[超高效液相色谱-三重四极杆质谱法同时测定植物油中的 21 种全氟和多氟烷基物质]。

Hao Feng, Wei Zhang, Bao-Shan He, Pan-Pan Li, Shu-Qing Gao, Bao-Yuan Guo, Yong-Tan Yang
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引用次数: 0

摘要

食用植物油是人类日常饮食的重要组成部分,植物油的质量和安全与人类健康息息相关。全氟和多氟烷基物质 (PFAS) 是一种污染物,可通过原材料加工或接触含有这些物质的材料而污染植物油。因此,建立一种灵敏、准确的 PFASs 分析方法对于确保植物油的安全性至关重要。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的全氟羧酸、全氟烷基磺酸和氟代磺酸等21种PFASs。优化了色谱条件和质谱参数,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,然后用弱阴离子交换(WAX)柱净化。21 种目标 PFAS 在反相 C18 色谱柱上分离,并使用带电喷雾离子源的三重四极杆质谱仪进行检测。质谱仪以负离子模式运行。目标化合物在多反应监测(MRM)模式下进行分析,并使用内标法进行定量。结果表明,在使用 WAX 色谱柱净化萃取混合物后,在检测共萃取物质中的全氟辛烷磺酸时观察到的严重干扰被完全消除。21 种目标全氟辛烷磺酸在相应的范围内表现出良好的线性关系,相关系数大于 0.995。该方法的检出限(LOD)和定量限(LOQ)分别为 0.004-0.015 和 0.015-0.050 μg/kg。回收率为95.6%~115.8%,相对标准偏差为0.3%~10.9%(n=9)。该方法样品前处理简单、灵敏度高、抗干扰能力强、稳定性好,适用于食用植物油中典型PFASs的快速准确测定。
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[Simultaneous determination of 21 perfluorinated and polyfluoroalkyl substances in plant oils by ultra-high performance liquid chromatography-triple quadrupole mass spectrometry].

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% (n=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.

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