Otimização e validação de metodologia para determinação de aldicarbe e carbofurano em amostras de café bebida

Detalhes bibliográficos
Autor(a) principal: Alves, Renata Domingos
Data de Publicação: 2010
Tipo de documento: Dissertação
Idioma: por
Título da fonte: LOCUS Repositório Institucional da UFV
Texto Completo: http://locus.ufv.br/handle/123456789/2090
Resumo: Domestic use of aldicarb and carbofuran has resulted in accidental or even intentional poisonings, making it a severe public health problem. A mixture of "chumbinho" (aldicarb) in coffee is frequently a poisoning agent due to strong odor and color of coffee which hide the presende of "chumbinho". Thus, the objective of this study was to adapt, optimize and validate a liquid-liquid extraction technique with low temperature partitioning (LLE-LTP) for determination of aldicarb and carbofuran in coffee by high performance liquid chromatography (HPLC-UV), aiming to make the technique available for poisoning cases of forensic and agrarian interest. Preliminary tests were performed on optimization of the method for the evaluation of variables from extraction of pesticides such as: solvent extractor, volume of the sample and solvent extractor, pH of the sample, ionic force, homogenization mode and times of agitation, fortification and partitioning. Later, a complete 22 factorial scheme was used for evaluation of the simultaneous behavior of NaCl concentration in the sample (0% or 3% w/v) and pH of the sample (3.0 or 5.5) on extraction efficiency of the carbamates. The optimized method consisted of adding 2.0 mL of the coffee sample (8% w/v) and 4.0 mL of acetonitrile, verifying the formation of a single phase. This mixture is then agitated on a table agitator (5 minutes) and placed in a freezer at -20°C for 3 hours. Under these conditions the phases are separated and the organic extract which contains the active principles which is recovered and analyzed by HPLC, employing water and acetonitrile as the mobile phase (65:35). The optimized technique was validated, determining the principle figures of merit, including: selectivity, detection and quantification limits and linearity. Effect of the matrix on quantification of these active principles by HPLC was also evaluated. The results indicated that the LLE-LTP method is efficient for extraction of the two pesticides in coffee samples, showing recovery percentages greater than 94%. Detection and quantification limits of the method were 0.54 and 1.80 mg L-1 respectively for aldicarb and 0.28 and 0.92 mg L-1 for carbofuran. The effect of the matrix showed to be present on quantification of the pesticides by liquid chromatography. In the study of the stability of these active principles, it was observed that of the three factors analyzed, storage temperature of the samples was the factor that most affected degradation of the carbamates. At room temperature, fungi growth as wellas greater degradation of the composts was observed after 5 days. Therefore, optimization of the LLE-LTP method for extraction of pesticide residues from coffee samples and analysis by HPLC resulted in a simple and effective method, with little consumption of solvent, high analytical frequency and low cost.
id UFV_470ccde0f07a79c00a1b620e9058e0e8
oai_identifier_str oai:locus.ufv.br:123456789/2090
network_acronym_str UFV
network_name_str LOCUS Repositório Institucional da UFV
repository_id_str 2145
spelling Alves, Renata Domingoshttp://lattes.cnpq.br/0515651682967753Neves, Antônio Augustohttp://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4788868U1Zambolim, Laérciohttp://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4787254T6Queiroz, Maria Eliana Lopes Ribeiro dehttp://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4781671U3Reis, Efraim Lázarohttp://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4788214H7Paula, Washington Xavier dehttp://lattes.cnpq.br/79591816971217522015-03-26T13:00:17Z2011-10-212015-03-26T13:00:17Z2010-02-09ALVES, Renata Domingos. Optimization and validation of methodology for determination of aldicarb and carbofuran in coffee samples. 2010. 