Determination of Pesticide Residues in Foods by Acetonitrile Extraction and Partitioning with Magnesium Sulfate: Collaborative Study
A collaborative study was conducted to determine multiple pesticide residues in fruits and vegetables using a quick, simple, inexpensive, and effective sample preparation method followed by concurrent analysis with gas chromatography/mass spectrometry (GC/MS) and liquid chromatography/ tandem mass s...
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| Veröffentlicht in: | Journal of AOAC International 2007-03, Vol.90 (2), p.485-520 |
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| description | A collaborative study was conducted to determine multiple pesticide residues in fruits and vegetables using a quick, simple, inexpensive, and effective sample preparation method followed by concurrent analysis with gas chromatography/mass spectrometry (GC/MS) and liquid chromatography/ tandem mass spectrometry (LC/MS/MS). For short, the method is known as QuEChERS, which stands for quick, easy, cheap, effective, rugged, and safe. Twenty representative pesticides were fortified in 3 matrixes (grapes, lettuces, and oranges) at 3 duplicate levels unknown to the collaborators ranging from 10 to 1000 ng/g. Additionally, 8 incurred pesticide residues were determined. Thirteen laboratories from 7 countries provided results in the study, and a variety of different instruments were used by collaborators. The QuEChERS procedure simply entails 3 main steps: (1) a 15 g homogenized sample is weighed into a 50 mL centrifuge tube to which 15 mL acetonitrile containing 1% HOAc is added along with 6 g MgSO4 and 1.5 g NaOAc, and the tube is shaken and centrifuged; (2) a portion of the extract is mixed with 3 + 1 (w/w) MgSO4-primary secondary amine sorbent (200 mg/mL extract) and centrifuged; and (3) the final extract is analyzed by GC/MS and LC/MS/MS. To detect residues |
| doi_str_mv | 10.1093/jaoac/90.2.485 |
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For short, the method is known as QuEChERS, which stands for quick, easy, cheap, effective, rugged, and safe. Twenty representative pesticides were fortified in 3 matrixes (grapes, lettuces, and oranges) at 3 duplicate levels unknown to the collaborators ranging from 10 to 1000 ng/g. Additionally, 8 incurred pesticide residues were determined. Thirteen laboratories from 7 countries provided results in the study, and a variety of different instruments were used by collaborators. The QuEChERS procedure simply entails 3 main steps: (1) a 15 g homogenized sample is weighed into a 50 mL centrifuge tube to which 15 mL acetonitrile containing 1% HOAc is added along with 6 g MgSO4 and 1.5 g NaOAc, and the tube is shaken and centrifuged; (2) a portion of the extract is mixed with 3 + 1 (w/w) MgSO4-primary secondary amine sorbent (200 mg/mL extract) and centrifuged; and (3) the final extract is analyzed by GC/MS and LC/MS/MS. To detect residues <10 ng/g in GC/MS, large-volume injection of 8 μL is typically needed, or the extract can be concentrated to 4 g/mL in toluene, in which case 2 μL splitless injection is used. In the study, the averaged results for data from 7-13 laboratories (not using internal standardization) for the 18 blind duplicates at the 9 spiking levels in the 3 matrixes are as follows [%recovery and reproducibility relative standard deviation (RSDR, %)]: atrazine, 92 (18); azoxystrobin, 93 (15); bifenthrin, 90 (16); carbaryl, 96 (20); chlorothalonil, 70 (34); chlorpyrifos, 89 (25); cyprodinil, 89 (19); o, p'-DDD, 89 (18); dichlorvos, 82 (21); endosulfan sulfate, 80 (27); imazalil, 77 (33); imidacloprid, 96 (16); linuron, 89 (19);methamidophos, 87 (17); methomyl, 96 (17); procymidone, 91 (20); pymetrozine, 69 (19); tebuconazole, 89 (15); tolylfluanid (in grapes and oranges), 68 (33); and trifluralin, 85 (20). For incurred pesticides, kresoxim-methyl (9.2 ± 3.2 ng/g) and cyprodinil (112 ± 18) were