Validation of a fast and easy method for the determination of residues from 229 pesticides in fruits and vegetables using gas and liquid chromatography and mass spectrometric detection
Validation experiments were conducted of a simple, fast, and inexpensive method for the determination of 229 pesticides fortified at 10-100 ng/g in lettuce and orange matrixes. The method is known as the quick, easy, cheap, effective, rugged, and safe (QuEChERS) method for pesticide residues in food...
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| Veröffentlicht in: | Journal of AOAC International 2005-03, Vol.88 (2), p.595-614 |
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| creator | Lehotay, S.J Kok, A. de Hiemstra, M Bodegraven, P. van |
| description | Validation experiments were conducted of a simple, fast, and inexpensive method for the determination of 229 pesticides fortified at 10-100 ng/g in lettuce and orange matrixes. The method is known as the quick, easy, cheap, effective, rugged, and safe (QuEChERS) method for pesticide residues in foods. The procedure involved the extraction of a 15 g sample with 15 mL acetonitrile, followed by a liquid-liquid partitioning step performed by adding 6 g anhydrous MgSO4 plus 1.5 g NaCl. After centrifugation, the extract was decanted into a tube containing 300 mg primary secondary amine (PSA) sorbent plus 1.8 g anhydrous MgSO4, which constituted a cleanup procedure called dispersive solid-phase extraction (dispersive SPE). After a second shaking and centrifugation step, the acetonitrile extract was transferred to autosampler vials for concurrent analysis by gas chromatography/mass spectrometry with an ion trap instrument and liquid chromatography/tandem mass spectrometry with a triple quadrupole instrument using electrospray ionization. Each analytical method was designed to analyze 144 pesticides, with 59 targeted by both instruments. Recoveries for all but 11 of the analytes in at least one of the matrixes were between 70-120% (90-110% for 206 pesticides), and repeatabilities typically |
| doi_str_mv | 10.1093/jaoac/88.2.595 |
| format | Article |
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The method is known as the quick, easy, cheap, effective, rugged, and safe (QuEChERS) method for pesticide residues in foods. The procedure involved the extraction of a 15 g sample with 15 mL acetonitrile, followed by a liquid-liquid partitioning step performed by adding 6 g anhydrous MgSO4 plus 1.5 g NaCl. After centrifugation, the extract was decanted into a tube containing 300 mg primary secondary amine (PSA) sorbent plus 1.8 g anhydrous MgSO4, which constituted a cleanup procedure called dispersive solid-phase extraction (dispersive SPE). After a second shaking and centrifugation step, the acetonitrile extract was transferred to autosampler vials for concurrent analysis by gas chromatography/mass spectrometry with an ion trap instrument and liquid chromatography/tandem mass spectrometry with a triple quadrupole instrument using electrospray ionization. Each analytical method was designed to analyze 144 pesticides, with 59 targeted by both instruments. Recoveries for all but 11 of the analytes in at least one of the matrixes were between 70-120% (90-110% for 206 pesticides), and repeatabilities typically <10% were achieved for a wide range of fortified pesticides, including methamidophos, spinosad, imidacloprid, and imazalil. Dispersive SPE with PSA retained carboxylic acids (e.g., daminozide), and <50% recoveries were obtained for asulam, pyridate, dicofol, thiram, and chlorothalonil. Many actual samples and proficiency test samples were analyzed by the method, and the results compared favorably with those from traditional methods.