Otimização de método analítico para determinação do inseticida bifentrina em amostras de alimentos industrializados
Ano de defesa: | 2018 |
---|---|
Autor(a) principal: | |
Orientador(a): | |
Banca de defesa: | , |
Tipo de documento: | Dissertação |
Tipo de acesso: | Acesso aberto |
Idioma: | por |
Instituição de defesa: |
Universidade Federal do Maranhão
|
Programa de Pós-Graduação: |
PROGRAMA DE PÓS-GRADUAÇÃO EM QUÍMICA/CCET
|
Departamento: |
DEPARTAMENTO DE TECNOLOGIA QUÍMICA/CCET
|
País: |
Brasil
|
Palavras-chave em Português: | |
Área do conhecimento CNPq: | |
Link de acesso: | https://tedebc.ufma.br/jspui/handle/tede/tede/2230 |
Resumo: | The bifenthrin pyrethroid insecticide has been widely used for pest control, not only in crops, but also in industrial settings and commercial establishments. If integrated pest control is not performed properly, there is a risk of contamination of shelf products. The objective of this work was to develop and compare two analytical methods based on gas chromatography with electron capture detection (GC/ECD) and high performance liquid chromatography coupled todiode array detector (HPLC/DAD), for determination of bifenthrin insecticide in samples of industrialized foods with varied compositions and characteristics. After optimization of the separation by HPLC/DAD and CG/ECD, representative samples of the whole sample (high moisture content/low lipid content and low moisture content/high lipid content) were submitted to numerous tests in order to optimize the analytical conditions. Thus, the conditions for the microwave extraction and clean up through using solid phase extraction (EFS) in activated Florisil column were optimized. Then, the previously optimized methods were evaluated by comparing the following figures of merit: linearity, sensitivity, accuracy and precision. For both methods, adequate selectivity and high accuracy were observed, with recoveries ranging from 86.4 to 101.1% and from 99.5 to 90% for CLAE/DAD and CG/ECD, respectively. Coefficients of variation <5% evidenced high precision for both methods. Regarding sensitivity, however, the method based on CG/ECDwas more efficient, with LD and LQ values of 2.1 ng/L and 7.1 ng/L, respectively, whereas the method based on HPLC/DAD presented values of LD and LQ of 7.4 ng/L and 24.5 ng/L, respectively. Thus, the method based on the CG/ECD technique was selected to analyze 22 samples of supposedly contaminated foodstuffs as well as some of the packages. The results evidenced the absence of contamination in the samples, being the analytical methodology considered adequate for routine analysis of complex samples, since it presented high efficiency, quickness and relatively low cost. |
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NUNES, Gilvanda Silva279.288.533-53http://lattes.cnpq.br/5833210771020427VILLIS, Paulo Cesar Mendeshttp://lattes.cnpq.br/7997037826193766ROCHA, Cláudia Quintino dahttp://lattes.cnpq.br/5609489233382242039.272.013-24http://lattes.cnpq.br/8218567050633495SOARES, Thaynara Ferreira2018-05-16T20:21:15Z2018-03-16SOARES, Thaynara Ferreira. Otimização de método analítico para determinação do inseticida bifentrina em amostras de alimentos industrializados. 2018. 