153 f. Dissertação (Mestrado em Agroquímica analítica; Agroquímica inorgânica e Físico-química; Agroquímica orgânica) - Universidade Federal de Viçosa, Viçosa, 2010.http://locus.ufv.br/handle/123456789/2090Domestic use of aldicarb and carbofuran has resulted in accidental or even intentional poisonings, making it a severe public health problem. A mixture of "chumbinho" (aldicarb) in coffee is frequently a poisoning agent due to strong odor and color of coffee which hide the presende of "chumbinho". Thus, the objective of this study was to adapt, optimize and validate a liquid-liquid extraction technique with low temperature partitioning (LLE-LTP) for determination of aldicarb and carbofuran in coffee by high performance liquid chromatography (HPLC-UV), aiming to make the technique available for poisoning cases of forensic and agrarian interest. Preliminary tests were performed on optimization of the method for the evaluation of variables from extraction of pesticides such as: solvent extractor, volume of the sample and solvent extractor, pH of the sample, ionic force, homogenization mode and times of agitation, fortification and partitioning. Later, a complete 22 factorial scheme was used for evaluation of the simultaneous behavior of NaCl concentration in the sample (0% or 3% w/v) and pH of the sample (3.0 or 5.5) on extraction efficiency of the carbamates. The optimized method consisted of adding 2.0 mL of the coffee sample (8% w/v) and 4.0 mL of acetonitrile, verifying the formation of a single phase. This mixture is then agitated on a table agitator (5 minutes) and placed in a freezer at -20°C for 3 hours. Under these conditions the phases are separated and the organic extract which contains the active principles which is recovered and analyzed by HPLC, employing water and acetonitrile as the mobile phase (65:35). The optimized technique was validated, determining the principle figures of merit, including: selectivity, detection and quantification limits and linearity. Effect of the matrix on quantification of these active principles by HPLC was also evaluated. The results indicated that the LLE-LTP method is efficient for extraction of the two pesticides in coffee samples, showing recovery percentages greater than 94%. Detection and quantification limits of the method were 0.54 and 1.80 mg L-1 respectively for aldicarb and 0.28 and 0.92 mg L-1 for carbofuran. The effect of the matrix showed to be present on quantification of the pesticides by liquid chromatography. In the study of the stability of these active principles, it was observed that of the three factors analyzed, storage temperature of the samples was the factor that most affected degradation of the carbamates. At room temperature, fungi growth as wellas greater degradation of the composts was observed after 5 days. Therefore, optimization of the LLE-LTP method for extraction of pesticide residues from coffee samples and analysis by HPLC resulted in a simple and effective method, with little consumption of solvent, high analytical frequency and low cost.O emprego doméstico de aldicarbe e carbofurano tem acarretado envenenamento acidental ou intencional, tornando-se um grave problema de saúde pública. A mistura do chumbinho em café (pó e bebida) é uma alternativa frequente de envenenamento em função do forte odor e cor do café que disfarçam a presença do chumbinho. Assim, o objetivo desse trabalho foi adaptar, otimizar e validar a técnica de extração líquido-líquido com partição em baixa temperatura (ELL-PBT) para determinação de aldicarbe e carbofurano em café bebida por cromatografia líquida de alta eficiência (CLAEUV) visando a disponibilização da técnica para elucidação de casos de interesse forense e agrário. Testes preliminares foram realizados na otimização do método para avaliação de variáveis na extração dos agrotóxicos como: solvente extrator, volume de amostra e de solvente extrator, pH da amostra, força iônica, modo de homogeneização e tempos de agitação, de fortificação e de partição. Posteriormente, um planejamento fatorial completo 22, foi realizado para avaliação do comportamento simultâneo da concentração de NaCl na amostra (0% ou 3% m/v) e do pH da amostra (3,0 ou 5,5) na eficiência de extração dos carbamatos. O método otimizado consiste em acrescentar a 2,0 mL do café bebida (8% m/v), 4,0 mL de acetonitrila, verificando-se a formação de fase única. Essa mistura é então, agitada em mesa agitadora (5 minutos) e levada ao freezer à -20 ºC por 3 horas. Nestas condições as fases são separadas e o extrato orgânico, contendo os princípios ativos são recuperados e analisados por CLAE, empregando água e acetonitrila como fase móvel (65:35). A técnica otimizada foi validada, determinando as principais figuras de mérito, tais como: seletividade, limites de detecção e de quantificação e linearidade. Avaliou-se também o efeito de matriz na quantificação desses princípios ativos por CLAE. Os resultados indicam que o método de ELL-PBT é eficiente para a extração dos dois agrotóxicos em amostras de café bebida, mostrando porcentagens de recuperação maiores que 94%. Os limites de detecção e quantificação do método foram 0,54 e 1,80 mg L-1 respectivamente, para o aldicarbe e 0,28 e 0,92 mg L-1 para o carbofurano. O efeito da matriz mostrou-se presente na quantificação dos agrotóxicos por cromatografia líquida. No