Otimização de método analítico para determinação do inseticida bifentrina em amostras de alimentos industrializados

Detalhes bibliográficos
Ano de defesa: 2018
Autor(a) principal: SOARES, Thaynara Ferreira lattes
Orientador(a): NUNES, Gilvanda Silva lattes
Banca de defesa: VILLIS, Paulo Cesar Mendes lattes, ROCHA, Cláudia Quintino da lattes
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.
id UFMA_0b8ab234f3ead9051c909b4e72b9a640
oai_identifier_str oai:tede2:tede/2230
network_acronym_str UFMA
network_name_str Biblioteca Digital de Teses e Dissertações da UFMA
repository_id_str
spelling 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: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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
dc.language.iso.fl_str_mv por
language por
dc.rights.driver.fl_str_mv info:eu-repo/semantics/openAccess
eu_rights_str_mv openAccess
dc.format.none.fl_str_mv application/pdf
dc.publisher.none.fl_str_mv 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
dc.source.none.fl_str_mv reponame:Biblioteca Digital de Teses e Dissertações da UFMA
instname:Universidade Federal do Maranhão (UFMA)
instacron:UFMA
instname_str Universidade Federal do Maranhão (UFMA)
instacron_str UFMA
institution UFMA
reponame_str Biblioteca Digital de Teses e Dissertações da UFMA
collection Biblioteca Digital de Teses e Dissertações da UFMA
bitstream.url.fl_str_mv http://tedebc.ufma.br:8080/bitstream/tede/2230/2/ThaynaraSoares.pdf
http://tedebc.ufma.br:8080/bitstream/tede/2230/1/license.txt
bitstream.checksum.fl_str_mv 67a7c70215a187ee5331509e8b456c27
97eeade1fce43278e63fe063657f8083
bitstream.checksumAlgorithm.fl_str_mv MD5
MD5
repository.name.fl_str_mv Biblioteca Digital de Teses e Dissertações da UFMA - Universidade Federal do Maranhão (UFMA)
repository.mail.fl_str_mv repositorio@ufma.br||repositorio@ufma.br
_version_ 1797055609530482688