An analytical method was developed and validated for the analysis of four priority perfluoroalkyl substances (PFAS), namely, perfluorooctanoic acid (PFOA), perfluorononanoic acid (PFNA), perfluorohexanesulfonic acid (PFHxS), and perfluorooctanesulfonate (PFOS) in food products using nanoscale liquid chromatography (nano-LC) coupled with nanoscale electrospray ionization (nano-ESI) and Orbitrap mass spectrometry (Orbitrap-MS) detection. The efficiency of two different nano-LC setups for chromatographic separation of selected PFAS was evaluated. The optimal LC separation of analytes was achieved using a reversed phase C18 (RP-C18) nano bore column with an integrated emitter. The effect of matrix concentration factor on signal suppression/enhancement was evaluated for different matrices. The method validation indicated analyte recoveries in the range 83–118% and within-laboratory reproducibility from 7 to 18%, while reanalysis of the materials from proficiency tests (PTs) showed that the accuracy of the obtained concentrations ranged from 85 to 124% of the provided consensus values. The method limits of quantification (m-LOQs) were set as first validation levels ranging from 0.001 to 0.3 ng g⁻¹ sample depending on the type of the food group. The observed method performance characteristics met the criteria stated in Commission Regulation (EU) 2022/1428, Commission Recommendation (EU) 2022/1431, as well as Guidance Document on Analytical Parameters for the Determination of Per- and Polyfluoroalkyl Substances (PFAS) in Food and Feed with regards to the compliance testing of PFAS maximum levels (MLs) and monitoring purposes. The elaborated method was applied for the analysis of selected priority PFAS in different food groups collected from the Latvian retail market.

开发并验证了一种分析方法，用于使用纳米级液体分析食品中的四种优先全氟烷基物质 (PFAS)，即全氟辛酸 (PFOA)、全氟壬酸 (PFNA)、全氟己烷磺酸 (PFHxS) 和全氟辛烷磺酸 (PFOS)色谱法 (nano-LC) 与纳米级电喷雾电离 (nano-ESI) 和 Orbitrap 质谱 (Orbitrap-MS) 检测相结合。评估了两种不同的纳流液相色谱装置对所选 PFAS 进行色谱分离的效率。使用带有集成发射器的反相 C18 (RP-C18) 纳米孔色谱柱实现了分析物的最佳 LC 分离。针对不同的基质评估了基质浓度因子对信号抑制/增强的影响。方法验证表明分析物回收率在 83-118% 范围内，实验室内重现性在 7% 到 18% 之间，而对能力验证 (PT) 材料的重新分析表明，所获得浓度的准确度在 85% 到 124% 之间提供的共识值。方法定量限 (m-LOQ) 设置为 0.001 至 0.3 ng g 的第一个验证水平^{−1 个}样本，具体取决于食物组的类型。观察到的方法性能特征符合委员会条例 (EU) 2022/1428、委员会建议 (EU) 2022/1431 以及食品中全氟和多氟烷基物质 (PFAS) 测定分析参数指导文件中规定的标准和饲料关于 PFAS 最高水平 (ML) 的合规性测试和监测目的。该详细方法用于分析从拉脱维亚零售市场收集的不同食品组中选定的优先 PFAS。