色谱2024，Vol.42Issue(11)：1032-1041,10.DOI:10.3724/SP.J.1123.2024.02010
基于EMR-Lipid分散固相萃取-超高效液相色谱-串联质谱法同时测定牛肉中17种全氟烷基化合物
Simultaneous determination of 17 perfluoroalkyl substances in beef by EMR-Lipid dispersive solid-phase extraction a-nd ultra performance liquid chromatography-tandem mass spectrometry
摘要
Abstract
The ability to accurately analyze perfluoroalkyl substance(PFAS)levels in beef is imperative in order to effectively assess food-safety risks and ensure consumer safety because PFASs are harmful and prevalent in beef.In this study,we developed a rapid and accurate method for the simultaneously determination of the 17 PFASs in beef using dispersive solid-phase extraction(d-SPE)and ultra performance liquid chromatography-tandem mass spectrom-etry(UPLC-MS/MS),and optimized the mobile phase system,extraction solvent,and d-SPE materials.Samples were finally extracted using 0.1％(v/v)formic acid in acetonitrile,cleaned using d-SPE with PSA,C18,GCB,and EMR-Lipid,separated using an Acquity Premier BEH C18 column(100 mm×2.1 mm,1.7 μm)with 0.5 mmol/L ammonium fluoride aqueous solution and methanol as the mobile phases at a flow rate of 0.3 mL/min.Analytes were detected in negative ion switching mode(ESI-)with multiple reaction monitoring(MRM)scanning,and quantitatively analyzed using the internal standard method.The 17 PFASs exhibited linearity in the 0.2-20.0 μg/L range under the optimal experimental conditions,with correlation coeffi-cients of 0.991 5-0.999 9.The method delivered limits of detection(LODs)of 0.003-0.007μg/kg and limits of quantification(LOQs)of 0.01-0.02 μg/kg.The 17 PFASs exhibited recov-eries of 71.1％-127.4％with RSDs of 0.6％-14.4％when spiked at three levels(0.05,0.5,and 1.8 μg/kg).We optimized the mobile phase system,which revealed that,compared with 2.0,5.0,and 10.0 mmol/L ammonium formate or ammonium acetate in aqueous methanol,0.5 mmol/L ammonium fluoride in aqueous methanol exhibited higher sensitivities for all the 17 PFASs,with PFASs bearing long-chain carboxylic acids(C10-C18)showing 1-2 fold increases in sensitivity.PFASs do not dissociate in acidic environments,favoring their entry into the or-ganic phase.Therefore,we investigated the effect of extractant acidity,which revealed that the 17 PFASs were better extracted using 0.1％(v/v)formic acid in acetonitrile.The beef matrix has a complex composition;consequently,d-SPE adsorbents were required to purify samples and reduce matrix effects.The purification effects of four adsorbents(PSA,C18,GCB,and EMR-Lipid)toward the 17 PFASs and the amount of EMR-Lipid used were investigated,which revealed that 100 mg PSA+80 mg C18+40 mg GCB+150 mg EMR-Lipid exhibited superior matrix-purification behavior.We also investigated the effects of various injection solutions and types of syringe filter,with pure methanol selected for reconstitution and high-speed supernatant cen-trifugation applied prior to injection.The developed method is simple,rapid,sensitive,and re-producible,and can be used to simultaneously,rapidly,and accurately determine various per-fluoroalkyl compounds in beef.关键词
分散固相萃取/超高效液相色谱-串联质谱/全氟烷基化合物/牛肉Key words
dispersive solid-phase extraction(d-SPE)/ultra performance liquid chromatogra-phy-tandem mass spectrometry(UPLC-MS/MS)/perfluoroalkyl substances(PFASs)/beef分类
化学化工引用本文复制引用
邱巧丽,潘胜东,王立,方兰云,陈晓红,金米聪..基于EMR-Lipid分散固相萃取-超高效液相色谱-串联质谱法同时测定牛肉中17种全氟烷基化合物[J].色谱,2024,42(11):1032-1041,10.基金项目
浙江省基础公益研究计划(LTGC23B050002) （LTGC23B050002）
宁波市公益重点科技计划项目(2021S102,2022S091) （2021S102,2022S091）
宁波市医学重点学科建设项目(2022-B18).Basic Public Welfare Research Project of Zhejiang Province(No.LTGC23B050002) （2022-B18）
Ningbo Public Welfare Key Science and Technology Project(Nos.2021S102,2022S091) （Nos.2021S102,2022S091）
Project of Ningbo Leading Medical &Health Discipline(No.2022-B18). （No.2022-B18）
