Análise multirresíduo de agrotóxicos em abacaxi por CG/DCE
Autor(a) principal: | |
---|---|
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/123456789/2089 |
Resumo: | The objectives of this work were to optimize the technique of extraction by matrix solid-phase dispersion (MSPD) and the solid-liquid with partition in low temperature extraction technique (SLE-LTP), and to validate this latter, to the residues analysis of the pesticides atrazine, thiamethoxam, triadimenol and deltamethrin in pineapple samples, by gas chromatography with electron capture detector (GC/ECD). In the optimization stage of the extraction technique solid-liquid with partition in low temperature, factors that influence in the percentage of recovery of pesticides, and provide ideal conditions of analysis, were evaluated. The optimized method was validated thorugh the determination of the selectivity, the linearity of answer of the method, the limit detection, the limit quantification, the accuracy and the precision. The obtained results showed that the technique SLE-LTP is efficient for analysis of the pesticides thiamethoxam, triadimenol and deltamethrin, with superior recovery percentages up to 90%, and atrazina, with percentage of recovery of approximately 60%. Besides, the quantification limits for the thiamethoxam, triadimenol and deltamethrin (0,050; 0,17 e 0,040 μg g-1) were smaller than the allowed maximum limits of residues (LMR), established for these pesticides in pineapple, by the European Union. The optimized and validated technique was applied to samples of pineapple, 'Pérola' cultivar, from the cities Marataízes (ES), Miracema do Tocantins (TO) e Monte Alegre de Minas (MG), not being detected the presence of residues of the pesticides studied in the pineapple samples analyzed. It was also studied, the influence of the components of the pineapple in the quantification of the pesticides in analyses for chromatography in gaseous phase, using the matrix method overlap. The results showed that the co-extractives of the matrix affect significantly in the quantification of the pesticides in study. With the intention of comparing the technique SLE-LTP, the technique of extraction matrix solid-phase dispersion was optimized, being appraised the adsorbent, the eluent, and later accomplished a planning factorial 23 to evaluate the simultaneous behavior of the factors: (1) proportion between adsorbent and sample, (2) co-column use and (3) ultrasound use. The cocolumn presence, besides influencing in the percentage of recovery of the pesticides atrazine, thiamethoxam and triadimenol, affects qualitatively the chromatogram. Comparing the extraction techniques SLE-LTP and MSPD, both present high recovery levels for the pesticides in study, except for the atrazine, in that SLE-LTP presented recovery percentages higher. Besides, the extracts obtained in SLE-LTP are less susceptible to the presence of interferences. |
id |
UFV_ba81ca0a15ca948770da3572bb83e2b9 |
---|---|
oai_identifier_str |
oai:locus.ufv.br:123456789/2089 |
network_acronym_str |
UFV |
network_name_str |
LOCUS Repositório Institucional da UFV |
repository_id_str |
2145 |
spelling |
Costa, Elisa Helena dahttp://lattes.cnpq.br/8638527720963185Neves, 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, Césarhttp://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4785327P6Okumura, Leonardo Luizhttp://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4762150J02015-03-26T13:00:16Z2011-07-042015-03-26T13:00:16Z2010-02-10COSTA, Elisa Helena da. Analysis multiresidue of pesticides in pineapple by GC/ECD. 2010. 