found in the grapes; permethrins (112 ± 41), λ-cyhalothrin (58 ± 11), and imidacloprid (12 ± 2) were determined in the lettuces; and ethion (198 ± 36), thiabendazole (53 ± 8), and imazalil (13 ± 4) were determined in the oranges. Chlorpyrifosmethyl (200 ng/g) was used as a quality control standard added during sample homogenization and yielded 86% recovery and 19% RSDR. Intralaboratory repeatabilities for the method averaged 9.8% RSD for all analytes. The results demonstrate that the method is fit-for- purpose to monitor many pesticide residues in fruits and vegetables, and the Study Director recommends that it be adopted Official First Action.</description><identifier>ISSN: 1060-3271</identifier><identifier>EISSN: 1944-7922</identifier><identifier>DOI: 10.1093/jaoac/90.2.485</identifier><identifier>PMID: 17474521</identifier><language>eng</language><publisher>Gaithersburg, MD: AOAC International</publisher><subject>Acetonitrile ; Acetonitriles - analysis ; Biological and medical sciences ; capillary gas chromatography ; Citrus ; collaborative testing ; Cost-Benefit Analysis ; environmental fate ; Food Analysis - methods ; Food Contamination ; Food engineering ; Food industries ; food matrix ; Fruit ; fruits (food) ; Fundamental and applied biological sciences. Psychology ; fungicide residues ; Gas chromatography ; Gas Chromatography-Mass Spectrometry - methods ; General aspects ; grapes ; herbicide residues ; insecticide residues ; Lactuca ; lettuce ; Liquid chromatography ; Magnesium sulfate ; Magnesium Sulfate - analysis ; Magnesium Sulfate - chemistry ; Mass spectrometry ; maximum residue limits ; Methods ; oranges ; pesticide residues ; Pesticide Residues - analysis ; Pesticides ; Pesticides - analysis ; Pesticides - chemistry ; Quality Control ; Reproducibility of Results ; solid phase extraction ; Solvents - chemistry ; Testing ; Trace analysis ; Vegetables</subject><ispartof>Journal of AOAC International, 2007-03, Vol.90 (2), p.485-520</ispartof><rights>2007 INIST-CNRS</rights><rights>COPYRIGHT 2007 Oxford University Press</rights><lds50>peer_reviewed</lds50><oa>free_for_read</oa><woscitedreferencessubscribed>false</woscitedreferencessubscribed><citedby>FETCH-LOGICAL-c454t-b13d20946bccf9e6c0a1646f4913c0e4cd90ca01a7dce8926cc6584a19e81eb63</citedby></display><links><openurl>$$Topenurl_article</openurl><openurlfulltext>$$Topenurlfull_article</openurlfulltext><thumbnail>$$Tsyndetics_thumb_exl</thumbnail><link.rule.ids>314,777,781,27905,27906</link.rule.ids><backlink>$$Uhttp://pascal-francis.inist.fr/vibad/index.php?action=getRecordDetail&idt=18690576$$DView record in Pascal Francis$$Hfree_for_read</backlink><backlink>$$Uhttps://www.ncbi.nlm.nih.gov/pubmed/17474521$$D View this record in MEDLINE/PubMed$$Hfree_for_read</backlink></links><search><creatorcontrib>Lehotay, S.J</creatorcontrib><creatorcontrib>Collaborators</creatorcontrib><title>Determination of Pesticide Residues in Foods by Acetonitrile Extraction and Partitioning with Magnesium Sulfate: Collaborative Study</title><title>Journal of AOAC International</title><addtitle>J AOAC Int</addtitle><description>A collaborative study was conducted to determine multiple pesticide residues in fruits and vegetables using a quick, simple, inexpensive, and effective sample preparation method followed by concurrent analysis with gas chromatography/mass spectrometry (GC/MS) and liquid chromatography/ tandem mass spectrometry (LC/MS/MS). For short, the method is known as QuEChERS, which stands for quick, easy, cheap, effective, rugged, and safe. Twenty representative pesticides were fortified in 3 matrixes (grapes, lettuces, and oranges) at 3 duplicate levels unknown to the collaborators ranging from 10 to 1000 ng/g. Additionally, 8 incurred pesticide residues were determined. Thirteen laboratories from 7 countries provided results in the study, and a variety of different instruments were used by collaborators. The QuEChERS procedure