Validação de método de extração e análise multirresíduo de agrotóxicos em carne bovina por cromatografia gasosa
Autor(a) principal: | |
---|---|
Data de Publicação: | 2008 |
Tipo de documento: | Dissertação |
Idioma: | por |
Título da fonte: | LOCUS Repositório Institucional da UFV |
Texto Completo: | http://locus.ufv.br/handle/123456789/2069 |
Resumo: | The objective of this study was to optimize and validate the liquid-solid extraction with low-temperature purification (LSE- LTP) method for the analysis of chlorpyrifos, endosulfan, cypermethrin and deltamethrin pesticides residues in beef samples. Ideal conditions for the extraction of the pesticides of interest from the rump and liver cattle samples were determined by the employment of experimental planning to optimize the process. Sample mass, solvent extractor, ionic force, extraction time and agitation form were all evaluated. Rump and liver cattle samples were agitated with one-phase solvent mixtures and placed in a freezer for approximately 12 hours. The solids matrix and frozen aqueous phase were separated from the superior liquid phase. This superior phase was filtered and submitted to chromatography analysis using bifenthrin as an internal standard. The optimal technique consisted of supplementing 3.0000 g of beef with 1.0 mL of water, 6.5 mL of acetonitrile, 1.5 mL of ethyl acetate for the rump samples or 1.0 mL of water and 8.0 mL of acetonitrile for the liver samples, and submitting this mixture to ultrasound agitation for 10 minutes, followed by freezing. After separating the phases by freezing the aqueous phase, the supernatant liquid (10 mL) was removed and analyzed by gas chromatography with an electron capture detector. The clean up stage was evaluated for the liver extracts, however, during this stage, not only was the analysis time and cost increased, the percentage of analyte recovery diminished. With the intention of comparing the LSE-LTP with other techniques, the rump and liver samples were submitted to matrix solid phase dispersion (MSPD) extraction. However, this methodology presented recoveries inferior to those of the LSE-LTP in rump samples. For the liver samples, the MSPD technique showed to be little selective, presenting extracts less pure than those obtained by LSE-LTP, due to the greater extraction of matrix components. The optimized method was validated according to selectivity, linearity, detection limits and quantification of the method, precision and accuracy. The results showed that optimized LSE-LTP is efficient for the analysis of the pesticide residues of interest in rump and liver cattle with recovery percentages greater than 70 % and detection limits below the maximum residue limits (MRL) established by Codex Alimentarius the for these pesticides in the studied beef samples. This methodology also presents the small consumption of solvent and absence of purification steps of extracts before chromatography analysis. The effect of the matrix was found to be present in the quantification of pesticides by gas chromatography. To overcome these effects, calibration curves were prepared from organic extracts, obtained from rump and liver cattle free of contaminants. The optimized and validated technique was applied in beef samples acquired commercially in the city of Viçosa, Minas Gerais, Brazil. No trace of chlorpyrifos, endosulfan, cypermethrin or deltamethrin residues were found in either rump or liver samples. |
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Silva, Érica Pachecohttp://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4746300Y0Neves, Antônio Augustohttp://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4788868U1Queiroz, José Humberto dehttp://lattes.cnpq.br/4881556650652069Queiroz, Maria Eliana Lopes Ribeiro dehttp://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4781671U3Afonso, Robson José Cássia Francohttp://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4781403E2Mendonça, Regina Célia Santoshttp://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4790986E32015-03-26T13:00:12Z2009-07-032015-03-26T13:00:12Z2008-10-13SILVA, Érica Pacheco. Validation of method for extraction and pesticide multiresidue analysis in beef by gas chromatography. 