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Determination of perfluorinated compounds in fish fillet homogenates: Method validation and application to fillet homogenates from the Mississippi River

We report herein a simple protein precipitation extraction-liquid chromatography tandem mass spectrometry (LC/MS/MS) method, validation, and application for the analysis of perfluorinated carboxylic acids (C7–C12), perfluorinated sulfonic acids (C4, C6, and C8), and perfluorooctane sulfonamide (FOSA...

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Published in:Analytica chimica acta 2011-01, Vol.683 (2), p.248-257
Main Authors: Malinsky, Michelle Duval, Jacoby, Cliffton B., Reagen, William K.
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cited_by cdi_FETCH-LOGICAL-c438t-7d149ab966546f15b5a19c19c7b6645425c8a0b0e6f0217f6cc6e2560d36dc833
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description We report herein a simple protein precipitation extraction-liquid chromatography tandem mass spectrometry (LC/MS/MS) method, validation, and application for the analysis of perfluorinated carboxylic acids (C7–C12), perfluorinated sulfonic acids (C4, C6, and C8), and perfluorooctane sulfonamide (FOSA) in fish fillet tissue. The method combines a rapid homogenization and protein precipitation tissue extraction procedure using stable-isotope internal standard (IS) calibration. Method validation in bluegill ( Lepomis macrochirus) fillet tissue evaluated the following: (1) method accuracy and precision in both extracted matrix-matched calibration and solvent (unextracted) calibration, (2) quantitation of mixed branched and linear isomers of perfluorooctanoate (PFOA) and perfluorooctanesulfonate (PFOS) with linear isomer calibration, (3) quantitation of low level (ppb) perfluorinated compounds (PFCs) in the presence of high level (ppm) PFOS, and (4) specificity from matrix interferences. Both calibration techniques produced method accuracy of at least 100 ± 13% with a precision (%RSD) ≤18% for all target analytes. Method accuracy and precision results for fillet samples from nine different fish species taken from the Mississippi River in 2008 and 2009 are also presented.
doi_str_mv 10.1016/j.aca.2010.10.028
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The method combines a rapid homogenization and protein precipitation tissue extraction procedure using stable-isotope internal standard (IS) calibration. Method validation in bluegill ( Lepomis macrochirus) fillet tissue evaluated the following: (1) method accuracy and precision in both extracted matrix-matched calibration and solvent (unextracted) calibration, (2) quantitation of mixed branched and linear isomers of perfluorooctanoate (PFOA) and perfluorooctanesulfonate (PFOS) with linear isomer calibration, (3) quantitation of low level (ppb) perfluorinated compounds (PFCs) in the presence of high level (ppm) PFOS, and (4) specificity from matrix interferences. Both calibration techniques produced method accuracy of at least 100 ± 13% with a precision (%RSD) ≤18% for all target analytes. Method accuracy and precision results for fillet samples from nine different fish species taken from the Mississippi River in 2008 and 2009 are also presented.</abstract><cop>Amsterdam</cop><pub>Elsevier B.V</pub><pmid>21167978</pmid><doi>10.1016/j.aca.2010.10.028</doi><tpages>10</tpages></addata></record>
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ispartof Analytica chimica acta, 2011-01, Vol.683 (2), p.248-257
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subjects accuracy
Analytical chemistry
Animals
Calibration
Caprylates - analysis
Caprylates - standards
carboxylic acids
chemical analysis
chemical precipitation
Chemistry
Chromatographic methods and physical methods associated with chromatography
Chromatography, High Pressure Liquid - methods
Chromatography, High Pressure Liquid - standards
Exact sciences and technology
filleting
Fillets
Fish
fish fillets
Fish tissues
Fluorocarbons - analysis
Fluorocarbons - standards
food analysis
food contamination
Freshwater
high performance liquid chromatography
homogenization
Homogenizing
Hydrocarbons, Fluorinated - analysis
Hydrocarbons, Fluorinated - standards
Isomerism
Isomers
Lepomis macrochirus
Liquid chromatography–tandem mass spectrometry (LC/MS/MS)
Matrix-matched calibration
Method validation
Mississippi
Other chromatographic methods
Perciformes
Perfluorinated compounds
perfluorocarbons
Perfluorooctanesulfonate
Perfluorooctanoic acid
PFOA
PFOS
pollutants
Precipitation
precision
Proteins
quantitative analysis
Rivers
solid phase extraction
Spectrometric and optical methods
stable isotopes
Sulfonamides - analysis
Sulfonamides - standards
sulfonic acid
tandem mass spectrometry
Tandem Mass Spectrometry - methods
Tandem Mass Spectrometry - standards
Water Pollutants, Chemical - analysis
Water Pollutants, Chemical - standards
water pollution
title Determination of perfluorinated compounds in fish fillet homogenates: Method validation and application to fillet homogenates from the Mississippi River
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