simply entails 3 main steps: (1) a 15 g homogenized sample is weighed into a 50 mL centrifuge tube to which 15 mL acetonitrile containing 1% HOAc is added along with 6 g MgSO4 and 1.5 g NaOAc, and the tube is shaken and centrifuged; (2) a portion of the extract is mixed with 3 + 1 (w/w) MgSO4-primary secondary amine sorbent (200 mg/mL extract) and centrifuged; and (3) the final extract is analyzed by GC/MS and LC/MS/MS. To detect residues <10 ng/g in GC/MS, large-volume injection of 8 μL is typically needed, or the extract can be concentrated to 4 g/mL in toluene, in which case 2 μL splitless injection is used. In the study, the averaged results for data from 7-13 laboratories (not using internal standardization) for the 18 blind duplicates at the 9 spiking levels in the 3 matrixes are as follows [%recovery and reproducibility relative standard deviation (RSDR, %)]: atrazine, 92 (18); azoxystrobin, 93 (15); bifenthrin, 90 (16); carbaryl, 96 (20); chlorothalonil, 70 (34); chlorpyrifos, 89 (25); cyprodinil, 89 (19); o, p'-DDD, 89 (18); dichlorvos, 82 (21); endosulfan sulfate, 80 (27); imazalil, 77 (33); imidacloprid, 96 (16); linuron, 89 (19);methamidophos, 87 (17); methomyl, 96 (17); procymidone, 91 (20); pymetrozine, 69 (19); tebuconazole, 89 (15); tolylfluanid (in grapes and oranges), 68 (33); and trifluralin, 85 (20). For incurred pesticides, kresoxim-methyl (9.2 ± 3.2 ng/g) and cyprodinil (112 ± 18) were found in the grapes; permethrins (112 ± 41), λ-cyhalothrin (58 ± 11), and imidacloprid (12 ± 2) were determined in the lettuces; and ethion (198 ± 36), thiabendazole (53 ± 8), and imazalil (13 ± 4) were determined in the oranges. Chlorpyrifosmethyl (200 ng/g) was used as a quality control standard added during sample homogenization and yielded 86% recovery and 19% RSDR. Intralaboratory repeatabilities for the method averaged 9.8% RSD for all analytes. The results demonstrate that the method is fit-for- purpose to monitor many pesticide residues in fruits and vegetables, and the Study Director recommends that it be adopted Official First Action.</description><subject>Acetonitrile</subject><subject>Acetonitriles - analysis</subject><subject>Biological and medical sciences</subject><subject>capillary gas chromatography</subject><subject>Citrus</subject><subject>collaborative testing</subject><subject>Cost-Benefit Analysis</subject><subject>environmental fate</subject><subject>Food Analysis - methods</subject><subject>Food Contamination</subject><subject>Food engineering</subject><subject>Food industries</subject><subject>food matrix</subject><subject>Fruit</subject><subject>fruits (food)</subject><subject>Fundamental and applied biological sciences. Psychology</subject><subject>fungicide residues</subject><subject>Gas chromatography</subject><subject>Gas Chromatography-Mass Spectrometry - methods</subject><subject>General aspects</subject><subject>grapes</subject><subject>herbicide residues</subject><subject>insecticide residues</subject><subject>Lactuca</subject><subject>lettuce</subject><subject>Liquid chromatography</subject><subject>Magnesium sulfate</subject><subject>Magnesium Sulfate - analysis</subject><subject>Magnesium Sulfate - chemistry</subject><subject>Mass spectrometry</subject><subject>maximum residue limits</subject><subject>Methods</subject><subject>oranges</subject><subject>pesticide residues</subject><subject>Pesticide Residues - analysis</subject><subject>Pesticides</subject><subject>Pesticides - analysis</subject><subject>Pesticides - chemistry</subject><subject>Quality Control</subject><subject>Reproducibility of Results</subject><subject>solid phase extraction</subject><subject>Solvents - chemistry</subject><subject>Testing</subject><subject>Trace