2008. 119 f. Dissertação (Mestrado em Agroquímica analítica; Agroquímica inorgânica e Físico-química; Agroquímica orgânica) - Universidade Federal de Viçosa, Viçosa, 2008.http://locus.ufv.br/handle/123456789/2069The objective of this study was to optimize and validate the liquid-solid extraction with low-temperature purification (LSE- LTP) method for the analysis of chlorpyrifos, endosulfan, cypermethrin and deltamethrin pesticides residues in beef samples. Ideal conditions for the extraction of the pesticides of interest from the rump and liver cattle samples were determined by the employment of experimental planning to optimize the process. Sample mass, solvent extractor, ionic force, extraction time and agitation form were all evaluated. Rump and liver cattle samples were agitated with one-phase solvent mixtures and placed in a freezer for approximately 12 hours. The solids matrix and frozen aqueous phase were separated from the superior liquid phase. This superior phase was filtered and submitted to chromatography analysis using bifenthrin as an internal standard. The optimal technique consisted of supplementing 3.0000 g of beef with 1.0 mL of water, 6.5 mL of acetonitrile, 1.5 mL of ethyl acetate for the rump samples or 1.0 mL of water and 8.0 mL of acetonitrile for the liver samples, and submitting this mixture to ultrasound agitation for 10 minutes, followed by freezing. After separating the phases by freezing the aqueous phase, the supernatant liquid (10 mL) was removed and analyzed by gas chromatography with an electron capture detector. The clean up stage was evaluated for the liver extracts, however, during this stage, not only was the analysis time and cost increased, the percentage of analyte recovery diminished. With the intention of comparing the LSE-LTP with other techniques, the rump and liver samples were submitted to matrix solid phase dispersion (MSPD) extraction. However, this methodology presented recoveries inferior to those of the LSE-LTP in rump samples. For the liver samples, the MSPD technique showed to be little selective, presenting extracts less pure than those obtained by LSE-LTP, due to the greater extraction of matrix components. The optimized method was validated according to selectivity, linearity, detection limits and quantification of the method, precision and accuracy. The results showed that optimized LSE-LTP is efficient for the analysis of the pesticide residues of interest in rump and liver cattle with recovery percentages greater than 70 % and detection limits below the maximum residue limits (MRL) established by Codex Alimentarius the for these pesticides in the studied beef samples. This methodology also presents the small consumption of solvent and absence of purification steps of extracts before chromatography analysis. The effect of the matrix was found to be present in the quantification of pesticides by gas chromatography. To overcome these effects, calibration curves were prepared from organic extracts, obtained from rump and liver cattle free of contaminants. The optimized and validated technique was applied in beef samples acquired commercially in the city of Viçosa, Minas Gerais, Brazil. No trace of chlorpyrifos, endosulfan, cypermethrin or deltamethrin residues were found in either rump or liver samples.O objetivo deste trabalho foi otimizar e validar a técnica extração sólido-líquido com purificação em baixa temperatura (ESL-PBT) para análise de resíduos dos agrotóxicos clorpirifós, endosulfan, cipermetrina e deltametrina em amostras de carne bovina. Na etapa de otimização, as condições ideais para extração dos agrotóxicos de interesse de amostras de alcatra e fígado bovino fortificados, foram determinadas empregando planejamento experimental. Foram avaliados a massa de amostra, solvente extrator, força iônica, tempo de extração e de fortificação e forma de agitação. As amostras de alcatra e fígado bovino e a mistura extratora em fase única foram agitadas e deixadas em