116 f. Dissertação (Mestrado em Agroquímica analítica; Agroquímica inorgânica e Físico-química; Agroquímica orgânica) - Universidade Federal de Viçosa, Viçosa, 2010.http://locus.ufv.br/handle/123456789/2089The objectives of this work were to optimize the technique of extraction by matrix solid-phase dispersion (MSPD) and the solid-liquid with partition in low temperature extraction technique (SLE-LTP), and to validate this latter, to the residues analysis of the pesticides atrazine, thiamethoxam, triadimenol and deltamethrin in pineapple samples, by gas chromatography with electron capture detector (GC/ECD). In the optimization stage of the extraction technique solid-liquid with partition in low temperature, factors that influence in the percentage of recovery of pesticides, and provide ideal conditions of analysis, were evaluated. The optimized method was validated thorugh the determination of the selectivity, the linearity of answer of the method, the limit detection, the limit quantification, the accuracy and the precision. The obtained results showed that the technique SLE-LTP is efficient for analysis of the pesticides thiamethoxam, triadimenol and deltamethrin, with superior recovery percentages up to 90%, and atrazina, with percentage of recovery of approximately 60%. Besides, the quantification limits for the thiamethoxam, triadimenol and deltamethrin (0,050; 0,17 e 0,040 μg g-1) were smaller than the allowed maximum limits of residues (LMR), established for these pesticides in pineapple, by the European Union. The optimized and validated technique was applied to samples of pineapple, 'Pérola' cultivar, from the cities Marataízes (ES), Miracema do Tocantins (TO) e Monte Alegre de Minas (MG), not being detected the presence of residues of the pesticides studied in the pineapple samples analyzed. It was also studied, the influence of the components of the pineapple in the quantification of the pesticides in analyses for chromatography in gaseous phase, using the matrix method overlap. The results showed that the co-extractives of the matrix affect significantly in the quantification of the pesticides in study. With the intention of comparing the technique SLE-LTP, the technique of extraction matrix solid-phase dispersion was optimized, being appraised the adsorbent, the eluent, and later accomplished a planning factorial 23 to evaluate the simultaneous behavior of the factors: (1) proportion between adsorbent and sample, (2) co-column use and (3) ultrasound use. The cocolumn presence, besides influencing in the percentage of recovery of the pesticides atrazine, thiamethoxam and triadimenol, affects qualitatively the chromatogram. Comparing the extraction techniques SLE-LTP and MSPD, both present high recovery levels for the pesticides in study, except for the atrazine, in that SLE-LTP presented recovery percentages higher. Besides, the extracts obtained in SLE-LTP are less susceptible to the presence of interferences.Os objetivos deste trabalho foram otimizar a técnica de extração por dispersão de matriz em fase sólida (DMFS) e a técnica extração sólido-líquido com partição em baixa temperatura (ESL-PBT), e validar esta última, para análise de resíduos dos agrotóxicos atrazina, thiamethoxam, triadimenol e deltametrina em amostras de abacaxi, por cromatografia gasosa com detector por captura de elétrons (CG/DCE). Na etapa de otimização da técnica extração sólido-líquido com partição em baixa temperatura, fatores que influenciam na porcentagem de recuperação dos agrotóxicos, e proporcionam condições ideais de análise, foram avaliados. O método otimizado foi validado determinando-se a seletividade, a linearidade de resposta do método, o limite de detecção, o limite de quantificação, a exatidão e a precisão. Os resultados obtidos mostraram que a técnica ESL-PBT é eficiente para análise dos agrotóxicos thiamethoxam, triadimenol e deltametrina, com porcentagens de recuperação superiores a 90%, e atrazina, com porcentagem de recuperação de aproximadamente 60%. Além disso, os limites de quantificação para o thiamethoxam, triadimenol e deltametrina (0,050; 0,17 e 0,040 µg g-1) foram menores que os limites máximos de resíduos (LMR), estabelecidos para estes agrotóxicos em abacaxi, pela União Européia. A técnica otimizada e validada foi aplicada a amostras de abacaxi, cultivar Pérola , procedentes das cidades Marataízes (ES), Miracema do Tocantins (TO) e Monte Alegre de Minas (MG), não sendo detectada a presença de resíduos dos agrotóxicos estudados nas amostras de abacaxi analisadas. Foi estudada também, a influência dos componentes do abacaxi na quantificação dos agrotóxicos por cromatografia gasosa, empregando o