analysis</subject><subject>Vegetables</subject><issn>1060-3271</issn><issn>1944-7922</issn><fulltext>true</fulltext><rsrctype>article</rsrctype><creationdate>2007</creationdate><recordtype>article</recordtype><sourceid>EIF</sourceid><recordid>eNptkUFv1DAQhSMEoqVw5QiWKo7Z2o7jxNxWSwtIRVQsPVsTe7y4SuLK9gJ754fj7a7US-XD2NL3ZvzmVdVbRheMqubiDgKYC0UXfCH69ll1ypQQdac4f17uVNK64R07qV6ldEepYJLyl9UJ60QnWs5Oq3-fMGOc_AzZh5kER24wZW-8RfIDk7dbTMTP5CoEm8iwI0uDOcw-Rz8iufybI5gHJcyW3EDMfv_y84b88fkX-QabuXTZTmS9HR1k_EhWYRxhCLEM_I1knbd297p64WBM-OZYz6rbq8ufqy_19ffPX1fL69qIVuR6YI3lVAk5GOMUSkOBSSGdUKwxFIWxihqgDDprsFdcGiPbXgBT2DMcZHNWnR_6bmBE7WcX9t-ffDJ6WVbSKtlKWqjFE1Q5FidvwoyuWH9SYGJIKaLT99FPEHeaUb1PST-kpBXVXJeUiuDdQXC_HSa0j_gxlgJ8OAKQDIwuwmx8euR6qWjb7Q29P3AOgoZNLMztmlPWUNr1bdeJ5j-5xqX9</recordid><startdate>20070301</startdate><enddate>20070301</enddate><creator>Lehotay, S.J</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>20070301</creationdate><title>Determination of Pesticide Residues in Foods by Acetonitrile Extraction and Partitioning with Magnesium Sulfate: Collaborative Study</title><author>Lehotay, S.J</author></sort><facets><frbrtype>5</frbrtype><frbrgroupid>cdi_FETCH-LOGICAL-c454t-b13d20946bccf9e6c0a1646f4913c0e4cd90ca01a7dce8926cc6584a19e81eb63</frbrgroupid><rsrctype>articles</rsrctype><prefilter>articles</prefilter><language>eng</language><creationdate>2007</creationdate><topic>Acetonitrile</topic><topic>Acetonitriles - analysis</topic><topic>Biological and medical sciences</topic><topic>capillary gas chromatography</topic><topic>Citrus</topic><topic>collaborative testing</topic><topic>Cost-Benefit Analysis</topic><topic>environmental fate</topic><topic>Food Analysis - methods</topic><topic>Food Contamination</topic><topic>Food engineering</topic><topic>Food industries</topic><topic>food matrix</topic><topic>Fruit</topic><topic>fruits (food)</topic><topic>Fundamental and applied biological sciences. Psychology</topic><topic>fungicide residues</topic><topic>Gas chromatography</topic><topic>Gas Chromatography-Mass Spectrometry - methods</topic><topic>General aspects</topic><topic>grapes</topic><topic>herbicide residues</topic><topic>insecticide residues</topic><topic>Lactuca</topic><topic>lettuce</topic><topic>Liquid chromatography</topic><topic>Magnesium sulfate</topic><topic>Magnesium Sulfate - analysis</topic><topic>Magnesium Sulfate - chemistry</topic><topic>Mass spectrometry</topic><topic>maximum residue limits</topic><topic>Methods</topic><topic>oranges</topic><topic>pesticide residues</topic><topic>Pesticide Residues - analysis</topic><topic>Pesticides</topic><topic>Pesticides - analysis</topic><topic>Pesticides - chemistry</topic><topic>Quality Control</topic><topic>Reproducibility of Results</topic><topic>solid phase extraction</topic><topic>Solvents - chemistry</topic><topic>Testing</topic><topic>Trace analysis</topic><topic>Vegetables</topic><toplevel>peer_reviewed</toplevel><toplevel>online_resources</toplevel><creatorcontrib>Lehotay, S.J</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><jtitle>Journal of AOAC International</jtitle></facets><delivery><delcategory>Remote Search Resource</delcategory><fulltext>fulltext</fulltext></delivery><addata><au>Lehotay, S.J</au><aucorp>Collaborators</aucorp><format>journal</format><genre>article</genre><ristype>JOUR</ristype><atitle>Determination of Pesticide Residues in Foods by Acetonitrile Extraction and Partitioning with Magnesium Sulfate: Collaborative Study</atitle><jtitle>Journal of AOAC International</jtitle><addtitle>J AOAC Int</addtitle><date>2007-03-01</date><risdate>2007</risdate><volume>90</volume><issue>2</issue><spage>485</spage><epage>520</epage><pages>485-520</pages><issn>1060-3271</issn><eissn>1944-7922</eissn><abstract>A collaborative study was conducted to determine multiple pesticide residues in fruits and vegetables using a quick, simple, inexpensive, and effective sample preparation method followed by concurrent analysis with gas chromatography/mass spectrometry (GC/MS) and liquid chromatography/ tandem mass spectrometry (LC/MS/MS). For short, the method is known as QuEChERS, which stands for quick, easy, cheap, effective, rugged, and