Determinação de resíduos de pesticidas em plantas de arroz empregando QuEChERS modificado e GC-ECD
Autor(a) principal: | |
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Data de Publicação: | 2008 |
Tipo de documento: | Dissertação |
Idioma: | por |
Título da fonte: | Manancial - Repositório Digital da UFSM |
Texto Completo: | http://repositorio.ufsm.br/handle/1/10439 |
Resumo: | Rice culture is an activity that has currently been gaining more importance due to its use in human feeding, allowing enough food and acceptable quality to the population. There is a great concern regarding the intensive use of pesticides, the main strategy employed in the countryside to combat and prevent plagues, as well as the residues resulting from such practice. This paper has been developed and validated on an analytical procedure, using the QuEChERS modified extraction approach and gas chromatography with electron-capture detection (GC-ECD) for the determination of residual insecticides lambda-cyhalothrin and bifenthrin and azoxystrobin fungicides and trifloxystrobin in rice plants. The QuEChERS modified method was applied in an initial stage of extraction using 3.0 g of rice plants in which was added 15 mL of acetonitrile containing 1% (v/v) acetic acid, followed by a partition step after the addition of a mixture of anhydrous salts (3 g of magnesium sulphate and 1.7 grams of sodium acetate). Next, the clean-up stage was carried out 4 mL extract using 200 mg of activated charcoal and 600 mg of magnesium sulfate and the analysed by GC-ECD using an apolar DB-5 column. During method validation, LOD; LOQ; linearity; precision (repeatability and intermediate precision); and accuracy, evaluated in terms of recovery, were determined. Using this method, LOQ quantities were 1 mg kg-1 for azoxystrobin and 0.05 mg kg-1 for lambdacyhalothrin, bifenthrin and trifloxystrobin. The analytical curves presented linearity between 0.01 and 1.0 mg L-1, with coefficient of determination greater than 0.993. The method had shown good precision, with RSD values smaller than 19.0%, and accuracy, with recoveries between 71.2 and 103.6%. The method was considered adequate to the analysis of pesticides in rice plants, considering that all validation parameters meet the levels required for validation of chromatographic methods. After being validated, the method was applied to the study of the residual concentration of pesticides in rice plants, from rice crops irrigated with an experiment carried through at the UFSM Campus; where the pesticides azoxystrobin, bifenthrin, lambda-cyhalothrin, and trifloxystrobin were individually applied in 2007/2008 harvest. All pesticides in this study were detected up to approximately twenty (20) days after being applied. |
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Determinação de resíduos de pesticidas em plantas de arroz empregando QuEChERS modificado e GC-ECDDetermination of pesticide residues in rice plants using modified QuEChERS and GC-ECDResíduos de pesticidasArrozPlantas de arrozQuEChERSResidues of pesticidesRiceRice plantsGC-ECDCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICARice culture is an activity that has currently been gaining more importance due to its use in human feeding, allowing enough food and acceptable quality to the population. There is a great concern regarding the intensive use of pesticides, the main strategy employed in the countryside to combat and prevent plagues, as well as the residues resulting from such practice. This paper has been developed and validated on an analytical procedure, using the QuEChERS modified extraction approach and gas chromatography with electron-capture detection (GC-ECD) for the determination of residual insecticides lambda-cyhalothrin and bifenthrin and azoxystrobin fungicides and trifloxystrobin in rice plants. The QuEChERS modified method was applied in an initial stage of extraction using 3.0 g of rice plants in which was added 15 mL of acetonitrile containing 1% (v/v) acetic acid, followed by a partition step after the addition of a mixture of anhydrous salts (3 g of magnesium sulphate and 1.7 grams of sodium acetate). Next, the clean-up stage was carried out 4 mL extract using 200 mg of activated charcoal and 600 mg of magnesium sulfate