</description><identifier>ISSN: 1060-3271</identifier><identifier>EISSN: 1944-7922</identifier><identifier>DOI: 10.1093/jaoac/88.2.595</identifier><identifier>PMID: 15859089</identifier><language>eng</language><publisher>Gaithersburg, MD: AOAC International</publisher><subject>Acetone ; Biological and medical sciences ; Calibration ; capillary gas chromatography ; Chromatography, Liquid ; detection ; food contamination ; Food industries ; Fruit - chemistry ; Fruit and vegetable industries ; fruits (food) ; Fundamental and applied biological sciences. Psychology ; Gas Chromatography-Mass Spectrometry ; General aspects ; Indicators and Reagents ; lettuce ; Liquid chromatography ; Mass Spectrometry ; Methods ; Methods of analysis, processing and quality control, regulation, standards ; model validation ; Nitriles ; oranges ; Organic acids ; pesticide residues ; Pesticide Residues - analysis ; Pesticides - analysis ; rapid methods ; Reference Standards ; Reproducibility of Results ; Solvents ; Vegetables ; Vegetables - chemistry</subject><ispartof>Journal of AOAC International, 2005-03, Vol.88 (2), p.595-614</ispartof><rights>2005 INIST-CNRS</rights><rights>COPYRIGHT 2005 Oxford University Press</rights><lds50>peer_reviewed</lds50><oa>free_for_read</oa><woscitedreferencessubscribed>false</woscitedreferencessubscribed><citedby>FETCH-LOGICAL-c492t-b5eb008a4a7ae23275cf46988da8517c2ea23eb296f55c0c80b76dca41f758b13</citedby></display><links><openurl>$$Topenurl_article</openurl><openurlfulltext>$$Topenurlfull_article</openurlfulltext><thumbnail>$$Tsyndetics_thumb_exl</thumbnail><link.rule.ids>314,780,784,27923,27924</link.rule.ids><backlink>$$Uhttp://pascal-francis.inist.fr/vibad/index.php?action=getRecordDetail&idt=16634906$$DView record in Pascal Francis$$Hfree_for_read</backlink><backlink>$$Uhttps://www.ncbi.nlm.nih.gov/pubmed/15859089$$D View this record in MEDLINE/PubMed$$Hfree_for_read</backlink></links><search><creatorcontrib>Lehotay, S.J</creatorcontrib><creatorcontrib>Kok, A. de</creatorcontrib><creatorcontrib>Hiemstra, M</creatorcontrib><creatorcontrib>Bodegraven, P. van</creatorcontrib><title>Validation of a fast and easy method for the determination of residues from 229 pesticides in fruits and vegetables using gas and liquid chromatography and mass spectrometric detection</title><title>Journal of AOAC International</title><addtitle>J AOAC Int</addtitle><description>Validation experiments were conducted of a simple, fast, and inexpensive method for the determination of 229 pesticides fortified at 10-100 ng/g in lettuce and orange matrixes. The method is known as the quick, easy, cheap, effective, rugged, and safe (QuEChERS) method for pesticide residues in foods. The procedure involved the extraction of a 15 g sample with 15 mL acetonitrile, followed by a liquid-liquid partitioning step performed by adding 6 g anhydrous MgSO4 plus 1.5 g NaCl. After centrifugation, the extract was decanted into a tube containing 300 mg primary secondary amine (PSA) sorbent plus 1.8 g anhydrous MgSO4, which constituted a cleanup procedure called dispersive solid-phase extraction (dispersive SPE). After a second shaking and centrifugation step, the acetonitrile extract was transferred to autosampler vials for concurrent analysis by gas chromatography/mass spectrometry with an ion trap instrument and liquid chromatography/tandem mass spectrometry with a triple quadrupole instrument using electrospray ionization. Each analytical method was designed to analyze 144 pesticides, with 59 targeted by both instruments. Recoveries for all but 11 of the analytes in at least one of the matrixes were between 70-120% (90-110% for 206 pesticides), and repeatabilities typically <10% were achieved for a wide range of fortified pesticides, including methamidophos, spinosad, imidacloprid, and imazalil. Dispersive SPE with PSA retained carboxylic acids (e.g., daminozide), and <50% recoveries were obtained for asulam, pyridate, dicofol, thiram, and chlorothalonil. Many actual samples and proficiency test samples were analyzed by the method, and the results compared favorably with those from traditional methods.