estudo da estabilidade desses princípios ativos, observou-se que dos três fatores analisados, a temperatura de armazenamento das amostras foi o fator que mais afetou a degradação dos carbamatos. À temperatura ambiente, observouse após 5 dias o crescimento de fungos e também maior degradação dos compostos. Logo, a otimização da ELL-PBT para extração de resíduos de agrotóxicos em amostras de café bebida e análise por CLAE resultou em um método simples, eficaz, com pequeno consumo de solvente, alta frequência analítica e baixo custo.application/pdfporUniversidade Federal de ViçosaMestrado em AgroquímicaUFVBRAgroquímica analítica; Agroquímica inorgânica e Físico-química; Agroquímica orgânicaAnálise de resíduosCarbamatosPartição em baixa temperaturaResidue analysisCarbamatesLow temperature partitioningCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA::QUIMICA ANALITICAOtimização e validação de metodologia para determinação de aldicarbe e carbofurano em amostras de café bebidaOptimization and validation of methodology for determination of aldicarb and carbofuran in coffee samplesinfo: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/pdf3595778https://locus.ufv.br//bitstream/123456789/2090/1/texto%20completo.pdfb2ff5d942fe0c26e0c016e1a629ae5d9MD51TEXTtexto completo.pdf.txttexto completo.pdf.txtExtracted texttext/plain274630https://locus.ufv.br//bitstream/123456789/2090/2/texto%20completo.pdf.txt15f26fdd226c4fc2bc644cb6a1bddd35MD52THUMBNAILtexto completo.pdf.jpgtexto completo.pdf.jpgIM Thumbnailimage/jpeg3818https://locus.ufv.br//bitstream/123456789/2090/3/texto%20completo.pdf.jpged0e48f9e66fcfe8a992a25e0eccc0f3MD53123456789/20902016-04-07 23:20:51.328oai:locus.ufv.br:123456789/2090Repositório InstitucionalPUBhttps://www.locus.ufv.br/oai/requestfabiojreis@ufv.bropendoar:21452016-04-08T02:20:51LOCUS Repositório Institucional da UFV - Universidade Federal de Viçosa (UFV)false
dc.title.por.fl_str_mv Otimização e validação de metodologia para determinação de aldicarbe e carbofurano em amostras de café bebida
dc.title.alternative.eng.fl_str_mv Optimization and validation of methodology for determination of aldicarb and carbofuran in coffee samples
title Otimização e validação de metodologia para determinação de aldicarbe e carbofurano em amostras de café bebida
spellingShingle Otimização e validação de metodologia para determinação de aldicarbe e carbofurano em amostras de café bebida
Alves, Renata Domingos
Análise de resíduos
Carbamatos
Partição em baixa temperatura
Residue analysis
Carbamates
Low temperature partitioning
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA::QUIMICA ANALITICA
title_short Otimização e validação de metodologia para determinação de aldicarbe e carbofurano em amostras de café bebida
title_full Otimização e validação de metodologia para determinação de aldicarbe e carbofurano em amostras de café bebida
title_fullStr Otimização e validação de metodologia para determinação de aldicarbe e carbofurano em amostras de café bebida
title_full_unstemmed Otimização e validação de metodologia para determinação de aldicarbe e carbofurano em amostras de café bebida
title_sort Otimização e validação de metodologia para determinação de aldicarbe e carbofurano em amostras de café bebida
author Alves, Renata Domingos
author_facet Alves, Renata Domingos
author_role author
dc.contributor.authorLattes.por.fl_str_mv http://lattes.cnpq.br/0515651682967753
dc.contributor.author.fl_str_mv Alves, Renata Domingos
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 Zambolim, Laércio
dc.contributor.advisor-co2Lattes.fl_str_mv http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4787254T6
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 Reis, Efraim Lázaro
dc.contributor.referee1Lattes.fl_str_mv http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4788214H7
dc.contributor.referee2.fl_str_mv Paula, Washington Xavier de
dc.contributor.referee2Lattes.fl_str_mv http://lattes.cnpq.br/7959181697121752
contributor_str_mv Neves, Antônio Augusto
Zambolim, Laércio
Queiroz, Maria Eliana Lopes Ribeiro de
Reis, Efraim Lázaro
Paula, Washington Xavier de
dc.subject.por.fl_str_mv Análise de resíduos
Carbamatos
Partição em baixa temperatura
topic Análise de resíduos
Carbamatos
Partição em baixa temperatura
Residue analysis
Carbamates
Low temperature partitioning
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA::QUIMICA ANALITICA
dc.subject.eng.fl_str_mv Residue analysis
Carbamates
Low temperature partitioning
dc.subject.cnpq.fl_str_mv CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA::QUIMICA ANALITICA
