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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 |
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creator | Malinsky, Michelle Duval Jacoby, Cliffton B. Reagen, William K. |
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 |
format | article |
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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.</description><identifier>ISSN: 0003-2670</identifier><identifier>EISSN: 1873-4324</identifier><identifier>DOI: 10.1016/j.aca.2010.10.028</identifier><identifier>PMID: 21167978</identifier><identifier>CODEN: ACACAM</identifier><language>eng</language><publisher>Amsterdam: Elsevier B.V</publisher><subject>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</subject><ispartof>Analytica chimica acta, 2011-01, Vol.683 (2), p.248-257</ispartof><rights>2010 Elsevier B.V.</rights><rights>2015 INIST-CNRS</rights><rights>Copyright © 2010 Elsevier B.V. All rights reserved.</rights><lds50>peer_reviewed</lds50><woscitedreferencessubscribed>false</woscitedreferencessubscribed><citedby>FETCH-LOGICAL-c438t-7d149ab966546f15b5a19c19c7b6645425c8a0b0e6f0217f6cc6e2560d36dc833</citedby><cites>FETCH-LOGICAL-c438t-7d149ab966546f15b5a19c19c7b6645425c8a0b0e6f0217f6cc6e2560d36dc833</cites></display><links><openurl>$$Topenurl_article</openurl><openurlfulltext>$$Topenurlfull_article</openurlfulltext><thumbnail>$$Tsyndetics_thumb_exl</thumbnail><link.rule.ids>314,780,784,27924,27925</link.rule.ids><backlink>$$Uhttp://pascal-francis.inist.fr/vibad/index.php?action=getRecordDetail&idt=23725205$$DView record in Pascal Francis$$Hfree_for_read</backlink><backlink>$$Uhttps://www.ncbi.nlm.nih.gov/pubmed/21167978$$D View this record in MEDLINE/PubMed$$Hfree_for_read</backlink></links><search><creatorcontrib>Malinsky, Michelle Duval</creatorcontrib><creatorcontrib>Jacoby, Cliffton B.</creatorcontrib><creatorcontrib>Reagen, William K.</creatorcontrib><title>Determination of perfluorinated compounds in fish fillet homogenates: Method validation and application to fillet homogenates from the Mississippi River</title><title>Analytica chimica acta</title><addtitle>Anal Chim Acta</addtitle><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.</description><subject>accuracy</subject><subject>Analytical chemistry</subject><subject>Animals</subject><subject>Calibration</subject><subject>Caprylates - analysis</subject><subject>Caprylates - standards</subject><subject>carboxylic acids</subject><subject>chemical analysis</subject><subject>chemical precipitation</subject><subject>Chemistry</subject><subject>Chromatographic methods and physical methods associated with chromatography</subject><subject>Chromatography, High Pressure Liquid - methods</subject><subject>Chromatography, High Pressure Liquid - standards</subject><subject>Exact sciences and technology</subject><subject>filleting</subject><subject>Fillets</subject><subject>Fish</subject><subject>fish fillets</subject><subject>Fish tissues</subject><subject>Fluorocarbons - analysis</subject><subject>Fluorocarbons - standards</subject><subject>food analysis</subject><subject>food contamination</subject><subject>Freshwater</subject><subject>high performance liquid chromatography</subject><subject>homogenization</subject><subject>Homogenizing</subject><subject>Hydrocarbons, Fluorinated - analysis</subject><subject>Hydrocarbons, Fluorinated - standards</subject><subject>Isomerism</subject><subject>Isomers</subject><subject>Lepomis