Article

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

MOE Key Laboratory of Pollution Processes and Environmental Criteria, Nankai University, Tianjin 300071, China.
Journal of Chromatography A (Impact Factor: 4.61). 07/2010; 1217(31):5026-34. DOI: 10.1016/j.chroma.2010.05.061
Source: PubMed

ABSTRACT 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.

0 Bookmarks
 · 
110 Views
  • [Show abstract] [Hide abstract]
    ABSTRACT: The occurrence and levels of perfluoroalkyl acids (PFAAs) emitted from specific pollution sources into the aquatic environment in Switzerland were studied using digested sewage sludges from 45 wastewater treatment plants in catchments containing a wide range of potential industrial emitters. Concentrations of individual PFAAs show a high spatial and temporal variability, which infers different contributions from industrial technologies and activities. Perfluorooctane sulfonic acid (PFOS) was generally the predominant PFAA with concentrations varying between 4 and 2440μgkg(-1) (median 75μgkg(-1)). Elevated emissions were especially observed in catchments capturing discharges from metal plating industries (median 82μgkg(-1)), aqueous firefighting foams (median 215μgkg(-1)) and landfill leachates (median 107μgkg(-1)). Some elevated perfluoroalkyl carboxylic acids (PFCAs) levels could be attributed to emissions from textile finishing industries with concentrations up to 233μgkg(-1) in sewage sludge. Assuming sorption to sludge for PFOS and PFCAs of 15% and 2%, respectively, concentrations in wastewater effluents up to the low μgL(-1) level were estimated. Even if wastewater may be expected to be diluted between 10 and 100 times by the receiving waters, elevated concentrations may be reached at specific locations. Although sewage sludge is a minor compartment for PFAAs in WWTPs, these investigations are helpful for the identification of hot-spots from industrial emitters as well as to estimate monthly average concentrations in wastewater.
    Chemosphere 08/2014; DOI:10.1016/j.chemosphere.2014.07.045 · 3.50 Impact Factor
  • [Show abstract] [Hide abstract]
    ABSTRACT: An analytical method for the simultaneous determination in fish liver and muscle tissue and mussel samples of 14 perfluorinated compounds (PFCs) including three perfluoroalkylsulfonates (PFSAs), seven perfluorocarboxylic acids (PFCAs), three perfluorophosphonic acids (PFPAs) and perfluorooctanesulfonamide (PFOSA), and 10 potential precursors, including four polyfluoroalkyl phosphates (PAPs), four fluorotelomer saturated acids (FTCAs) and two fluorotelomer unsaturated acids (FTUCAs), was developed in the present work. Different clean-up strategies by means of solid-phase extraction (SPE) using mix-mode weak anion exchanger (WAX), reverse phase Envi-Carb or a combination of them was optimized and evaluated for the clean-up of focused ultrasonic solid-liquid (FUSLE) extracts before the analysis by liquid chromatography-triple quadrupole tandem mass spectrometry (LC-MS/MS). Mix-mode WAX coupled in-line to Envi-Carb was finally selected since it rendered the cleanest extracts and minimum matrix effect. The FUSLE-SPE-LC-MS/MS methodology was validated in terms of recovery, precision and method detection limits (MDLs). Apparent recovery values in the 65-116%, 59-119% and 67-126% range and MDLs in the 0.1-2.7 ng/g, 0.1-3.8 ng/g and 0.2-3.1 ng/g range were obtained for liver, mussel and fish muscle tissue samples, respectively. The method developed was applied to the analysis of grey mullet liver (Chelon labrosus) and mussel (Mytilus galloprovincialis) samples from the Basque Coast (North of Spain) and Yellowfin tuna muscle tissue (Thunnus albacares) samples from the Indian Ocean. To the best of our knowledge this is the first method that describes the simultaneous determination of 14 PFCs and 10 potential precursors in fish liver, fish muscle tissue and mussel samples. Besides, this is the first time that 8:2 monosubstituted polyfluorodecyl phosphate (8:2 monoPAP) and 8:2 disubstituted polyfluorodecyl phosphate (8:2 diPAP) were detected in mussel and tuna samples.
    Journal of Chromatography A 02/2015; 1387. DOI:10.1016/j.chroma.2015.01.089 · 4.26 Impact Factor
  • [Show abstract] [Hide abstract]
    ABSTRACT: Biotransformation of polyfluoroalkyl precursors contributes in part to the perfluoroalkyl carboxylates and sulfonates detected in the global environment and biota. Robust sample preparation and sensitive analytical techniques for maximum analyte recovery are essential to identify and to quantify biotransformation products often present at low levels in environmental matrices and experimental systems. This critical review covers current sample-preparation and analytical methods, including extraction, concentration, clean-up and derivatization, mass spectrometry coupled to gas or liquid chromatography, and radioisotope labeling and tracking techniques. We also critically review methodologies for molecular structural elucidation and in-silico prediction of potential transformation products. We describe current knowledge gaps and challenges in studying novel alternative polyfluoroalkyl substances. We discuss future trends on utilizing advanced analytical techniques.
    TrAC Trends in Analytical Chemistry 01/2015; DOI:10.1016/j.trac.2014.11.017 · 6.61 Impact Factor

Full-text (2 Sources)

Download
30 Downloads
Available from
May 22, 2014