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J Chromatogr A. 2014 Feb 28;1331:27-37. doi: 10.1016/j.chroma.2014.01.025. Epub 2014 Jan 22.

Focused ultrasound solid-liquid extraction for the determination of perfluorinated compounds in fish, vegetables and amended soil.

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Department of Analytical Chemistry, Faculty of Science and Technology, University of the Basque Country (UPV/EHU), P.O. Box 644, 48080 Bilbao, Spain.
Department of Analytical Chemistry, Faculty of Science and Technology, University of the Basque Country (UPV/EHU), P.O. Box 644, 48080 Bilbao, Spain. Electronic address:


In the present work a method was developed for the determination of different perfluorinated compounds (PFCs), including three perfluorinated sulfonic acids (PFSAs), seven perfluorocarboxylic acids (PFCAs), three perfluorophosphonic acids (PFPAs) and perfluorooctanesulfonamide (PFOSA) in fish, vegetables and amended soil samples based on focused ultrasound solid-liquid extraction (FUSLE) followed by solid-phase extraction (SPE) clean-up and liquid chromatography-tandem mass spectrometry (LC-MS/MS). Different variables affecting the chromatographic separation (column type and pH of the mobile phase), the electrospray ionization (capillary voltage, nebulizer pressure and drying gas flow) and mass spectrometric detection (fragmentor voltage and collision energy) were optimized in order to improve the sensitivity of the separation and detection steps. In the case of FUSLE variables such as the solvent type, the solvent volume, the extraction temperature, the sonication and extraction time and the percentage of applied irradiation power were studied. Under optimized conditions, sonication of 2.5min with pulse times on of 0.8s and pulse times off of 0.2s in 7mL of (9:1) acetonitrile (ACN): water mixture in duplicate guaranteed exhaustive extraction of the matrices analyzed. Due to the non-selective extraction using FUSLE, different SPE cartridges (200-mg Waters Oasis-HLB, 150-mg Waters Oasis-WAX and 150-mg Waters Oasis-MAX) were tested in terms of extraction efficiency and matrix effect both in the extraction and detection steps. Mix mode SPE using Waters Oasis-WAX provided the best extraction efficiencies with the lowest matrix effect. The final method was validated in terms of recovery at two fortification levels (in the 80-120% for most of the analytes and matrices), precision (relative standard deviation in the 2-15% range) and method detection limits (MDLs, 0.3-12.4ng/g for vegetables, 0.2-12.5ng/g for fish and 1-22ng/g for amended soil). Finally the method was applied for the determination of the 14 PFCs in different vegetables and fish samples from a local supermarket and in a soil amended with a compost from a local wastewater treatment plant (WWTP).


Amended soil; Fish; Focused ultrasound solid–liquid extraction; Matrix effect; Perfluorinated compounds; Vegetables

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