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Comparison of two extraction methods for the analysis of per- and polyfluorinated chemicals in digested sewage sludge

机译:两种用于分析消化污泥中全氟和多氟化学品的提取方法的比较

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A rapid and reliable analytical method, based on ion-pair extraction, clean-up on Envicarb cartridge and detection by liquid chromatography-tandem mass spectrometry (LC-MS/MS), was developed for determination of 17 per- and polyfluorinated chemicals (PFCs) in digested sewage sludge. Envicarb cartridge and six labeled internal standards were selected for the elimination/reduction and correction of matrix effects, respectively. As a result, the matrix effect for perfluorooctane sulfonamides (FOSAs) and perfluorocarboxylic acids (PFCAs) with carbon chain length from C6 to C14 was lowered to a range of -14% to +28%. However, the matrix effect for other analytes was still great mainly due to the absence of appropriate internal standard. Mean recoveries of the target analytes based on matrix spikes, at different spike levels (10-300. ng/g), ranged from 70% to 169%. Relative standard deviations (RSDs) were in the range of 2-20% at different spike levels. The limit of quantification (LOQ) ranged between 0.6 and 30. ng/g. The method was successfully applied to several sewage sludge samples from wastewater treatment plants nearby Zürich, Switzerland. In addition, by comparing the accuracy and precision of ion-pair extraction method and methanol extraction method, we further demonstrated that the ion-pair extraction method can be used for the analysis of PFCs in sludge samples. To our knowledge, this is the first study to extract the PFCs in sewage sludge with ion-pair method and to find unsaturated fluorotelomer carboxylic acids (FTUCAs) in sewage sludge.
机译:建立了一种快速可靠的分析方法,该方法基于离子对萃取,Envicarb柱净化和液相色谱-串联质谱(LC-MS / MS)检测方法,用于测定17种全氟和多氟化学品(PFC) )中的消化污泥。选择了Envicarb滤芯和六种标记的内标,分别用于消除/减少和校正基质效应。结果,碳链长度为C6至C14的全氟辛烷磺酰胺(FOSA)和全氟羧酸(PFCA)的基质效应降低到-14%至+ 28%的范围。但是,其他分析物的基质效应仍然很大,这主要是由于缺乏适当的内标物。在不同的峰值水平(10-300 ng / g)下,基于基质峰值的目标分析物的平均回收率范围为70%至169%。在不同的尖峰水平下,相对标准偏差(RSD)在2-20%的范围内。定量极限(LOQ)在0.6到30. ng / g之间。该方法已成功应用于瑞士苏黎世附近污水处理厂的数个污水污泥样品。此外,通过比较离子对萃取法和甲醇萃取法的准确性和精密度,我们进一步证明了离子对萃取法可用于污泥样品中PFC的分析。据我们所知,这是首次采用离子对方法提取污泥中的PFC并在污泥中寻找不饱和氟调聚物羧酸(FTUCAs)的研究。

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