método de superposição de matriz. Os resultados mostraram que co-extrativos da matriz afetam significativamente na quantificação dos agrotóxicos em estudo. Com o intuito de comparar a técnica ESL-PBT, a técnica de extração por dispersão de matriz em fase sólida foi otimizada, sendo avaliados o adsorvente, o eluente, e posteriormente realizado um planejamento fatorial 23, para avaliar o comportamento simultâneo dos fatores: (1) proporção entre adsorvente e amostra, (2) utilização de co-coluna e (3) utilização de ultra-som. A presença de co-coluna, além de influenciar na porcentagem de recuperação dos agrotóxicos atrazina, thiamethoxam e triadimenol, afeta qualitativamente os cromatogramas. Comparando-se as técnicas de extração ESL-PBT e DMFS, ambas apresentam altos níveis de recuperação para os agrotóxicos em estudo, exceto para a atrazina, em que a ESL-PBT apresentou porcentagens de recuperação mais altas. Além disso, os extratos obtidos na ESL-PBT são menos suscepitíveis à presença de interferentes.Conselho Nacional de Desenvolvimento Científico e Tecnológicoapplication/pdfporUniversidade Federal de ViçosaMestrado em AgroquímicaUFVBRAgroquímica analítica; Agroquímica inorgânica e Físico-química; Agroquímica orgânicaAnálise de multirresíduosAbacaxiPartição em baixa temperaturaAnalysis multiresiduePineapplePartition in low temperatureCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA::QUIMICA ANALITICAAnálise multirresíduo de agrotóxicos em abacaxi por CG/DCEAnalysis multiresidue of pesticides in pineapple by GC/ECDinfo: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/pdf779587https://locus.ufv.br//bitstream/123456789/2089/1/texto%20completo.pdff783bad27f2d6a13f6b8893ecf0bd54aMD51TEXTtexto completo.pdf.txttexto completo.pdf.txtExtracted texttext/plain199312https://locus.ufv.br//bitstream/123456789/2089/2/texto%20completo.pdf.txt19c621f656ce6d4cc8b55e87b9a3b600MD52THUMBNAILtexto completo.pdf.jpgtexto completo.pdf.jpgIM Thumbnailimage/jpeg3655https://locus.ufv.br//bitstream/123456789/2089/3/texto%20completo.pdf.jpg27bb38ce0b5089b60af27fce9a7b734dMD53123456789/20892016-04-07 23:20:40.135oai:locus.ufv.br:123456789/2089Repositório InstitucionalPUBhttps://www.locus.ufv.br/oai/requestfabiojreis@ufv.bropendoar:21452016-04-08T02:20:40LOCUS Repositório Institucional da UFV - Universidade Federal de Viçosa (UFV)false |
dc.title.por.fl_str_mv |
Análise multirresíduo de agrotóxicos em abacaxi por CG/DCE |
dc.title.alternative.eng.fl_str_mv |
Analysis multiresidue of pesticides in pineapple by GC/ECD |
title |
Análise multirresíduo de agrotóxicos em abacaxi por CG/DCE |
spellingShingle |
Análise multirresíduo de agrotóxicos em abacaxi por CG/DCE Costa, Elisa Helena da Análise de multirresíduos Abacaxi Partição em baixa temperatura Analysis multiresidue Pineapple Partition in low temperature CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA::QUIMICA ANALITICA |
title_short |
Análise multirresíduo de agrotóxicos em abacaxi por CG/DCE |
title_full |
Análise multirresíduo de agrotóxicos em abacaxi por CG/DCE |
title_fullStr |
Análise multirresíduo de agrotóxicos em abacaxi por CG/DCE |
title_full_unstemmed |
Análise multirresíduo de agrotóxicos em abacaxi por CG/DCE |
title_sort |
Análise multirresíduo de agrotóxicos em abacaxi por CG/DCE |
author |
Costa, Elisa Helena da |
author_facet |
Costa, Elisa Helena da |
author_role |
author |
dc.contributor.authorLattes.por.fl_str_mv |
http://lattes.cnpq.br/8638527720963185 |
dc.contributor.author.fl_str_mv |
Costa, Elisa Helena da |
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, César |
dc.contributor.referee1Lattes.fl_str_mv |
http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4785327P6 |
dc.contributor.referee2.fl_str_mv |
Okumura, Leonardo Luiz |
dc.contributor.referee2Lattes.fl_str_mv |
http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4762150J0 |
contributor_str_mv |
Neves, Antônio Augusto Zambolim, Laércio Queiroz, Maria Eliana Lopes Ribeiro de Reis, César Okumura, Leonardo Luiz |
dc.subject.por.fl_str_mv |
Análise de multirresíduos Abacaxi Partição em baixa temperatura |
topic |