safe. Twenty representative pesticides were fortified in 3 matrixes (grapes, lettuces, and oranges) at 3 duplicate levels unknown to the collaborators ranging from 10 to 1000 ng/g. Additionally, 8 incurred pesticide residues were determined. Thirteen laboratories from 7 countries provided results in the study, and a variety of different instruments were used by collaborators. The QuEChERS procedure simply entails 3 main steps: (1) a 15 g homogenized sample is weighed into a 50 mL centrifuge tube to which 15 mL acetonitrile containing 1% HOAc is added along with 6 g MgSO4 and 1.5 g NaOAc, and the tube is shaken and centrifuged; (2) a portion of the extract is mixed with 3 + 1 (w/w) MgSO4-primary secondary amine sorbent (200 mg/mL extract) and centrifuged; and (3) the final extract is analyzed by GC/MS and LC/MS/MS. To detect residues <10 ng/g in GC/MS, large-volume injection of 8 μL is typically needed, or the extract can be concentrated to 4 g/mL in toluene, in which case 2 μL splitless injection is used. In the study, the averaged results for data from 7-13 laboratories (not using internal standardization) for the 18 blind duplicates at the 9 spiking levels in the 3 matrixes are as follows [%recovery and reproducibility relative standard deviation (RSDR, %)]: atrazine, 92 (18); azoxystrobin, 93 (15); bifenthrin, 90 (16); carbaryl, 96 (20); chlorothalonil, 70 (34); chlorpyrifos, 89 (25); cyprodinil, 89 (19); o, p'-DDD, 89 (18); dichlorvos, 82 (21); endosulfan sulfate, 80 (27); imazalil, 77 (33); imidacloprid, 96 (16); linuron, 89 (19);methamidophos, 87 (17); methomyl, 96 (17); procymidone, 91 (20); pymetrozine, 69 (19); tebuconazole, 89 (15); tolylfluanid (in grapes and oranges), 68 (33); and trifluralin, 85 (20). For incurred pesticides, kresoxim-methyl (9.2 ± 3.2 ng/g) and cyprodinil (112 ± 18) were found in the grapes; permethrins (112 ± 41), λ-cyhalothrin (58 ± 11), and imidacloprid (12 ± 2) were determined in the lettuces; and ethion (198 ± 36), thiabendazole (53 ± 8), and imazalil (13 ± 4) were determined in the oranges. Chlorpyrifosmethyl (200 ng/g) was used as a quality control standard added during sample homogenization and yielded 86% recovery and 19% RSDR. Intralaboratory repeatabilities for the method averaged 9.8% RSD for all analytes. The results demonstrate that the method is fit-for- purpose to monitor many pesticide residues in fruits and vegetables, and the Study Director recommends that it be adopted Official First Action.</abstract><cop>Gaithersburg, MD</cop><pub>AOAC International</pub><pmid>17474521</pmid><doi>10.1093/jaoac/90.2.485</doi><tpages>36</tpages><oa>free_for_read</oa></addata></record> |
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| ispartof | Journal of AOAC International, 2007-03, Vol.90 (2), p.485-520 |
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| subjects | Acetonitrile Acetonitriles - analysis Biological and medical sciences capillary gas chromatography Citrus collaborative testing Cost-Benefit Analysis environmental fate Food Analysis - methods Food Contamination Food engineering Food industries food matrix Fruit fruits (food) Fundamental and applied biological sciences. Psychology fungicide residues Gas chromatography Gas Chromatography-Mass Spectrometry - methods General aspects grapes herbicide residues insecticide residues Lactuca lettuce Liquid chromatography Magnesium sulfate Magnesium Sulfate - analysis Magnesium Sulfate - chemistry Mass spectrometry maximum residue limits Methods oranges pesticide residues Pesticide Residues - analysis Pesticides Pesticides - analysis Pesticides - chemistry Quality Control Reproducibility of Results solid phase extraction Solvents - chemistry Testing Trace analysis Vegetables |
| title | Determination of Pesticide Residues in Foods by Acetonitrile Extraction and Partitioning with Magnesium Sulfate: Collaborative Study |
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