description Domestic use of aldicarb and carbofuran has resulted in accidental or even intentional poisonings, making it a severe public health problem. A mixture of "chumbinho" (aldicarb) in coffee is frequently a poisoning agent due to strong odor and color of coffee which hide the presende of "chumbinho". Thus, the objective of this study was to adapt, optimize and validate a liquid-liquid extraction technique with low temperature partitioning (LLE-LTP) for determination of aldicarb and carbofuran in coffee by high performance liquid chromatography (HPLC-UV), aiming to make the technique available for poisoning cases of forensic and agrarian interest. Preliminary tests were performed on optimization of the method for the evaluation of variables from extraction of pesticides such as: solvent extractor, volume of the sample and solvent extractor, pH of the sample, ionic force, homogenization mode and times of agitation, fortification and partitioning. Later, a complete 22 factorial scheme was used for evaluation of the simultaneous behavior of NaCl concentration in the sample (0% or 3% w/v) and pH of the sample (3.0 or 5.5) on extraction efficiency of the carbamates. The optimized method consisted of adding 2.0 mL of the coffee sample (8% w/v) and 4.0 mL of acetonitrile, verifying the formation of a single phase. This mixture is then agitated on a table agitator (5 minutes) and placed in a freezer at -20°C for 3 hours. Under these conditions the phases are separated and the organic extract which contains the active principles which is recovered and analyzed by HPLC, employing water and acetonitrile as the mobile phase (65:35). The optimized technique was validated, determining the principle figures of merit, including: selectivity, detection and quantification limits and linearity. Effect of the matrix on quantification of these active principles by HPLC was also evaluated. The results indicated that the LLE-LTP method is efficient for extraction of the two pesticides in coffee samples, showing recovery percentages greater than 94%. Detection and quantification limits of the method were 0.54 and 1.80 mg L-1 respectively for aldicarb and 0.28 and 0.92 mg L-1 for carbofuran. The effect of the matrix showed to be present on quantification of the pesticides by liquid chromatography. In the study of the stability of these active principles, it was observed that of the three factors analyzed, storage temperature of the samples was the factor that most affected degradation of the carbamates. At room temperature, fungi growth as wellas greater degradation of the composts was observed after 5 days. Therefore, optimization of the LLE-LTP method for extraction of pesticide residues from coffee samples and analysis by HPLC resulted in a simple and effective method, with little consumption of solvent, high analytical frequency and low cost.
publishDate 2010
dc.date.issued.fl_str_mv 2010-02-09
dc.date.available.fl_str_mv 2011-10-21
2015-03-26T13:00:17Z
dc.date.accessioned.fl_str_mv 2015-03-26T13:00:17Z
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 ALVES, Renata Domingos. Optimization and validation of methodology for determination of aldicarb and carbofuran in coffee samples. 2010. 153 f. Dissertação (Mestrado em Agroquímica analítica; Agroquímica inorgânica e Físico-química; Agroquímica orgânica) - Universidade Federal de Viçosa, Viçosa, 2010.
dc.identifier.uri.fl_str_mv http://locus.ufv.br/handle/123456789/2090
identifier_str_mv ALVES, Renata Domingos. Optimization and validation of methodology for determination of aldicarb and carbofuran in coffee samples. 2010. 153 f. Dissertação (Mestrado em Agroquímica analítica; Agroquímica inorgânica e Físico-química; Agroquímica orgânica) - Universidade Federal de Viçosa, Viçosa, 2010.
url http://locus.ufv.br/handle/123456789/2090
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 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
publisher.none.fl_str_mv Universidade Federal de Viçosa
dc.source.none.fl_str_mv reponame:LOCUS Repositório Institucional da UFV
instname:Universidade Federal de Viçosa (UFV)
instacron:UFV
instname_str Universidade Federal de Viçosa (UFV)
instacron_str UFV
institution UFV
reponame_str LOCUS Repositório Institucional da UFV
collection LOCUS Repositório Institucional da UFV
bitstream.url.fl_str_mv https://locus.ufv.br//bitstream/123456789/2090/1/texto%20completo.pdf
https://locus.ufv.br//bitstream/123456789/2090/2/texto%20completo.pdf.txt
https://locus.ufv.br//bitstream/123456789/2090/3/texto%20completo.pdf.jpg
bitstream.checksum.fl_str_mv b2ff5d942fe0c26e0c016e1a629ae5d9
15f26fdd226c4fc2bc644cb6a1bddd35
ed0e48f9e66fcfe8a992a25e0eccc0f3
bitstream.checksumAlgorithm.fl_str_mv MD5
MD5
MD5
repository.name.fl_str_mv LOCUS Repositório Institucional da UFV - Universidade Federal de Viçosa (UFV)
repository.mail.fl_str_mv fabiojreis@ufv.br
_version_ 1801213124728061952