macrochirus</subject><subject>Liquid chromatography–tandem mass spectrometry (LC/MS/MS)</subject><subject>Matrix-matched calibration</subject><subject>Method validation</subject><subject>Mississippi</subject><subject>Other chromatographic methods</subject><subject>Perciformes</subject><subject>Perfluorinated compounds</subject><subject>perfluorocarbons</subject><subject>Perfluorooctanesulfonate</subject><subject>Perfluorooctanoic acid</subject><subject>PFOA</subject><subject>PFOS</subject><subject>pollutants</subject><subject>Precipitation</subject><subject>precision</subject><subject>Proteins</subject><subject>quantitative analysis</subject><subject>Rivers</subject><subject>solid phase extraction</subject><subject>Spectrometric and optical methods</subject><subject>stable isotopes</subject><subject>Sulfonamides - analysis</subject><subject>Sulfonamides - standards</subject><subject>sulfonic acid</subject><subject>tandem mass spectrometry</subject><subject>Tandem Mass Spectrometry - methods</subject><subject>Tandem Mass Spectrometry - standards</subject><subject>Water Pollutants, Chemical - analysis</subject><subject>Water Pollutants, Chemical - standards</subject><subject>water pollution</subject><issn>0003-2670</issn><issn>1873-4324</issn><fulltext>true</fulltext><rsrctype>article</rsrctype><creationdate>2011</creationdate><recordtype>article</recordtype><recordid>eNqNkU2LFDEQhoMo7rj6A7xoLuKpx3x0km49yfoJuwjqnkM6qexk6O70Jj0D_hN_rml71IuIUCRU8dRblbwIPaZkSwmVL_ZbY82WkZ_5lrDmDtrQRvGq5qy-izaEEF4xqcgZepDzvqSMkvo-OmOUStWqZoO-v4EZ0hBGM4c44ujxBMn3h5iWEjhs4zDFw-gyDiP2Ie_K0fcw410c4g0sUH6Jr2DeRYePpg9uVTKjw2aa-mDXfI5_acQ-xQHPO8BXIeclpingz-EI6SG6502f4dHpPkfX795-vfhQXX56__Hi9WVla97MlXK0bk3XSilq6anohKGtLaE6KWtRM2EbQzoC0pfHKy-tlcCEJI5LZxvOz9HzVXdK8fYAedZDyBb63owQD1k3gtdNS8l_kIyoRlEuCklX0qaYcwKvpxQGk75pSvTinN7r4pxenFtKxbnS8-SkfugGcL87fllVgGcnwGRrep_MaEP-w3HFBCPL8Kcr503U5iYV5vpLmSSK_Uo0vC3Eq5WA8q_HAElnG2C04EICO2sXwz8W_QF03cG-</recordid><startdate>20110110</startdate><enddate>20110110</enddate><creator>Malinsky, Michelle Duval</creator><creator>Jacoby, Cliffton B.</creator><creator>Reagen, William K.</creator><general>Elsevier B.V</general><general>Elsevier</general><scope>FBQ</scope><scope>IQODW</scope><scope>CGR</scope><scope>CUY</scope><scope>CVF</scope><scope>ECM</scope><scope>EIF</scope><scope>NPM</scope><scope>AAYXX</scope><scope>CITATION</scope><scope>7X8</scope><scope>7U5</scope><scope>8FD</scope><scope>L7M</scope></search><sort><creationdate>20110110</creationdate><title>Determination of perfluorinated compounds in fish fillet homogenates: Method validation and application to fillet homogenates from the Mississippi River</title><author>Malinsky, Michelle Duval ; Jacoby, Cliffton B. ; Reagen, William K.</author></sort><facets><frbrtype>5</frbrtype><frbrgroupid>cdi_FETCH-LOGICAL-c438t-7d149ab966546f15b5a19c19c7b6645425c8a0b0e6f0217f6cc6e2560d36dc833</frbrgroupid><rsrctype>articles</rsrctype><prefilter>articles</prefilter><language>eng</language><creationdate>2011</creationdate><topic>accuracy</topic><topic>Analytical chemistry</topic><topic>Animals</topic><topic>Calibration</topic><topic>Caprylates - analysis</topic><topic>Caprylates - standards</topic><topic>carboxylic acids</topic><topic>chemical analysis</topic><topic>chemical precipitation</topic><topic>Chemistry</topic><topic>Chromatographic methods and physical methods associated with chromatography</topic><topic>Chromatography, High Pressure Liquid - methods</topic><topic>Chromatography, High Pressure Liquid - standards</topic><topic>Exact sciences and technology</topic><topic>filleting</topic><topic>Fillets</topic><topic>Fish</topic><topic>fish fillets</topic><topic>Fish tissues</topic><topic>Fluorocarbons - analysis</topic><topic>Fluorocarbons - standards</topic><topic>food analysis</topic><topic>food contamination</topic><topic>Freshwater</topic><topic>high performance liquid chromatography</topic><topic>homogenization</topic><topic>Homogenizing</topic><topic>Hydrocarbons, Fluorinated - analysis</topic><topic>Hydrocarbons, Fluorinated - standards</topic><topic>Isomerism</topic><topic>Isomers</topic><topic>Lepomis macrochirus</topic><topic>Liquid chromatography–tandem mass spectrometry (LC/MS/MS)</topic><topic>Matrix-matched calibration</topic><topic>Method validation</topic><topic>Mississippi</topic><topic>Other chromatographic methods</topic><topic>Perciformes</topic><topic>Perfluorinated compounds</topic><topic>perfluorocarbons</topic><topic>Perfluorooctanesulfonate</topic><topic>Perfluorooctanoic acid</topic><topic>PFOA</topic><topic>PFOS</topic><topic>pollutants</topic><topic>Precipitation</topic><topic>precision</topic><topic>Proteins</topic><topic>quantitative analysis</topic><topic>Rivers</topic><topic>solid phase extraction</topic><topic>Spectrometric and optical methods</topic><topic>stable isotopes</topic><topic>Sulfonamides - analysis</topic><topic>Sulfonamides - standards</topic><topic>sulfonic acid</topic><topic>tandem mass spectrometry</topic><topic>Tandem Mass Spectrometry - methods</topic><topic>Tandem Mass Spectrometry - standards</topic><topic>Water Pollutants, Chemical - analysis</topic><topic>Water Pollutants, Chemical - standards</topic><topic>water pollution</topic><toplevel>peer_reviewed</toplevel><toplevel>online_resources</toplevel><creatorcontrib>Malinsky, Michelle Duval</creatorcontrib><creatorcontrib>Jacoby, Cliffton B.</creatorcontrib><creatorcontrib>Reagen, William K.</creatorcontrib><collection>AGRIS</collection><collection>Pascal-Francis</collection><collection>Medline</collection><collection>MEDLINE</collection><collection>MEDLINE (Ovid)</collection><collection>MEDLINE</collection><collection>MEDLINE</collection><collection>PubMed</collection><collection>CrossRef</collection><collection>MEDLINE - Academic</collection><collection>Solid State and Superconductivity Abstracts</collection><collection>Technology Research Database</collection><collection>Advanced Technologies Database with Aerospace</collection><jtitle>Analytica chimica acta</jtitle></facets><delivery><delcategory>Remote Search Resource</delcategory><fulltext>fulltext</fulltext></delivery><addata><au>Malinsky, Michelle Duval</au><au>Jacoby, Cliffton B.</au><au>Reagen, William K.</au><format>journal</format><genre>article</genre><ristype>JOUR</ristype><atitle>Determination of perfluorinated compounds in fish fillet homogenates: Method validation and application to fillet homogenates from the Mississippi River</atitle><jtitle>Analytica chimica acta</jtitle><addtitle>Anal Chim Acta</addtitle><date>2011-01-10</date><risdate>2011</risdate><volume>683</volume><issue>2</issue><spage>248</spage><epage>257</epage><pages>248-257</pages><issn>0003-2670</issn><eissn>1873-4324</eissn><coden>ACACAM</coden><abstract>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.</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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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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