81 f. Dissertação (Dissertação em Química) - Universidade Federal do Maranhão, São Luís, 2018.https://tedebc.ufma.br/jspui/handle/tede/tede/2230The bifenthrin pyrethroid insecticide has been widely used for pest control, not only in crops, but also in industrial settings and commercial establishments. If integrated pest control is not performed properly, there is a risk of contamination of shelf products. The objective of this work was to develop and compare two analytical methods based on gas chromatography with electron capture detection (GC/ECD) and high performance liquid chromatography coupled todiode array detector (HPLC/DAD), for determination of bifenthrin insecticide in samples of industrialized foods with varied compositions and characteristics. After optimization of the separation by HPLC/DAD and CG/ECD, representative samples of the whole sample (high moisture content/low lipid content and low moisture content/high lipid content) were submitted to numerous tests in order to optimize the analytical conditions. Thus, the conditions for the microwave extraction and clean up through using solid phase extraction (EFS) in activated Florisil column were optimized. Then, the previously optimized methods were evaluated by comparing the following figures of merit: linearity, sensitivity, accuracy and precision. For both methods, adequate selectivity and high accuracy were observed, with recoveries ranging from 86.4 to 101.1% and from 99.5 to 90% for CLAE/DAD and CG/ECD, respectively. Coefficients of variation <5% evidenced high precision for both methods. Regarding sensitivity, however, the method based on CG/ECDwas more efficient, with LD and LQ values of 2.1 ng/L and 7.1 ng/L, respectively, whereas the method based on HPLC/DAD presented values of LD and LQ of 7.4 ng/L and 24.5 ng/L, respectively. Thus, the method based on the CG/ECD technique was selected to analyze 22 samples of supposedly contaminated foodstuffs as well as some of the packages. The results evidenced the absence of contamination in the samples, being the analytical methodology considered adequate for routine analysis of complex samples, since it presented high efficiency, quickness and relatively low cost.O inseticida piretróide bifentrina tem sido amplamente usado para controle de pragas, não só nas lavouras, como também em ambientes industriais e em estabelecimentos comerciais. Se o controle integrado de pragas não for realizado adequadamente, existe o risco de contaminação dos produtos de prateleira. O objetivo desse trabalho foi desenvolver e comparar dois métodos analíticos, baseados na cromatografia a gás com detecção por captura de elétrons (CG/DCE) e na cromatografia a líquido de alta eficiência com detecção por arranjos de fotodiodos (CLAE/DAD), para determinação do inseticida bifentrina em amostras de alimentos industrializados com variadas composições e características. Após otimização da separação por CLAE/DAD e CG/DCE, amostras de alimentos representativas do todo amostral (elevado teor de umidade/baixo teor de lipídeos e baixo teor de umidade/elevado teor de lipídeos) foram submetidas a testes para otimização das condições analíticas. Assim, foram variadas as condições para as etapas de extração em forno microondas e de clean up empregando extração em fase sólida (EFS) em coluna de Florisil ativado. Depois, procedeu-se à avaliação dos métodos previamente otimizados, mediante comparação das seguintes figuras de mérito: linearidade, sensibilidade, exatidão e precisão. Para ambos os métodos, foi constatada adequada seletividade e elevada exatidão, com índices de recuperações nas faixas de 86,4-101,1% e de 99,5-90% para CLAE/DAD e para CG/DCE, respectivamente. Os coeficientes de variação abaixo de 5% evidenciaram elevada precisão para ambos os métodos. Em relação à sensibilidade, porém, o método baseado na técnica CG/DCE mostrou-se mais eficiente, com valores de LD e LQ de 2,1 ng/L e 7,1 ng/L, respectivamente, enquanto que o método baseado em CLAE/DAD apresentou valores de LD e LQ de 7,4ng/L e 24,5ng/L, respectivamente. Com isso, o método baseado na técnica CG/DCE foi selecionado para analisar 22 amostras de alimentos industrializados, supostamente contaminados com o pesticida bifentrina, bem como algumas das