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超高效液相色谱-三重四极杆质谱法同时检测植物油中21种全氟及多氟烷基化合物OA北大核心CSTPCDMEDLINE

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

中文摘要英文摘要

食用植物油是人们生活中重要的膳食组成,其质量安全关系到消费者健康.全氟及多氟烷基化合物(PFASs)可通过原料、加工过程、包装材料等多种途径污染植物油.因此建立植物油中PFASs的高灵敏、高准确分析方法对保障植物油质量安全至关重要.本研究建立了乙腈提取-固相萃取净化-超高效液相色谱-串联质谱法(UHPLC-MS/MS)同时检测植物油中全氟烷基羧酸、全氟烷基磺酸及多氟调聚磺酸三类21种PFASs的分析方法.实验对色谱分离条件、质谱检测参数进行优化,并考察了提取溶剂、固相萃取净化填料等样品前处理条件对样品回收率和净化效果的影响.确定植物油样品经乙腈直接提取,采用弱阴离子WAX SPE柱净化后,通过C18反相色谱柱进行分离;质谱检测器在电喷雾负离子模式下,采用多反应监测(MRM)模式进行检测,通过特征离子对及保留时间定性,采用内标法定量.结果表明,21种目标分析物在其相应的范围内线性关系良好,相关系数均≥0.995;方法的检出限和定量限分别为0.004~0.015 μg/kg和0.015~0.050 μg/kg,方法回收率为95.6%~115.8%,相对标准偏差为0.3%~10.9%(n=9).本方法前处理操作简便,分析速度快,灵敏度高,抗干扰性强,稳定性高,适用于多种植物油中全氟烷基羧酸、全氟烷基磺酸及多氟调聚磺酸的快速检测分析.

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 accu-rate 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 purifi-cation 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 systemat-ically 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 ob-served 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 im-munity to interferences,and good stability,rendering it suitable for the rapid analysis and accu-rate determination of typical PFASs in edible plant oils.

冯灏;张炜;何保山;李盼盼;高树青;郭宝元;杨永坛

河南工业大学粮油食品学院,河南郑州 450001国家粮食和物资储备局科学研究院,北京 100037河南工业大学粮油食品学院,河南郑州 450001||国家粮食和物资储备局科学研究院,北京 100037

化学

超高效液相色谱-三重四极杆质谱固相萃取全氟及多氟烷基化合物植物油

ultra-high performance liquid chromatography-triple quadrupole mass spectrometry(UHPLC-MS/MS)solid phase extraction(SPE)perfluorinated and polyfluoroalkyl sub-stances(PFASs)plant oil

《色谱》 2024 (008)

731-739 / 9

中央级公益性基本科研业务费专项资金项目(ZX2241).Fundamental Research Funds of Nonprofit Central Institutes(No.ZX2241).

10.3724/SP.J.1123.2024.01014

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