MOE Key Laboratory of Pollution Processes and Environmental Criteria, Nankai University, Tianjin 300071, China.
J Chromatogr A. 2010 Jul 30;1217(31):5026-34. doi: 10.1016/j.chroma.2010.05.061. Epub 2010 Jun 4.
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 (10-300ng/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 30ng/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.
建立了一种基于离子对萃取、Envicarb 小柱净化和液相色谱-串联质谱（LC-MS/MS）检测的快速、可靠的分析方法，用于测定消化污泥中 17 种全氟和多氟化合物（PFCs）。分别选择 Envicarb 小柱和 6 种标记内标用于消除/减少基质效应和校正基质效应。结果表明，对于碳链长度为 C6 至 C14 的全氟辛烷磺酰胺（FOSAs）和全氟羧酸（PFCAs）的基质效应降低到-14%至+28%的范围。然而，由于缺乏合适的内标，其他分析物的基质效应仍然很大。基于基质加标，在不同加标水平（10-300ng/g）下，目标分析物的平均回收率在 70%-169%之间。不同加标水平的相对标准偏差（RSDs）在 2%-20%之间。定量限（LOQ）范围为 0.6-30ng/g。该方法成功应用于瑞士苏黎世附近几家污水处理厂的几个污泥样品中。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，进一步证明了离子对萃取法可用于污泥样品中 PFCs 的分析。据我们所知，这是首次采用离子对法提取污水污泥中的 PFCs，并首次在污水污泥中发现不饱和氟调聚物羧酸（FTUCAs）。