and the analysed by GC-ECD using an apolar DB-5 column. During method validation, LOD; LOQ; linearity; precision (repeatability and intermediate precision); and accuracy, evaluated in terms of recovery, were determined. Using this method, LOQ quantities were 1 mg kg-1 for azoxystrobin and 0.05 mg kg-1 for lambdacyhalothrin, bifenthrin and trifloxystrobin. The analytical curves presented linearity between 0.01 and 1.0 mg L-1, with coefficient of determination greater than 0.993. The method had shown good precision, with RSD values smaller than 19.0%, and accuracy, with recoveries between 71.2 and 103.6%. The method was considered adequate to the analysis of pesticides in rice plants, considering that all validation parameters meet the levels required for validation of chromatographic methods. After being validated, the method was applied to the study of the residual concentration of pesticides in rice plants, from rice crops irrigated with an experiment carried through at the UFSM Campus; where the pesticides azoxystrobin, bifenthrin, lambda-cyhalothrin, and trifloxystrobin were individually applied in 2007/2008 harvest. All pesticides in this study were detected up to approximately twenty (20) days after being applied.A cultura do arroz é uma atividade de importância cada vez maior pela sua utilização na alimentação humana, garantindo alimento suficiente e de qualidade para a população. A grande preocupação é o uso intensivo de pesticidas; principal estratégia no campo para o combate e a prevenção de pragas, e os resíduos decorrentes desta prática. Neste trabalho, desenvolveu-se e validou-se um procedimento analítico, utilizando o método de extração QuEChERS modificado e Cromatografia Gasosa com Detecção por Captura de Elétrons (GC-ECD) para a determinação residual dos inseticidas bifentrina e lambda-cialotrina e dos fungicidas azoxistrobina e trifloxistrobina em plantas de arroz. O método QuEChERS modificado consistiu em uma etapa de extração inicial utilizando 3,0 g de plantas de arroz na qual foi adicionado 15 mL de acetonitrila contendo 1% (v/v) de ácido acético, seguida por uma etapa de partição após a adição de uma mistura de sais anidros (3 g de sulfato de magnésio e 1,7 g de acetato de sódio). Na seqüência foi realizada a etapa de clean-up de 4 mL de extrato com 20 mg de carvão ativado vegetal e 600 mg de sulfato de magnésio e a análise por GCECD utilizando-se coluna apolar DB-5. Na validação do método determinou-se LOD, LOQ, linearidade, precisão (repetitividade e precisão intermediária) e exatidão, avaliada pela recuperação. Os valores de LOQ do método foram 1,0 mg kg-1 para azoxistrobina e 0,05 mg kg-1 para lambda-cialotrina, bifentrina e trifloxistrobina. As curvas analíticas apresentaram linearidade entre 0,01 e 1,0 mg L-1, com valores de coeficiente de determinação maiores que 0,993. O método apresentou boa precisão, com valores de RSD inferiores a 19,0%, e boa exatidão, com recuperações entre 71,2 e 103,6%. O método foi considerado adequado à análise dos pesticidas em plantas de arroz, visto que todos os parâmetros de validação atendem os limites sugeridos para validação de métodos cromatográficos. Após ser validado, o método foi aplicado em um estudo da concentração residual dos pesticidas em plantas de arroz, oriundas de lavoura de arroz irrigado de um experimento realizado no Campus da UFSM, onde foram aplicados separadamente os pesticidas azoxistrobina, bifentrina, lambda-cialotrina e trifloxistrobina, na safra 2007/2008. Todos os pesticidas em estudo foram detectados até aproximadamente 20 dias após a sua aplicação.Universidade Federal de Santa MariaBRQuímicaUFSMPrograma de Pós-Graduação em QuímicaZanella, Renatohttp://lattes.cnpq.br/2541865299438479Leite, Natalicio Ferreirahttp://lattes.cnpq.br/6593917721152246Adaime, Martha Bohrerhttp://lattes.cnpq.br/4385786922516848Cogo, Juliana Pivetta2017-05-182017-05-182008-12-19info:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisapplication/pdfapplication/pdfCOGO, Juliana Pivetta. Determination of pesticide residues in rice plants using modified QuEChERS and GC-ECD. 2008. 113 f. Dissertação (Mestrado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2008.http://repositorio.ufsm.br/handle/1/10439porinfo:eu-repo/semantics/openAccessreponame:Manancial - Repositório Digital da UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSM2023-04-20T11:34:16Zoai:repositorio.ufsm.br:1/10439Biblioteca Digital de Teses e Dissertaçõeshttps://repositorio.ufsm.br/ONGhttps://repositorio.ufsm.br/oai/requestatendimento.sib@ufsm.br||tedebc@gmail.comopendoar:2023-04-20T11:34:16Manancial - Repositório Digital da UFSM - Universidade Federal de Santa Maria (UFSM)false |