freezer por aproximadamente 12 horas. A matriz e a fase aquosa congeladas foram separadas da fase superior ainda líquida. A fase superior foi filtrada e submetida à análise cromatográfica utilizando bifentrina como padrão interno. A técnica otimizada consiste em acrescentar a 3,0000 g de carne bovina, 1,0 mL de água, 6,5 mL de acetonitrila, 1,5 mL de acetato de etila, para amostras de alcatra e 1,0 mL de água e 8,0 mL de acetonitrila para amostras de fígado bovino e submeter essa mistura a agitação por ultra-som durante 10 minutos seguida de congelamento. Após separação das fases pelo congelamento da fase aquosa o sobrenadante líquido (10 mL) foi removido e analisado por cromatografia gasosa com detector por captura de elétrons. Avaliou-se a etapa de clean up para os extratos de fígado bovino, porém, esta etapa, além de aumentar o tempo e o custo da análise, reduziu a porcentagem de recuperação dos analitos. Com o intuito de comparar a ESL- PBT com outras técnicas, submeteram-se as amostras de alcatra e fígado bovino à extração por dispersão de matriz em fase sólida (DMFS). Porém esta metodologia apresentou recuperações inferiores às obtidas pela ESL-PBT em amostras de alcatra. Para amostras de fígado, a técnica DMFS se mostrou pouco seletiva, apresentando extratos mais impuros do que os obtidos pela ESL-PBT, devido à maior extração de componentes da matriz. O método otimizado foi validado determinando-se a seletividade, linearidade, limites detecção e quantificação do método, precisão e exatidão. Os resultados mostraram que a ESL-PBT otimizada é eficiente para análise de resíduos dos agrotóxicos de interesse em alcatra e fígado bovino com porcentagens de recuperação superior a 70 % e limites de detecção abaixo dos limites máximos de resíduos (LMR) estabelecidos pelo Codex Alimentarius para estes pesticidas neste tipo de alimento. Além disso, a metodologia apresenta um pequeno consumo de solvente e ausência de etapas de purificação dos extratos antes da análise cromatográfica. O efeito de matriz mostrou- se presente na quantificação dos pesticidas por cromatografia gasosa. Para contornar esse efeito curvas de calibração foram preparadas em extratos orgânicos, obtidos da extração de alcatra e fígado bovino isento dos contaminantes. A técnica otimizada e validada foi aplicada em amostras de carne bovina adquiridas no comércio da cidade de Viçosa-MG, não sendo detectada a presença de resíduos de clorpirifós, endosulfan, cipermetrina e deltametrina nas amostras de alcatra e fígado analisadas.Conselho Nacional de Desenvolvimento Científico e Tecnológicoapplication/pdfporUniversidade Federal de ViçosaMestrado em AgroquímicaUFVBRAgroquímica analítica; Agroquímica inorgânica e Físico-química; Agroquímica orgânicaAnálise de resíduosAgrotóxicosCarne bovinaCromatografia gasosaResidue analysisPesticidesBeefGas chomatographyCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA::QUIMICA ANALITICAValidação de método de extração e análise multirresíduo de agrotóxicos em carne bovina por cromatografia gasosaValidation of method for extraction and pesticide multiresidue analysis in beef by gas chromatographyinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisinfo:eu-repo/semantics/openAccessreponame:LOCUS Repositório Institucional da UFVinstname:Universidade Federal de Viçosa (UFV)instacron:UFVORIGINALtexto completo.pdfapplication/pdf970850https://locus.ufv.br//bitstream/123456789/2069/1/texto%20completo.pdf6cd375e77f84140769d12f1f235f3989MD51TEXTtexto completo.pdf.txttexto completo.pdf.txtExtracted texttext/plain192812https://locus.ufv.br//bitstream/123456789/2069/2/texto%20completo.pdf.txte743539aa8ee6d1fdfbf985ce2866759MD52THUMBNAILtexto completo.pdf.jpgtexto completo.pdf.jpgIM Thumbnailimage/jpeg3919https://locus.ufv.br//bitstream/123456789/2069/3/texto%20completo.pdf.jpg696420fadf3c7f9a891ae51eeef8f97fMD53123456789/20692017-04-19 12:34:19.969oai:locus.ufv.br:123456789/2069Repositório InstitucionalPUBhttps://www.locus.ufv.br/oai/requestfabiojreis@ufv.bropendoar:21452017-04-19T15:34:19LOCUS Repositório Institucional da UFV - Universidade Federal de Viçosa (UFV)false |