embalagens. Os resultados evidenciaram ausência de contaminação nos alimentos tomados para análise, tendo sido a metodologia analítica considerada adequada para análise de rotina de amostras complexas, por sua elevada eficiência e rapidez, e custo relativamente baixo.Submitted by Rosivalda Pereira (mrs.pereira@ufma.br) on 2018-05-16T20:21:15Z No. of bitstreams: 1 ThaynaraSoares.pdf: 1627425 bytes, checksum: 67a7c70215a187ee5331509e8b456c27 (MD5)Made available in DSpace on 2018-05-16T20:21:15Z (GMT). No. of bitstreams: 1 ThaynaraSoares.pdf: 1627425 bytes, checksum: 67a7c70215a187ee5331509e8b456c27 (MD5) Previous issue date: 2018-03-16CNPqapplication/pdfporUniversidade Federal do MaranhãoPROGRAMA DE PÓS-GRADUAÇÃO EM QUÍMICA/CCETUFMABrasilDEPARTAMENTO DE TECNOLOGIA QUÍMICA/CCETAlimentos industrializadosBifentrinaMétodo analíticoIndustrialized foodsBifenthrinAnalytical methodQuímica AnalíticaOtimização de método analítico para determinação do inseticida bifentrina em amostras de alimentos industrializadosOptimization of analytical method for determination of bifenthrin insecticide in samples of industrialized foodsinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisinfo:eu-repo/semantics/openAccessreponame:Biblioteca Digital de Teses e Dissertações da UFMAinstname:Universidade Federal do Maranhão (UFMA)instacron:UFMAORIGINALThaynaraSoares.pdfThaynaraSoares.pdfapplication/pdf1627425http://tedebc.ufma.br:8080/bitstream/tede/2230/2/ThaynaraSoares.pdf67a7c70215a187ee5331509e8b456c27MD52LICENSElicense.txtlicense.txttext/plain; charset=utf-82255http://tedebc.ufma.br:8080/bitstream/tede/2230/1/license.txt97eeade1fce43278e63fe063657f8083MD51tede/22302018-05-16 17:21:15.897oai:tede2:tede/2230IExJQ0VOw4dBIERFIERJU1RSSUJVScOHw4NPIE7Dg08tRVhDTFVTSVZBCgpDb20gYSBhcHJlc2VudGHDp8OjbyBkZXN0YSBsaWNlbsOnYSxvIGF1dG9yIChlcykgb3UgbyB0aXR1bGFyIGRvcyBkaXJlaXRvcyBkZSBhdXRvciBjb25jZWRlIMOgIFVuaXZlcnNpZGFkZSBGZWRlcmFsIGRvIE1hcmFuaMOjbyAoVUZNQSkgbyBkaXJlaXRvIG7Do28tZXhjbHVzaXZvIGRlIHJlcHJvZHV6aXIsIHRyYWR1emlyIChjb25mb3JtZSBkZWZpbmlkbyBhYmFpeG8pLCBlL291IGRpc3RyaWJ1aXIgYSBzdWEgdGVzZSBvdSBkaXNzZXJ0YcOnw6NvIChpbmNsdWluZG8gbyByZXN1bW8pIHBvciB0b2RvIG8gbXVuZG8gbm8gZm9ybWF0byBpbXByZXNzbyBlIGVsZXRyw7RuaWNvIGUgZW0gcXVhbHF1ZXIgbWVpbywgaW5jbHVpbmRvIG9zIGZvcm1hdG9zIMOhdWRpbyBvdSB2w61kZW8uCgpWb2PDqiBjb25jb3JkYSBxdWUgYSBVRk1BIHBvZGUsIHNlbSBhbHRlcmFyIG8gY29udGXDumRvLCB0cmFuc3BvciBhIHN1YSB0ZXNlIG91IGRpc3NlcnRhw6fDo28gcGFyYSBxdWFscXVlciBtZWlvIG91IGZvcm1hdG8gcGFyYSBmaW5zIGRlIHByZXNlcnZhw6fDo28uCgpWb2PDqiB0YW1iw6ltIGNvbmNvcmRhIHF1ZSBhIFVGTUEgcG9kZSBtYW50ZXIgbWFpcyBkZSB1bWEgY8OzcGlhIGRlIHN1YSB0ZXNlIG91IGRpc3NlcnRhw6fDo28gcGFyYSBmaW5zIGRlIHNlZ3VyYW7Dp2EsIGJhY2stdXAgZSBwcmVzZXJ2YcOnw6NvLgoKVm9jw6ogZGVjbGFyYSBxdWUgYSBzdWEgdGVzZSBvdSBkaXNzZXJ0YcOnw6NvIMOpIG9yaWdpbmFsIGUgcXVlIHZvY8OqIHRlbSBvIHBvZGVyIGRlIGNvbmNlZGVyIG9zIGRpcmVpdG9zIGNvbnRpZG9zIG5lc3RhIGxpY2Vuw6dhLiBWb2PDqiB0YW1iw6ltIGRlY2xhcmEgcXVlIG8gZGVww7NzaXRvIGRhIHN1YSB0ZXNlIG91IGRpc3NlcnRhw6fDo28gbsOjbywgcXVlIHNlamEgZGUgc2V1IGNvbmhlY2ltZW50bywgaW5mcmluZ2UgZGlyZWl0b3MgYXV0b3JhaXMgZGUgbmluZ3XDqW0uCgpDYXNvIGEgc3VhIHRlc2Ugb3UgZGlzc2VydGHDp8OjbyBjb250ZW5oYSBtYXRlcmlhbCBxdWUgdm9jw6ogbsOjbyBwb3NzdWkgYSB0aXR1bGFyaWRhZGUgZG9zIGRpcmVpdG9zIGF1dG9yYWlzLCB2b2PDqiBkZWNsYXJhIHF1ZSBvYnRldmUgYSBwZXJtaXNzw6NvIGlycmVzdHJpdGEgZG8gZGV0ZW50b3IgZG9zIGRpcmVpdG9zIGF1dG9yYWlzIHBhcmEgY29uY2VkZXIgw6AgVUZNQSBvcyBkaXJlaXRvcyBhcHJlc2VudGFkb3MgbmVzdGEgbGljZW7Dp2EsIGUgcXVlIGVzc2UgbWF0ZXJpYWwgZGUgcHJvcHJpZWRhZGUgZGUgdGVyY2Vpcm9zIGVzdMOhIGNsYXJhbWVudGUgaWRlbnRpZmljYWRvIGUgcmVjb25oZWNpZG8gbm8gdGV4dG8gb3Ugbm8gY29udGXDumRvIGRhIHRlc2Ugb3UgZGlzc2VydGHDp8OjbyBvcmEgZGVwb3NpdGFkYS4KCkNBU08gQSBURVNFIE9VIERJU1NFUlRBw4fDg08gT1JBIERFUE9TSVRBREEgVEVOSEEgU0lETyBSRVNVTFRBRE8gREUgVU0gUEFUUk9Dw41OSU8gT1UgQVBPSU8gREUgVU1BIEFHw4pOQ0lBIERFIEZPTUVOVE8gT1UgT1VUUk8gT1JHQU5JU01PIFFVRSBOw4NPIFNFSkEgQSBVRk1BLCBWT0PDiiBERUNMQVJBIFFVRSBSRVNQRUlUT1UgVE9ET1MgRSBRVUFJU1FVRVIgRElSRUlUT1MgREUgUkVWSVPDg08gQ09NTyBUQU1Cw4lNIEFTIERFTUFJUyBPQlJJR0HDh8OVRVMgRVhJR0lEQVMgUE9SIENPTlRSQVRPIE9VIEFDT1JETy4KCkEgVUZNQSBzZSBjb21wcm9tZXRlIGEgaWRlbnRpZmljYXIgY2xhcmFtZW50ZSBvIHNldSBub21lIG91IG8ocykgbm9tZShzKSBkbyhzKSBkZXRlbnRvcihlcykgZG9zIGRpcmVpdG9zIGF1dG9yYWlzIGRhIHRlc2Ugb3UgZGlzc2VydGHDp8OjbywgZSBuw6NvIGZhcsOhIHF1YWxxdWVyIGFsdGVyYcOnw6NvLCBhbMOpbSBkYXF1ZWxhcyBjb25jZWRpZGFzIHBvciBlc3RhIGxpY2Vuw6dhLgoKRGVjbGFyYSB0YW1iw6ltIHF1ZSB0b2RhcyBhcyBhZmlsaWHDp8O1ZXMgY29ycG9yYXRpdmFzIG91IGluc3RpdHVjaW9uYWlzIGUgdG9kYXMgYXMgZm9udGVzIGRlIGFwb2lvIGZpbmFuY2Vpcm8gYW8gdHJhYmFsaG8gZXN0w6NvIGRldmlkYW1lbnRlIGNpdGFkYXMgb3UgbWVuY2lvbmFkYXMgZSBjZXJ0aWZpY2EgcXVlIG7Do28gaMOhIG5lbmh1bSBpbnRlcmVzc2UgY29tZXJjaWFsIG91IGFzc29jaWF0aXZvIHF1ZSByZXByZXNlbnRlIGNvbmZsaXRvIGRlIGludGVyZXNzZSBlbSBjb25leMOjbyBjb20gbyB0cmFiYWxobyBzdWJtZXRpZG8uCgoKCgoKCgo=Biblioteca Digital de Teses e Dissertaçõeshttps://tedebc.ufma.br/jspui/PUBhttp://tedebc.ufma.br:8080/oai/requestrepositorio@ufma.br||repositorio@ufma.bropendoar:21312018-05-16T20:21:15Biblioteca Digital de Teses e Dissertações da UFMA - Universidade Federal do Maranhão (UFMA)false |
dc.title.por.fl_str_mv |
Otimização de método analítico para determinação do inseticida bifentrina em amostras de alimentos industrializados |
dc.title.alternative.eng.fl_str_mv |
Optimization of analytical method for determination of bifenthrin insecticide in samples of industrialized foods |
title |
Otimização de método analítico para determinação do inseticida bifentrina em amostras de alimentos industrializados |
spellingShingle |
Otimização de método analítico para determinação do inseticida bifentrina em amostras de alimentos industrializados SOARES, Thaynara Ferreira Alimentos industrializados Bifentrina Método analítico Industrialized foods Bifenthrin Analytical method Química Analítica |
title_short |
Otimização de método analítico para determinação do inseticida bifentrina em amostras de alimentos industrializados |
title_full |
Otimização de método analítico para determinação do inseticida bifentrina em amostras de alimentos industrializados |
title_fullStr |
Otimização de método analítico para determinação do inseticida bifentrina em amostras de alimentos industrializados |
title_full_unstemmed |
Otimização de método analítico para determinação do inseticida bifentrina em amostras de alimentos industrializados |
title_sort |
Otimização de método analítico para determinação do inseticida bifentrina em amostras de alimentos industrializados |
author |
SOARES, Thaynara Ferreira |
author_facet |
SOARES, Thaynara Ferreira |
author_role |
author |
dc.contributor.advisor1.fl_str_mv |
NUNES, Gilvanda Silva |
dc.contributor.advisor1ID.fl_str_mv |
279.288.533-53 |
dc.contributor.advisor1Lattes.fl_str_mv |
http://lattes.cnpq.br/5833210771020427 |
dc.contributor.referee1.fl_str_mv |
VILLIS, Paulo Cesar Mendes |
dc.contributor.referee1Lattes.fl_str_mv |
http://lattes.cnpq.br/7997037826193766 |
dc.contributor.referee2.fl_str_mv |
ROCHA, Cláudia Quintino da |
dc.contributor.referee2Lattes.fl_str_mv |
http://lattes.cnpq.br/5609489233382242 |
dc.contributor.authorID.fl_str_mv |
039.272.013-24 |
dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/8218567050633495 |
dc.contributor.author.fl_str_mv |
SOARES, Thaynara Ferreira |
contributor_str_mv |
NUNES, Gilvanda Silva VILLIS, Paulo Cesar Mendes ROCHA, Cláudia Quintino da |
dc.subject.por.fl_str_mv |
Alimentos industrializados Bifentrina Método analítico Industrialized foods Bifenthrin Analytical method |
topic |
Alimentos industrializados Bifentrina Método analítico Industrialized foods Bifenthrin Analytical method Química Analítica |