Análise de multirresíduos Abacaxi Partição em baixa temperatura Analysis multiresidue Pineapple Partition in low temperature CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA::QUIMICA ANALITICA |
dc.subject.eng.fl_str_mv |
Analysis multiresidue Pineapple Partition in low temperature |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA::QUIMICA ANALITICA |
description |
The objectives of this work were to optimize the technique of extraction by matrix solid-phase dispersion (MSPD) and the solid-liquid with partition in low temperature extraction technique (SLE-LTP), and to validate this latter, to the residues analysis of the pesticides atrazine, thiamethoxam, triadimenol and deltamethrin in pineapple samples, by gas chromatography with electron capture detector (GC/ECD). In the optimization stage of the extraction technique solid-liquid with partition in low temperature, factors that influence in the percentage of recovery of pesticides, and provide ideal conditions of analysis, were evaluated. The optimized method was validated thorugh the determination of the selectivity, the linearity of answer of the method, the limit detection, the limit quantification, the accuracy and the precision. The obtained results showed that the technique SLE-LTP is efficient for analysis of the pesticides thiamethoxam, triadimenol and deltamethrin, with superior recovery percentages up to 90%, and atrazina, with percentage of recovery of approximately 60%. Besides, the quantification limits for the thiamethoxam, triadimenol and deltamethrin (0,050; 0,17 e 0,040 μg g-1) were smaller than the allowed maximum limits of residues (LMR), established for these pesticides in pineapple, by the European Union. The optimized and validated technique was applied to samples of pineapple, 'Pérola' cultivar, from the cities Marataízes (ES), Miracema do Tocantins (TO) e Monte Alegre de Minas (MG), not being detected the presence of residues of the pesticides studied in the pineapple samples analyzed. It was also studied, the influence of the components of the pineapple in the quantification of the pesticides in analyses for chromatography in gaseous phase, using the matrix method overlap. The results showed that the co-extractives of the matrix affect significantly in the quantification of the pesticides in study. With the intention of comparing the technique SLE-LTP, the technique of extraction matrix solid-phase dispersion was optimized, being appraised the adsorbent, the eluent, and later accomplished a planning factorial 23 to evaluate the simultaneous behavior of the factors: (1) proportion between adsorbent and sample, (2) co-column use and (3) ultrasound use. The cocolumn presence, besides influencing in the percentage of recovery of the pesticides atrazine, thiamethoxam and triadimenol, affects qualitatively the chromatogram. Comparing the extraction techniques SLE-LTP and MSPD, both present high recovery levels for the pesticides in study, except for the atrazine, in that SLE-LTP presented recovery percentages higher. Besides, the extracts obtained in SLE-LTP are less susceptible to the presence of interferences. |
publishDate |
2010 |
dc.date.issued.fl_str_mv |
2010-02-10 |
dc.date.available.fl_str_mv |
2011-07-04 2015-03-26T13:00:16Z |
dc.date.accessioned.fl_str_mv |
2015-03-26T13:00:16Z |
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 |
COSTA, Elisa Helena da. Analysis multiresidue of pesticides in pineapple by GC/ECD. 2010. 116 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/123456789/2089 |
identifier_str_mv |
COSTA, Elisa Helena da. Analysis multiresidue of pesticides in pineapple by GC/ECD. 2010. 116 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/123456789/2089 |
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/123456789/2089/1/texto%20completo.pdf https://locus.ufv.br//bitstream/123456789/2089/2/texto%20completo.pdf.txt https://locus.ufv.br//bitstream/123456789/2089/3/texto%20completo.pdf.jpg |
bitstream.checksum.fl_str_mv |
f783bad27f2d6a13f6b8893ecf0bd54a 19c621f656ce6d4cc8b55e87b9a3b600 27bb38ce0b5089b60af27fce9a7b734d |
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_ |
1801213023107416064 |