</description><subject>Acetone</subject><subject>Biological and medical sciences</subject><subject>Calibration</subject><subject>capillary gas chromatography</subject><subject>Chromatography, Liquid</subject><subject>detection</subject><subject>food contamination</subject><subject>Food industries</subject><subject>Fruit - chemistry</subject><subject>Fruit and vegetable industries</subject><subject>fruits (food)</subject><subject>Fundamental and applied biological sciences. Psychology</subject><subject>Gas Chromatography-Mass Spectrometry</subject><subject>General aspects</subject><subject>Indicators and Reagents</subject><subject>lettuce</subject><subject>Liquid chromatography</subject><subject>Mass Spectrometry</subject><subject>Methods</subject><subject>Methods of analysis, processing and quality control, regulation, standards</subject><subject>model validation</subject><subject>Nitriles</subject><subject>oranges</subject><subject>Organic acids</subject><subject>pesticide residues</subject><subject>Pesticide Residues - analysis</subject><subject>Pesticides - analysis</subject><subject>rapid methods</subject><subject>Reference Standards</subject><subject>Reproducibility of Results</subject><subject>Solvents</subject><subject>Vegetables</subject><subject>Vegetables - chemistry</subject><issn>1060-3271</issn><issn>1944-7922</issn><fulltext>true</fulltext><rsrctype>article</rsrctype><creationdate>2005</creationdate><recordtype>article</recordtype><sourceid>EIF</sourceid><recordid>eNpFkk9v3CAQxa2qVfOnvfbYcunRG8AGwzGK2qZSpB7a9GqNYfAS2cYFNtJ-s368kt1VVxxA837zBvGoqg-MbhjVzc0TBDA3Sm34Rmjxqrpkum3rTnP-upyppHXDO3ZRXaX0RGnLJOVvqwsmlNBU6cvq72-YvIXsw0KCI0AcpExgsQQh7cmMeRsscSGSvEViMWOc_fKfj5i83WEiLoaZcK7Jiil7422p-aWUdz6ng98zjphhmIqwS34ZyQhHYfJ_dt4Ssy0WkMMYYd3uD8oMKZG0oslFwhy9OdzAvEx_V71xMCV8f9qvq8evX37d3dcPP759v7t9qE2rea4HgQOlClroAHl5C2FcK7VSFpRgneEIvMGBa-mEMNQoOnTSGmiZ64QaWHNdbY6-I0zY-8WFHMGUZXH2JizofKnfcqm05LoV5wYTQ0oRXb9GP0Pc94z2L5n1h8x6pXrel8xKw8djw7obZrRn_BRSAT6fAEgGJhdhMT6dOSmbVlNZuE9HzkHoYYyFefzJKWto-QgNY7T5B5rdrXo</recordid><startdate>20050301</startdate><enddate>20050301</enddate><creator>Lehotay, S.J</creator><creator>Kok, A. de</creator><creator>Hiemstra, M</creator><creator>Bodegraven, P. van</creator><general>AOAC International</general><general>Oxford University Press</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></search><sort><creationdate>20050301</creationdate><title>Validation of a fast and easy method for the determination of residues from 229 pesticides in fruits and vegetables using gas and liquid chromatography and mass spectrometric detection</title><author>Lehotay, S.J ; Kok, A. de ; Hiemstra, M ; Bodegraven, P. van</author></sort><facets><frbrtype>5</frbrtype><frbrgroupid>cdi_FETCH-LOGICAL-c492t-b5eb008a4a7ae23275cf46988da8517c2ea23eb296f55c0c80b76dca41f758b13</frbrgroupid><rsrctype>articles</rsrctype><prefilter>articles</prefilter><language>eng</language><creationdate>2005</creationdate><topic>Acetone</topic><topic>Biological and medical sciences</topic><topic>Calibration</topic><topic>capillary gas chromatography</topic><topic>Chromatography, Liquid</topic><topic>detection</topic><topic>food contamination</topic><topic>Food industries</topic><topic>Fruit - chemistry</topic><topic>Fruit and vegetable industries</topic><topic>fruits (food)</topic><topic>Fundamental and applied biological sciences. Psychology</topic><topic>Gas Chromatography-Mass Spectrometry</topic><topic>General aspects</topic><topic>Indicators and Reagents</topic><topic>lettuce</topic><topic>Liquid chromatography</topic><topic>Mass Spectrometry</topic><topic>Methods</topic><topic>Methods of analysis, processing and quality control, regulation, standards</topic><topic>model validation</topic><topic>Nitriles</topic><topic>oranges</topic><topic>Organic acids</topic><topic>pesticide residues</topic><topic>Pesticide Residues - analysis</topic><topic>Pesticides - analysis</topic><topic>rapid methods</topic><topic>Reference Standards</topic><topic>Reproducibility of Results</topic><topic>Solvents</topic><topic>Vegetables</topic><topic>Vegetables - chemistry</topic><toplevel>peer_reviewed</toplevel><toplevel>online_resources</toplevel><creatorcontrib>Lehotay, S.J</creatorcontrib><creatorcontrib>Kok, A. de</creatorcontrib><creatorcontrib>Hiemstra, M</creatorcontrib><creatorcontrib>Bodegraven, P. van</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><jtitle>Journal