MF）和 3-甲基呋喃（3-MF）的方法的性能和互补性，但也要全面探索其他呋喃衍生物。更具体地说，这是一个验证和比较两种最常用于分析呋喃化合物的顶空萃取方法的问题 - 顶空固相微萃取（HS-SPME）和静态顶空（SHS） - 与气相色谱联用高分辨率质量检测器（Q Exactive-Orbitrap MS），可同时进行靶向定量和可疑筛选。首先，实施准确度概况方法来评估、验证和比较 HS-SPME 和 SHS-GC-Q Exactive-Orbitrap MS 对两种模型婴儿食品（苹果泥和第一婴儿配方奶粉）中呋喃的定量。SHS-GC-Q Exactive-Orbitrap MS 显示出更好的准确度（不确定度 < 17.2% 比 HS-SPME-GC-Q Exactive-Orbitrap MS 的 22.5%）和更好的灵敏度（LOQ < 2.8 比 LOQ < 4.0 µg/kg），并且在更宽的验证范围内（2-100 µg/kg 比苹果泥中的 5-100 µg/kg）。其次，通过准确度概况评估和验证 SHS-GC-Q Exactive-Orbitrap MS 对 2-MF 和 3-MF 的定量，性能除了苹果泥中的 3-MF 外，与呋喃相似。第三，SHS-GC-Q Exactive-Orbitrap MS 用于定量分析 20 种商业样品（n = 3）中这些化合物的水平，这些样品属于婴儿食品的四个主要类别（婴儿配方奶粉、水果泥、婴儿谷物、蔬菜/鱼婴儿餐）。在 75%的样品中定量了呋喃，在基于蔬菜/鱼的婴儿食品中达到最高水平（高达 127 µg/kg），而 2-MF 和 3-MF 分别在 45%和 15%的产品中定量，最高水平分别为 14.1 µg/kg 继配方 3 年龄和 9.2 µg/kg 在苹果泥中。最后，使用 Compound Discoverer 软件以可疑筛选模式处理 20 种婴儿产品的 SHS 和 HS-SPME-GC-Q Exactive-Orbitrap MS 数据。与 HS-SPME 耦合，它可以鉴定出 13 种额外的呋喃衍生物，即比 SHS 多 5 种。讨论了鉴定化合物的相关性和安全性状况。
