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Simultaneous determination of 21 trace perfluoroalkyl substances in fish by isotope dilution ultrahigh performance liquid chromatography tandem mass spectrometry
Journal of Chromatography B ( IF 3 ) Pub Date : 2018-03-07 , DOI: 10.1016/j.jchromb.2018.03.008
Yan Gao , Xiaomin Li , Xiuqin Li , Qinghe Zhang , Hongmei Li

Perfluoroalkyl substances (PFASs) have been identified as emerging environmental contaminants. In this study, an efficient and accurate ultrahigh performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) method was developed for simultaneous determination of 21 PFASs in fish. Acetonitrile was used for sample extraction. Solid phase extraction (SPE) by WAX cartridges and then freezing at −30 °C were adopted as cleanup strategies. Strict measurements were performed to control background contamination during the whole procedure. Matrix effects were evaluated by external standard and isotope dilution mass spectrometry (IDMS) methods. IDMS can compensate the matrix effects to a large extent. The method detection limits (MDLs) ranged from 2 pg/g to 10 pg/g except for PFBA (120 pg/g). The method quantitation limits (MQLs) ranged from 5 pg/g to 30 pg/g except for PFBA (300 pg/g). The matrix spiked recoveries of three spiked levels were in the range of 79.6%–109%. The intra-day relative standard deviation (RSD) and inter-day RSD were from 0.94% to 13.9% and 0.36% to 11.2% respectively. Two fish tissue reference materials were analyzed by the developed method. The results of reference materials were within the uncertainty of the given value. The quantitative results of IDMS and standard addition (SA) - IDMS were comparable. The developed UHPLC-MS/MS method was applied for PFASs detection in 20 marine fish samples. 9 PFASs were detected in the samples with the ∑9PFASs concentration range of 0.04 to 2.14 ng/g wet weight (ww).



中文翻译:

同位素稀释超高效液相色谱串联质谱法同时测定鱼中21种微量全氟烷基物质

全氟烷基物质(PFAS)已被确定为新兴的环境污染物。在这项研究中,开发了一种高效,准确的超高效液相色谱串联质谱法(UHPLC-MS / MS),用于同时测定鱼类中的21种PFAS。乙腈用于样品提取。采用WAX柱进行固相萃取(SPE),然后在−30°C下冷冻作为净化策略。在整个过程中进行了严格的测量,以控制背景污染。基质效应通过外标和同位素稀释质谱法(IDMS)进行评估。IDMS可以在很大程度上补偿矩阵效应。除PFBA(120 pg / g)外,方法检测限(MDL)为2 pg / g至10 pg / g。除PFBA(300 pg / g)外,方法的定量限(MQL)为5 pg / g至30 pg / g。三种加标水平的加标基质回收率在79.6%–109%范围内。日内相对标准偏差(RSD)和日间RSD分别为0.94%至13.9%和0.36%至11.2%。通过开发的方法分析了两种鱼组织参考材料。参考物质的结果在给定值的不确定性范围内。IDMS和标准添加物(SA)-IDMS的定量结果具有可比性。所开发的UHPLC-MS / MS方法用于20种海水鱼类样品中PFAS的检测。带有∑的样品中检测到9种PFAS 日内相对标准偏差(RSD)和日间RSD分别为0.94%至13.9%和0.36%至11.2%。通过开发的方法分析了两种鱼组织参考材料。参考物质的结果在给定值的不确定性范围内。IDMS和标准添加物(SA)-IDMS的定量结果具有可比性。所开发的UHPLC-MS / MS方法用于20种海水鱼类样品中PFAS的检测。带有∑的样品中检测到9种PFAS 日内相对标准偏差(RSD)和日间RSD分别为0.94%至13.9%和0.36%至11.2%。通过开发的方法分析了两种鱼组织参考材料。参考物质的结果在给定值的不确定性范围内。IDMS和标准添加物(SA)-IDMS的定量结果具有可比性。所开发的UHPLC-MS / MS方法用于20种海水鱼类样品中PFAS的检测。带有∑的样品中检测到9种PFAS 所开发的UHPLC-MS / MS方法用于20种海水鱼类样品中PFAS的检测。带有∑的样品中检测到9种PFAS 所开发的UHPLC-MS / MS方法用于20种海水鱼类样品中PFAS的检测。带有∑的样品中检测到9种PFAS9种PFAS的湿重(ww)范围为0.04至2.14 ng / g。

更新日期:2018-03-07
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