of AOAC International</jtitle></facets><delivery><delcategory>Remote Search Resource</delcategory><fulltext>fulltext</fulltext></delivery><addata><au>Lehotay, S.J</au><au>Kok, A. de</au><au>Hiemstra, M</au><au>Bodegraven, P. van</au><format>journal</format><genre>article</genre><ristype>JOUR</ristype><atitle>Validation of a fast and easy method for the determination of residues from 229 pesticides in fruits and vegetables using gas and liquid chromatography and mass spectrometric detection</atitle><jtitle>Journal of AOAC International</jtitle><addtitle>J AOAC Int</addtitle><date>2005-03-01</date><risdate>2005</risdate><volume>88</volume><issue>2</issue><spage>595</spage><epage>614</epage><pages>595-614</pages><issn>1060-3271</issn><eissn>1944-7922</eissn><abstract>Validation experiments were conducted of a simple, fast, and inexpensive method for the determination of 229 pesticides fortified at 10-100 ng/g in lettuce and orange matrixes. The method is known as the quick, easy, cheap, effective, rugged, and safe (QuEChERS) method for pesticide residues in foods. The procedure involved the extraction of a 15 g sample with 15 mL acetonitrile, followed by a liquid-liquid partitioning step performed by adding 6 g anhydrous MgSO4 plus 1.5 g NaCl. After centrifugation, the extract was decanted into a tube containing 300 mg primary secondary amine (PSA) sorbent plus 1.8 g anhydrous MgSO4, which constituted a cleanup procedure called dispersive solid-phase extraction (dispersive SPE). After a second shaking and centrifugation step, the acetonitrile extract was transferred to autosampler vials for concurrent analysis by gas chromatography/mass spectrometry with an ion trap instrument and liquid chromatography/tandem mass spectrometry with a triple quadrupole instrument using electrospray ionization. Each analytical method was designed to analyze 144 pesticides, with 59 targeted by both instruments. Recoveries for all but 11 of the analytes in at least one of the matrixes were between 70-120% (90-110% for 206 pesticides), and repeatabilities typically <10% were achieved for a wide range of fortified pesticides, including methamidophos, spinosad, imidacloprid, and imazalil. Dispersive SPE with PSA retained carboxylic acids (e.g., daminozide), and <50% recoveries were obtained for asulam, pyridate, dicofol, thiram, and chlorothalonil. Many actual samples and proficiency test samples were analyzed by the method, and the results compared favorably with those from traditional methods.</abstract><cop>Gaithersburg, MD</cop><pub>AOAC International</pub><pmid>15859089</pmid><doi>10.1093/jaoac/88.2.595</doi><tpages>20</tpages><oa>free_for_read</oa></addata></record> |
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| ispartof | Journal of AOAC International, 2005-03, Vol.88 (2), p.595-614 |
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| source | MEDLINE; Oxford University Press Journals All Titles (1996-Current) |
| subjects | Acetone Biological and medical sciences Calibration capillary gas chromatography Chromatography, Liquid detection food contamination Food industries Fruit - chemistry Fruit and vegetable industries fruits (food) Fundamental and applied biological sciences. Psychology Gas Chromatography-Mass Spectrometry General aspects Indicators and Reagents lettuce Liquid chromatography Mass Spectrometry Methods Methods of analysis, processing and quality control, regulation, standards model validation Nitriles oranges Organic acids pesticide residues Pesticide Residues - analysis Pesticides - analysis rapid methods Reference Standards Reproducibility of Results Solvents Vegetables Vegetables - chemistry |
| title | Validation of a fast and easy method for the determination of residues from 229 pesticides in fruits and vegetables using gas and liquid chromatography and mass spectrometric detection |
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