Department of Environmental Chemistry, IDAEA-CSIC c/Jordi Girona, 18-26, 08034 Barcelona, Spain.
J Chromatogr A. 2009 Oct 23;1216(43):7195-204. doi: 10.1016/j.chroma.2009.06.062. Epub 2009 Jun 25.
This paper describes the development and validation of an analytical methodology to determine eight perfluorinated compounds (PFCs) in edible fish using pressurized liquid extraction (PLE) with water and solid-phase extraction (SPE) with an ion-exchanger as extraction and pre-concentration procedures, followed by liquid chromatography-quadrupole-linear ion trap mass spectrometry (LC-QqLIT-MS). The rapidity and effectiveness of the proposed extraction procedure were compared with those most commonly used to isolate PFCs from fish (ion-pairing and alkaline digestion). The average recoveries of the different fish samples, spiked with the eight PFCs at three levels (the LOQ, 10 and 100 microg kg(-1) of each PFC), were always higher than 85% with relative standard deviation (RSD) lower than 17%. A good linearity was established for the eight PFCs in the range from 0.003-0.05 to 100 microg kg(-1), with r>0.9994. The limits of quantification (LOQs) were between 0.003 and 0.05 microg kg(-1), which are well below those previously reported for this type of samples. Compared with previous methods, sample preparation time and/or LOQs are reduced. The method demonstrated its successful application for the analysis of different parts of several fish species. Most of the samples tested positive, mainly for perfluoropentanoic acid (PFPA), perfluorobutane sulfonate (PFBS) and perfluorooctanoic acid (PFOA) but other of the eight studied PFCs were also present.
本文描述了一种使用加压液体萃取(PLE)水和离子交换固相萃取(SPE)作为提取和预浓缩程序,结合液相色谱-四极杆-线性离子阱质谱(LC-QqLIT-MS)来测定食用鱼中八种全氟化合物(PFCs)的分析方法的开发和验证。与最常用于从鱼类中分离 PFCs 的离子对和碱性消化方法相比,比较了所提出的提取方法的快速性和有效性。不同鱼类样品的平均回收率,用这八种 PFCs 在三个水平(每种 PFC 的 LOQ、10 和 100μgkg-1)进行加标,总是高于 85%,相对标准偏差(RSD)低于 17%。八种 PFCs 在 0.003-0.05 至 100μgkg-1 范围内建立了良好的线性关系,r>0.9994。定量限(LOQs)在 0.003 和 0.05μgkg-1 之间,远低于以前报道的此类样品的 LOQs。与以前的方法相比,样品制备时间和/或 LOQs 有所减少。该方法成功应用于分析几种鱼类不同部位的分析。测试的大多数样本呈阳性,主要是全氟戊酸(PFPA)、全氟丁烷磺酸(PFBS)和全氟辛酸(PFOA),但也存在其他八种研究的 PFCs。