dc.title.por.fl_str_mv |
Validação de método de extração e análise multirresíduo de agrotóxicos em carne bovina por cromatografia gasosa |
dc.title.alternative.eng.fl_str_mv |
Validation of method for extraction and pesticide multiresidue analysis in beef by gas chromatography |
title |
Validação de método de extração e análise multirresíduo de agrotóxicos em carne bovina por cromatografia gasosa |
spellingShingle |
Validação de método de extração e análise multirresíduo de agrotóxicos em carne bovina por cromatografia gasosa Silva, Érica Pacheco Análise de resíduos Agrotóxicos Carne bovina Cromatografia gasosa Residue analysis Pesticides Beef Gas chomatography CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA::QUIMICA ANALITICA |
title_short |
Validação de método de extração e análise multirresíduo de agrotóxicos em carne bovina por cromatografia gasosa |
title_full |
Validação de método de extração e análise multirresíduo de agrotóxicos em carne bovina por cromatografia gasosa |
title_fullStr |
Validação de método de extração e análise multirresíduo de agrotóxicos em carne bovina por cromatografia gasosa |
title_full_unstemmed |
Validação de método de extração e análise multirresíduo de agrotóxicos em carne bovina por cromatografia gasosa |
title_sort |
Validação de método de extração e análise multirresíduo de agrotóxicos em carne bovina por cromatografia gasosa |
author |
Silva, Érica Pacheco |
author_facet |
Silva, Érica Pacheco |
author_role |
author |
dc.contributor.authorLattes.por.fl_str_mv |
http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4746300Y0 |
dc.contributor.author.fl_str_mv |
Silva, Érica Pacheco |
dc.contributor.advisor-co1.fl_str_mv |
Neves, Antônio Augusto |
dc.contributor.advisor-co1Lattes.fl_str_mv |
http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4788868U1 |
dc.contributor.advisor-co2.fl_str_mv |
Queiroz, José Humberto de |
dc.contributor.advisor-co2Lattes.fl_str_mv |
http://lattes.cnpq.br/4881556650652069 |
dc.contributor.advisor1.fl_str_mv |
Queiroz, Maria Eliana Lopes Ribeiro de |
dc.contributor.advisor1Lattes.fl_str_mv |
http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4781671U3 |
dc.contributor.referee1.fl_str_mv |
Afonso, Robson José Cássia Franco |
dc.contributor.referee1Lattes.fl_str_mv |
http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4781403E2 |
dc.contributor.referee2.fl_str_mv |
Mendonça, Regina Célia Santos |
dc.contributor.referee2Lattes.fl_str_mv |
http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4790986E3 |
contributor_str_mv |
Neves, Antônio Augusto Queiroz, José Humberto de Queiroz, Maria Eliana Lopes Ribeiro de Afonso, Robson José Cássia Franco Mendonça, Regina Célia Santos |
dc.subject.por.fl_str_mv |
Análise de resíduos Agrotóxicos Carne bovina Cromatografia gasosa |
topic |
Análise de resíduos Agrotóxicos Carne bovina Cromatografia gasosa Residue analysis Pesticides Beef Gas chomatography CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA::QUIMICA ANALITICA |
dc.subject.eng.fl_str_mv |
Residue analysis Pesticides Beef Gas chomatography |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA::QUIMICA ANALITICA |
description |
The objective of this study was to optimize and validate the liquid-solid extraction with low-temperature purification (LSE- LTP) method for the analysis of chlorpyrifos, endosulfan, cypermethrin and deltamethrin pesticides residues in beef samples. Ideal conditions for the extraction of the pesticides of interest from the rump and liver cattle samples were determined by the employment of experimental planning to optimize the process. Sample mass, solvent extractor, ionic force, extraction time and agitation form were all evaluated. Rump and liver cattle samples were agitated with one-phase solvent mixtures and placed in a freezer for approximately 12 hours. The solids matrix and frozen aqueous phase were separated from the superior liquid phase. This superior phase was filtered and submitted to chromatography analysis using bifenthrin as an internal standard. The optimal technique consisted of supplementing 3.0000 g of beef