dc.subject.cnpq.fl_str_mv |
Química Analítica |
description |
The bifenthrin pyrethroid insecticide has been widely used for pest control, not only in crops, but also in industrial settings and commercial establishments. If integrated pest control is not performed properly, there is a risk of contamination of shelf products. The objective of this work was to develop and compare two analytical methods based on gas chromatography with electron capture detection (GC/ECD) and high performance liquid chromatography coupled todiode array detector (HPLC/DAD), for determination of bifenthrin insecticide in samples of industrialized foods with varied compositions and characteristics. After optimization of the separation by HPLC/DAD and CG/ECD, representative samples of the whole sample (high moisture content/low lipid content and low moisture content/high lipid content) were submitted to numerous tests in order to optimize the analytical conditions. Thus, the conditions for the microwave extraction and clean up through using solid phase extraction (EFS) in activated Florisil column were optimized. Then, the previously optimized methods were evaluated by comparing the following figures of merit: linearity, sensitivity, accuracy and precision. For both methods, adequate selectivity and high accuracy were observed, with recoveries ranging from 86.4 to 101.1% and from 99.5 to 90% for CLAE/DAD and CG/ECD, respectively. Coefficients of variation <5% evidenced high precision for both methods. Regarding sensitivity, however, the method based on CG/ECDwas more efficient, with LD and LQ values of 2.1 ng/L and 7.1 ng/L, respectively, whereas the method based on HPLC/DAD presented values of LD and LQ of 7.4 ng/L and 24.5 ng/L, respectively. Thus, the method based on the CG/ECD technique was selected to analyze 22 samples of supposedly contaminated foodstuffs as well as some of the packages. The results evidenced the absence of contamination in the samples, being the analytical methodology considered adequate for routine analysis of complex samples, since it presented high efficiency, quickness and relatively low cost. |
publishDate |
2018 |
dc.date.accessioned.fl_str_mv |
2018-05-16T20:21:15Z |
dc.date.issued.fl_str_mv |
2018-03-16 |
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 |
SOARES, Thaynara Ferreira. Otimização de método analítico para determinação do inseticida bifentrina em amostras de alimentos industrializados. 2018. 81 f. Dissertação (Dissertação em Química) - Universidade Federal do Maranhão, São Luís, 2018. |
dc.identifier.uri.fl_str_mv |
https://tedebc.ufma.br/jspui/handle/tede/tede/2230 |
identifier_str_mv |
SOARES, Thaynara Ferreira. Otimização de método analítico para determinação do inseticida bifentrina em amostras de alimentos industrializados. 2018. 81 f. Dissertação (Dissertação em Química) - Universidade Federal do Maranhão, São Luís, 2018. |
url |
https://tedebc.ufma.br/jspui/handle/tede/tede/2230 |
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por |
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por |
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info:eu-repo/semantics/openAccess |
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openAccess |
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application/pdf |
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Universidade Federal do Maranhão |
dc.publisher.program.fl_str_mv |
PROGRAMA DE PÓS-GRADUAÇÃO EM QUÍMICA/CCET |
dc.publisher.initials.fl_str_mv |
UFMA |
dc.publisher.country.fl_str_mv |
Brasil |
dc.publisher.department.fl_str_mv |
DEPARTAMENTO DE TECNOLOGIA QUÍMICA/CCET |
publisher.none.fl_str_mv |
Universidade Federal do Maranhão |
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