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超高效液相色谱-三重四极杆质谱法同时测定植物油中21种全氟和多氟烷基物质

[Simultaneous determination of 21 perfluorinated and polyfluoroalkyl substances in plant oils by ultra-high performance liquid chromatography-triple quadrupole mass spectrometry].

作者信息

Feng Hao, Zhang Wei, He Bao-Shan, Li Pan-Pan, Gao Shu-Qing, Guo Bao-Yuan, Yang Yong-Tan

机构信息

College of Food Science and Technology, Henan University of Technology, Zhengzhou 450001, China.

Academy of National Food and Strategic Reserves Administration, Beijing 100037, China.

出版信息

Se Pu. 2024 Aug;42(8):731-739. doi: 10.3724/SP.J.1123.2024.01014.

Abstract

Edible plant oils are a key component of the daily human diet, and the quality and safety of plant oils are related to human health. Perfluorinated and polyfluoroalkyl substances (PFASs) are pollutants that can contaminate plant oil through the processing of raw materials or exposure to materials containing these substances. Thus, establishing a sensitive and accurate analytical method for the determination of PFASs is critical for ensuring the safety of plant oils. In this study, a method based on acetonitrile extraction and solid phase extraction purification combined with ultra-high performance liquid chromatography-triple quadrupole mass spectrometry (UHPLC-MS/MS) was developed for the simultaneous determination of 21 PFASs, including perfluorocarboxylic acids, perfluoroalkyl sulfonic acids, and fluorotelomer sulfonic acids, in edible plant oils. The chromatographic conditions and MS parameters were optimized, and the influences of the extraction solvents and purification method were systematically studied. Plant oil samples were directly extracted with acetonitrile and purified using a weak anion-exchange (WAX) column. The 21 target PFASs were separated on a reversed-phase C18 chromatographic column and detected using a triple quadrupole mass spectrometer with an electrospray ionization source. The mass spectrometer was operated in negative-ion mode. The target compounds were analyzed in multiple reaction monitoring (MRM) mode and quantified using an internal standard method. The results demonstrated that the severe interference observed during the detection of PFASs in the co-extracted substances was completely eliminated after the extraction mixture was purified using a WAX column. The 21 target PFASs showed good linearity in their corresponding ranges, with correlation coefficients greater than 0.995. The limits of detection (LODs) and limits of quantification (LOQs) of the method were in the range of 0.004-0.015 and 0.015-0.050 μg/kg, respectively. The recoveries ranged from 95.6% to 115.8%, with relative standard deviations (RSDs) in the range of 0.3%-10.9% (=9). The established method is characterized by simple sample pretreatment, good sensitivity, high immunity to interferences, and good stability, rendering it suitable for the rapid analysis and accurate determination of typical PFASs in edible plant oils.

摘要

食用植物油是人类日常饮食的关键组成部分,植物油的质量和安全与人类健康相关。全氟和多氟烷基物质(PFASs)是一类污染物,可通过原材料加工或接触含此类物质的材料污染植物油。因此,建立一种灵敏、准确的PFASs分析方法对于确保植物油安全至关重要。本研究建立了一种基于乙腈萃取和固相萃取净化,结合超高效液相色谱-三重四极杆质谱(UHPLC-MS/MS)的方法,用于同时测定食用植物油中21种PFASs,包括全氟羧酸、全氟烷基磺酸和氟调聚物磺酸。优化了色谱条件和质谱参数,并系统研究了萃取溶剂和净化方法的影响。植物油样品直接用乙腈萃取,并用弱阴离子交换(WAX)柱净化。21种目标PFASs在反相C18色谱柱上分离,采用电喷雾电离源的三重四极杆质谱仪进行检测。质谱仪在负离子模式下运行。目标化合物采用多反应监测(MRM)模式分析,内标法定量。结果表明,萃取混合物经WAX柱净化后,共萃取物中PFASs检测时观察到的严重干扰被完全消除。21种目标PFASs在相应范围内呈现良好的线性,相关系数大于0.995。该方法的检出限(LODs)和定量限(LOQs)分别在0.004-0.015和0.015-0.050 μg/kg范围内。回收率在95.6%至115.8%之间,相对标准偏差(RSDs)在0.3%-10.9%(n=9)范围内。所建立的方法具有样品前处理简单、灵敏度高、抗干扰能力强、稳定性好等特点,适用于食用植物油中典型PFASs的快速分析和准确测定。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/6872/11292476/a11795d7cebd/cjc-42-08-731-img_1.jpg

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