with 1.0 mL of water, 6.5 mL of acetonitrile, 1.5 mL of ethyl acetate for the rump samples or 1.0 mL of water and 8.0 mL of acetonitrile for the liver samples, and submitting this mixture to ultrasound agitation for 10 minutes, followed by freezing. After separating the phases by freezing the aqueous phase, the supernatant liquid (10 mL) was removed and analyzed by gas chromatography with an electron capture detector. The clean up stage was evaluated for the liver extracts, however, during this stage, not only was the analysis time and cost increased, the percentage of analyte recovery diminished. With the intention of comparing the LSE-LTP with other techniques, the rump and liver samples were submitted to matrix solid phase dispersion (MSPD) extraction. However, this methodology presented recoveries inferior to those of the LSE-LTP in rump samples. For the liver samples, the MSPD technique showed to be little selective, presenting extracts less pure than those obtained by LSE-LTP, due to the greater extraction of matrix components. The optimized method was validated according to selectivity, linearity, detection limits and quantification of the method, precision and accuracy. The results showed that optimized LSE-LTP is efficient for the analysis of the pesticide residues of interest in rump and liver cattle with recovery percentages greater than 70 % and detection limits below the maximum residue limits (MRL) established by Codex Alimentarius the for these pesticides in the studied beef samples. This methodology also presents the small consumption of solvent and absence of purification steps of extracts before chromatography analysis. The effect of the matrix was found to be present in the quantification of pesticides by gas chromatography. To overcome these effects, calibration curves were prepared from organic extracts, obtained from rump and liver cattle free of contaminants. The optimized and validated technique was applied in beef samples acquired commercially in the city of Viçosa, Minas Gerais, Brazil. No trace of chlorpyrifos, endosulfan, cypermethrin or deltamethrin residues were found in either rump or liver samples. |
publishDate |
2008 |
dc.date.issued.fl_str_mv |
2008-10-13 |
dc.date.available.fl_str_mv |
2009-07-03 2015-03-26T13:00:12Z |
dc.date.accessioned.fl_str_mv |
2015-03-26T13:00:12Z |
dc.type.status.fl_str_mv |
info:eu-repo/semantics/publishedVersion |
dc.type.driver.fl_str_mv |
info:eu-repo/semantics/masterThesis |
format |
masterThesis |
status_str |
publishedVersion |
dc.identifier.citation.fl_str_mv |
SILVA, Érica Pacheco. Validation of method for extraction and pesticide multiresidue analysis in beef by gas chromatography. 2008. 119 f. Dissertação (Mestrado em Agroquímica analítica; Agroquímica inorgânica e Físico-química; Agroquímica orgânica) - Universidade Federal de Viçosa, Viçosa, 2008. |
dc.identifier.uri.fl_str_mv |
http://locus.ufv.br/handle/123456789/2069 |
identifier_str_mv |
SILVA, Érica Pacheco. Validation of method for extraction and pesticide multiresidue analysis in beef by gas chromatography. 2008. 119 f. Dissertação (Mestrado em Agroquímica analítica; Agroquímica inorgânica e Físico-química; Agroquímica orgânica) - Universidade Federal de Viçosa, Viçosa, 2008. |
url |
http://locus.ufv.br/handle/123456789/2069 |
dc.language.iso.fl_str_mv |
por |
language |
por |
dc.rights.driver.fl_str_mv |
info:eu-repo/semantics/openAccess |
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openAccess |
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application/pdf |
dc.publisher.none.fl_str_mv |
Universidade Federal de Viçosa |
dc.publisher.program.fl_str_mv |
Mestrado em Agroquímica |
dc.publisher.initials.fl_str_mv |
UFV |
dc.publisher.country.fl_str_mv |
BR |
dc.publisher.department.fl_str_mv |
Agroquímica analítica; Agroquímica inorgânica e Físico-química; Agroquímica orgânica |
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Universidade Federal de Viçosa |
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LOCUS Repositório Institucional da UFV |
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