Determination of Fumonisins B1 and B2 in Corn by LC/MS with Immunoaffinity Column Cleanup: Interlaboratory Study
An interlaboratory validation study was conducted to establish the method performance characteristics of an immunoaffinity column (IAC) cleanup procedure followed by LC/MS for the determination of fumonisins B1 (FB1) and B2 (FB2) and combined FB1 + FB2 in corn. The test portion is extracted with ace...
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| Veröffentlicht in: | Journal of AOAC International 2010-03, Vol.93 (2), p.611-621 |
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| description | An interlaboratory validation study was conducted to establish the method performance characteristics of an immunoaffinity column (IAC) cleanup procedure followed by LC/MS for the determination of fumonisins B1 (FB1) and B2 (FB2) and combined FB1 + FB2 in corn. The test portion is extracted with acetonitrile–methanol–water (25 + 25 + 50). The extract is filtered, diluted with phosphate-buffered saline solution, and applied to an IAC. FB1 and FB2 are removed with methanol, followed by water, then directly determined by RPLC with MS detection using selected-ion monitoring of two characteristic ions in each case. Naturally contaminated corn samples were milled to a fine powder and mixed to produce three samples with target levels of combined FB1 + FB2 ranging from 350 to 4000 μg/kg. Of 15 initially participating laboratories, two failed to report results and another did not follow the prescribed method. Thus, valid results were obtained from 12 participants located in 11 countries. Statistical analysis of the results produced RSDr values of 4.6–11.9, 1.9–12.6, and 1.4–11.5% for FB1, FB2, and combined FB1 + FB2, respectively; the corresponding RSD(R) values were 19.8–23.8, 18.2–25.5, and 18.8–23.2%. The three concentration levels of combined FB1 + FB2 were 534, 1194, and 1954 μg/kg. HorRat values for r and R were all |
| doi_str_mv | 10.1093/jaoac/93.2.611 |
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The test portion is extracted with acetonitrile–methanol–water (25 + 25 + 50). The extract is filtered, diluted with phosphate-buffered saline solution, and applied to an IAC. FB1 and FB2 are removed with methanol, followed by water, then directly determined by RPLC with MS detection using selected-ion monitoring of two characteristic ions in each case. Naturally contaminated corn samples were milled to a fine powder and mixed to produce three samples with target levels of combined FB1 + FB2 ranging from 350 to 4000 μg/kg. Of 15 initially participating laboratories, two failed to report results and another did not follow the prescribed method. Thus, valid results were obtained from 12 participants located in 11 countries. Statistical analysis of the results produced RSDr values of 4.6–11.9, 1.9–12.6, and 1.4–11.5% for FB1, FB2, and combined FB1 + FB2, respectively; the corresponding RSD(R) values were 19.8–23.8, 18.2–25.5, and 18.8–23.2%. The three concentration levels of combined FB1 + FB2 were 534, 1194, and 1954 μg/kg. HorRat values for r and R were all <2.0, indicating that the method is suitable as a regulatory method for the enforcement of European Union limits for fumonisins in corn.