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采用高效液相色谱-串联质谱法测定食品和食品接触材料中全氟和多氟烷基物质的灵敏方法。

A sensitive method for the determination of per- and polyfluoroalkyl substances in food and food contact material using high-performance liquid chromatography coupled with tandem mass spectrometry.

机构信息

Chemical and Veterinary Analytical Institute Münsterland-Emscher-Lippe, Joseph-König-Str. 40, 48147 Münster, Germany; Institute of Food Chemistry, University of Münster, Corrensstr. 45, 48149 Münster, Germany.

Chemical and Veterinary Analytical Institute Münsterland-Emscher-Lippe, Joseph-König-Str. 40, 48147 Münster, Germany.

出版信息

J Chromatogr A. 2024 Aug 16;1730:465041. doi: 10.1016/j.chroma.2024.465041. Epub 2024 Jun 6.

Abstract

Dietary intake is the major pathway of human exposure to per- and polyfluoroalkyl substances (PFAS). Due to their generally very low concentrations in food, especially for foods of plant origin, and their toxicological relevance, demand is growing for improved selective and sensitive analytical methods for the determination of PFAS in the lower ng/kg range. The relevance is pointed out due to the fact that the European Commission has published limits of quantification (LOQs) in the lower ng/kg range for different food matrices in Recommendation (EU) 2022/1431 on the monitoring of perfluoroalkyl substances in food. For example, LOQs of 2 ng/kg for perfluorooctanesulfonic acid (PFOS), 1 ng/kg for perfluorooctanoic acid (PFOA), 1 ng/kg for perfluorononanoic acid (PFNA) and 4 ng/kg for perfluorohexanesulfonic acid (PFHxS) in fruit, vegetables and baby foods are required. A new, very sensitive method is presented here for the determination of 22 PFAS in food and food contact materials. The method is based on liquid-solid extraction and automated clean-up using two solid phase extraction techniques. The analytes are separated and detected by HPLC-MS/MS. A limit of detection (LOD) of 0.33 ng/kg and an LOQ of 1.0 ng/kg are attained for plant foods such as fruits and vegetables as well as for milk and baby food. For foods of animal origin such as egg, meat, fish and paper-based food contact materials an LOD of 1.6 ng/kg as well as an LOQ of 5.0 ng/kg are attained. PFOS and PFOA were the most abundant compounds in the food samples with concentration as high as 1,051 ng/kg of PFOA in sea weed samples and 772 ng/kg of PFOS in eggs samples. In food contact material samples, higher levels were found with a maximum of 310,000 ng/kg PFHxA. In sum the presented method firstly allows determination of PFAS in a wide variety of foodstuffs and paper-based food contact materials at EU-required concentration ranges.

摘要

饮食摄入是人类接触全氟和多氟烷基物质 (PFAS) 的主要途径。由于这些物质在食物中的浓度通常非常低,尤其是对于植物性食物,并且具有毒理学相关性,因此对于能够选择性和灵敏地检测 PFAS 的分析方法的需求日益增长,检测下限要求达到 ng/kg 级。这一点很重要,因为欧盟委员会在关于食品中全氟烷基物质监测的 (EU) 2022/1431 号建议中规定了不同食品基质中 PFAS 的定量限 (LOQ) 在 ng/kg 级。例如,水果、蔬菜和婴儿食品中需要检测到的全氟辛烷磺酸 (PFOS)、全氟辛酸 (PFOA)、全氟壬酸 (PFNA) 和全氟己烷磺酸 (PFHxS) 的 LOQ 分别为 2ng/kg、1ng/kg、1ng/kg 和 4ng/kg。本文提出了一种新的、非常灵敏的方法,用于测定食品和食品接触材料中的 22 种 PFAS。该方法基于液-固萃取和两种固相萃取技术的自动净化。采用高效液相色谱-串联质谱法对分析物进行分离和检测。对于水果和蔬菜等植物性食品以及牛奶和婴儿食品,可达到 0.33ng/kg 的检测限 (LOD) 和 1.0ng/kg 的定量限 (LOQ)。对于鸡蛋、肉类、鱼类和纸基食品接触材料等动物源性食品,可达到 1.6ng/kg 的 LOD 和 5.0ng/kg 的 LOQ。在食品样品中,PFOS 和 PFOA 是最丰富的化合物,海藻样品中 PFOA 的浓度高达 1051ng/kg,鸡蛋样品中 PFOS 的浓度高达 772ng/kg。在食品接触材料样品中,发现了更高的浓度,最大值为 310000ng/kg 的 PFHxA。总之,该方法首次允许在欧盟要求的浓度范围内检测各种食品和纸基食品接触材料中的 PFAS。

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