</description><identifier>ISSN: 1060-3271</identifier><identifier>EISSN: 1944-7922</identifier><identifier>DOI: 10.1093/jaoac/93.2.611</identifier><identifier>PMID: 20480909</identifier><language>eng</language><publisher>Gaithersburg, MD: AOAC International</publisher><subject>accuracy ; Acetonitriles - chemistry ; Biological and medical sciences ; Calibration ; Cereal and baking product industries ; chemical concentration ; Chemistry Techniques, Analytical ; Chromatography, High Pressure Liquid - methods ; Chromatography, Liquid - methods ; corn ; detection ; extraction ; Food Analysis - methods ; Food Contamination ; Food industries ; fumonisin B1 ; fumonisin B2 ; Fumonisins - analysis ; Fundamental and applied biological sciences. Psychology ; Hydrogen-Ion Concentration ; immunologic techniques ; International Cooperation ; mass spectrometry ; Mass Spectrometry - methods ; Methanol - chemistry ; methodology ; pretreatment ; quantitative analysis ; Reproducibility of Results ; reversed-phase liquid chromatography ; solvents ; statistical analysis ; validity ; Water - chemistry ; Zea mays - metabolism</subject><ispartof>Journal of AOAC International, 2010-03, Vol.93 (2), p.611-621</ispartof><rights>2015 INIST-CNRS</rights><lds50>peer_reviewed</lds50><oa>free_for_read</oa><woscitedreferencessubscribed>false</woscitedreferencessubscribed><citedby>FETCH-LOGICAL-c318t-641d06d4f8f2c3d80162f8f7c971f5d909eae1b966b96333b0d74af09d1599df3</citedby></display><links><openurl>$$Topenurl_article</openurl><openurlfulltext>$$Topenurlfull_article</openurlfulltext><thumbnail>$$Tsyndetics_thumb_exl</thumbnail><link.rule.ids>315,782,786,27933,27934</link.rule.ids><backlink>$$Uhttp://pascal-francis.inist.fr/vibad/index.php?action=getRecordDetail&idt=22745870$$DView record in Pascal Francis$$Hfree_for_read</backlink><backlink>$$Uhttps://www.ncbi.nlm.nih.gov/pubmed/20480909$$D View this record in MEDLINE/PubMed$$Hfree_for_read</backlink></links><search><creatorcontrib>Senyuva, Hamide Z</creatorcontrib><creatorcontrib>Gilbert, John</creatorcontrib><creatorcontrib>Stroka, Joerg</creatorcontrib><creatorcontrib>Collaborators</creatorcontrib><title>Determination of Fumonisins B1 and B2 in Corn by LC/MS with Immunoaffinity Column Cleanup: Interlaboratory Study</title><title>Journal of AOAC International</title><addtitle>J AOAC Int</addtitle><description>An interlaboratory validation study was conducted to establish the method performance characteristics of an immunoaffinity column (IAC) cleanup procedure followed by LC/MS for the determination of fumonisins B1 (FB1) and B2 (FB2) and combined FB1 + FB2 in corn. The test portion is extracted with acetonitrile–methanol–water (25 + 25 + 50). The extract is filtered, diluted with phosphate-buffered saline solution, and applied to an IAC. FB1 and FB2 are removed with methanol, followed by water, then directly determined by RPLC with MS detection using selected-ion monitoring of two characteristic ions in each case. Naturally contaminated corn samples were milled to a fine powder and mixed to produce three samples with target levels of combined FB1 + FB2 ranging from 350 to 4000 μg/kg. Of 15 initially participating laboratories, two failed to report results and another did not follow the prescribed method. Thus, valid results were obtained from 12 participants located in 11 countries. Statistical analysis of the results produced RSDr values of 4.6–11.9, 1.9–12.6, and 1.4–11.5% for FB1, FB2, and combined FB1 + FB2, respectively; the corresponding RSD(R) values were 19.8–23.8, 18.2–25.5, and 18.8–23.2%. The three concentration levels of combined FB1 + FB2 were 534, 1194, and 1954 μg/kg. HorRat values for r and R were all <2.0, indicating that the method is suitable as a regulatory method for the enforcement of European Union limits for fumonisins in corn.</description><subject>accuracy</subject><subject>Acetonitriles - chemistry</subject><subject>Biological and medical sciences</subject><subject>Calibration</subject><subject>Cereal and baking product industries</subject><subject>chemical concentration</subject><subject>Chemistry Techniques, Analytical</subject><subject>Chromatography, High Pressure Liquid - methods</subject><subject>Chromatography, Liquid - methods</subject><subject>corn</subject><subject>detection</subject><subject>extraction</subject><subject>Food Analysis - methods</subject><subject>Food Contamination</subject><subject>Food industries</subject><subject>fumonisin B1</subject><subject>fumonisin B2</subject><subject>Fumonisins - analysis</subject><subject>Fundamental and applied biological sciences. Psychology</subject><subject>Hydrogen-Ion Concentration</subject><subject>immunologic techniques</subject><subject>International Cooperation</subject><subject>mass spectrometry</subject><subject>Mass Spectrometry - methods</subject><subject>Methanol - chemistry</subject><subject>methodology</subject><subject>pretreatment</subject><subject>quantitative analysis</subject><subject>Reproducibility of Results</subject><subject>reversed-phase liquid chromatography</subject><subject>solvents</subject><subject>statistical analysis</subject><subject>validity</subject><subject>Water - chemistry</subject><subject>Zea mays - metabolism</subject><issn>1060-3271</issn><issn>1944-7922</issn><fulltext>true</fulltext><rsrctype>article</rsrctype><creationdate>2010</creationdate><recordtype>article</recordtype><sourceid>EIF</sourceid><recordid>eNpF0EuP0zAUBeAIgZgHbFmCN4hV2utH45jdTGGgUhGLMmvrJrbBo8QudiKUf4-ZFlhYPovPR9apqlcUVhQUXz9gxH6t-IqtGkqfVJdUCVFLxdjTkqGBmjNJL6qrnB8ABG2APa8uGIgWFKjL6vjBTjaNPuDkYyDRkbt5jMFnHzK5pQSDIbeM-EC2MQXSLWS_XX85kF9--kF24ziHiM754KeliGEeCxwshvn4nuxCqR6wiwmnmBZymGazvKieORyyfXm-r6v7u4_ftp_r_ddPu-3Nvu45bae6EdRAY4RrHeu5aYE2rGTZK0ndxpS_W7S0U01TDue8AyMFOlCGbpQyjl9X7069xxR_zjZPevS5t8OAwcY5a8k5Uxsl2iJXJ9mnmHOyTh-THzEtmoL-M7J-HFmXwHQZuTx4fa6eu9Gaf_zvqgW8PQPMPQ4uYeh9_u-YFJtWQnFvTs5h1Pg9FXN_YEA50FYoqiT_DQU7jm8</recordid><startdate>20100301</startdate><enddate>20100301</enddate><creator>Senyuva, Hamide Z</creator><creator>Gilbert, John</creator><creator>Stroka, Joerg</creator><general>AOAC International</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></search><sort><creationdate>20100301</creationdate><title>Determination of Fumonisins B1 and B2 in Corn by LC/MS with Immunoaffinity Column Cleanup: Interlaboratory Study</title><author>Senyuva, Hamide Z ; Gilbert, John ; Stroka, Joerg</author></sort><facets><frbrtype>5</frbrtype><frbrgroupid>cdi_FETCH-LOGICAL-c318t-641d06d4f8f2c3d80162f8f7c971f5d909eae1b966b96333b0d74af09d1599df3</frbrgroupid><rsrctype>articles</rsrctype><prefilter>articles</prefilter><language>eng</language><creationdate>2010</creationdate><topic>accuracy</topic><topic>Acetonitriles - chemistry</topic><topic>Biological and medical sciences</topic><topic>Calibration</topic><topic>Cereal and baking product industries</topic><topic>chemical concentration</topic><topic>Chemistry Techniques, Analytical</topic><topic>Chromatography, High Pressure Liquid - methods</topic><topic>Chromatography, Liquid - methods</topic><topic>corn</topic><topic>detection</topic><topic>extraction</topic><topic>Food Analysis - methods</topic><topic>Food Contamination</topic><topic>Food industries</topic><topic>fumonisin B1</topic><topic>fumonisin B2</topic><topic>Fumonisins - analysis</topic><topic>Fundamental and applied biological sciences. Psychology</topic><topic>Hydrogen-Ion Concentration</topic><topic>immunologic techniques</topic><topic>International Cooperation</topic><topic>mass spectrometry</topic><topic>Mass Spectrometry - methods</topic><topic>Methanol - chemistry</topic><topic>methodology</topic><topic>pretreatment</topic><topic>quantitative analysis</topic><topic>Reproducibility of Results</topic><topic>reversed-phase liquid chromatography</topic><topic>solvents</topic><topic>statistical analysis</topic><topic>validity</topic><topic>Water - chemistry</topic><topic>Zea mays - metabolism</topic><toplevel>peer_reviewed</toplevel><toplevel>online_resources</toplevel><creatorcontrib>Senyuva, Hamide Z</creatorcontrib><creatorcontrib>Gilbert, John</creatorcontrib><creatorcontrib>Stroka, Joerg</creatorcontrib><creatorcontrib>Collaborators</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><jtitle>Journal of AOAC International</jtitle></facets><delivery><delcategory>Remote Search Resource</delcategory><fulltext>fulltext</fulltext></delivery><addata><au>Senyuva, Hamide Z</au><au>Gilbert, John</au><au>Stroka, Joerg</au><aucorp>Collaborators</aucorp><format>journal</format><genre>article</genre><ristype>JOUR</ristype><atitle>Determination of Fumonisins B1 and B2 in Corn by LC/MS with Immunoaffinity Column Cleanup: Interlaboratory Study</atitle><jtitle>Journal of AOAC International</jtitle><addtitle>J AOAC Int</addtitle><date>2010-03-01</date><risdate>2010</risdate><volume>93</volume><issue>2</issue><spage>611</spage><epage>621</epage><pages>611-621</pages><issn>1060-3271</issn><eissn>1944-7922</eissn><abstract>An interlaboratory validation study was conducted to establish the method performance characteristics of an immunoaffinity column (IAC) cleanup procedure followed by LC/MS for the determination of fumonisins B1 (FB1) and B2 (FB2) and combined FB1 + FB2 in corn. The test portion is extracted with acetonitrile–methanol–water (25 + 25 + 50). The extract is filtered, diluted with phosphate-buffered saline solution, and applied to an IAC. FB1 and FB2 are removed with methanol, followed by water, then directly determined by RPLC with MS detection using selected-ion monitoring of two characteristic ions in each case. Naturally contaminated corn samples were milled to a fine powder and mixed to produce three samples with target levels of combined FB1 + FB2 ranging from 350 to 4000 μg/kg. Of 15 initially participating laboratories, two failed to report results and another did not follow the prescribed method. Thus, valid results were obtained from 12 participants located in 11 countries. Statistical analysis of the results produced RSDr values of 4.6–11.9, 1.9–12.6, and 1.4–11.5% for FB1, FB2, and combined FB1 + FB2, respectively; the corresponding RSD(R) values were 19.8–23.8, 18.2–25.5, and 18.8–23.2%. The three concentration levels of combined FB1 + FB2 were 534, 1194, and 1954 μg/kg. HorRat values for r and R were all <2.0, indicating that the method is suitable as a regulatory method for the enforcement of European Union limits for fumonisins in corn.</abstract><cop>Gaithersburg, MD</cop><pub>AOAC International</pub><pmid>20480909</pmid><doi>10.1093/jaoac/93.2.611</doi><tpages>11</tpages><oa>free_for_read</oa></addata></record> |
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| source | MEDLINE; Oxford University Press Journals All Titles (1996-Current) |
| subjects | accuracy Acetonitriles - chemistry Biological and medical sciences Calibration Cereal and baking product industries chemical concentration Chemistry Techniques, Analytical Chromatography, High Pressure Liquid - methods Chromatography, Liquid - methods corn detection extraction Food Analysis - methods Food Contamination Food industries fumonisin B1 fumonisin B2 Fumonisins - analysis Fundamental and applied biological sciences. Psychology Hydrogen-Ion Concentration immunologic techniques International Cooperation mass spectrometry Mass Spectrometry - methods Methanol - chemistry methodology pretreatment quantitative analysis Reproducibility of Results reversed-phase liquid chromatography solvents statistical analysis validity Water - chemistry Zea mays - metabolism |
| title | Determination of Fumonisins B1 and B2 in Corn by LC/MS with Immunoaffinity Column Cleanup: Interlaboratory Study |
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