dc.title.none.fl_str_mv |
Determinação de resíduos de pesticidas em plantas de arroz empregando QuEChERS modificado e GC-ECD Determination of pesticide residues in rice plants using modified QuEChERS and GC-ECD |
title |
Determinação de resíduos de pesticidas em plantas de arroz empregando QuEChERS modificado e GC-ECD |
spellingShingle |
Determinação de resíduos de pesticidas em plantas de arroz empregando QuEChERS modificado e GC-ECD Cogo, Juliana Pivetta Resíduos de pesticidas Arroz Plantas de arroz QuEChERS Residues of pesticides Rice Rice plants GC-ECD CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Determinação de resíduos de pesticidas em plantas de arroz empregando QuEChERS modificado e GC-ECD |
title_full |
Determinação de resíduos de pesticidas em plantas de arroz empregando QuEChERS modificado e GC-ECD |
title_fullStr |
Determinação de resíduos de pesticidas em plantas de arroz empregando QuEChERS modificado e GC-ECD |
title_full_unstemmed |
Determinação de resíduos de pesticidas em plantas de arroz empregando QuEChERS modificado e GC-ECD |
title_sort |
Determinação de resíduos de pesticidas em plantas de arroz empregando QuEChERS modificado e GC-ECD |
author |
Cogo, Juliana Pivetta |
author_facet |
Cogo, Juliana Pivetta |
author_role |
author |
dc.contributor.none.fl_str_mv |
Zanella, Renato http://lattes.cnpq.br/2541865299438479 Leite, Natalicio Ferreira http://lattes.cnpq.br/6593917721152246 Adaime, Martha Bohrer http://lattes.cnpq.br/4385786922516848 |
dc.contributor.author.fl_str_mv |
Cogo, Juliana Pivetta |
dc.subject.por.fl_str_mv |
Resíduos de pesticidas Arroz Plantas de arroz QuEChERS Residues of pesticides Rice Rice plants GC-ECD CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
topic |
Resíduos de pesticidas Arroz Plantas de arroz QuEChERS Residues of pesticides Rice Rice plants GC-ECD CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
Rice culture is an activity that has currently been gaining more importance due to its use in human feeding, allowing enough food and acceptable quality to the population. There is a great concern regarding the intensive use of pesticides, the main strategy employed in the countryside to combat and prevent plagues, as well as the residues resulting from such practice. This paper has been developed and validated on an analytical procedure, using the QuEChERS modified extraction approach and gas chromatography with electron-capture detection (GC-ECD) for the determination of residual insecticides lambda-cyhalothrin and bifenthrin and azoxystrobin fungicides and trifloxystrobin in rice plants. The QuEChERS modified method was applied in an initial stage of extraction using 3.0 g of rice plants in which was added 15 mL of acetonitrile containing 1% (v/v) acetic acid, followed by a partition step after the addition of a mixture of anhydrous salts (3 g of magnesium sulphate and 1.7 grams of sodium acetate). Next, the clean-up stage was carried out 4 mL extract using 200 mg of activated charcoal and 600 mg of magnesium sulfate and the analysed by GC-ECD using an apolar DB-5 column. During method validation, LOD; LOQ; linearity; precision (repeatability and intermediate precision); and accuracy, evaluated in terms of recovery, were determined. Using this method, LOQ quantities were 1 mg kg-1 for azoxystrobin and 0.05 mg kg-1 for lambdacyhalothrin, bifenthrin and trifloxystrobin. The analytical curves presented linearity between 0.01 and 1.0 mg L-1, with coefficient of determination greater than 0.993. The method had shown good precision, with RSD values smaller than 19.0%, and accuracy, with recoveries between 71.2 and 103.6%. The method was considered adequate to the analysis of pesticides in rice plants, considering that all validation parameters meet the levels required for validation of chromatographic methods. After being validated, the method was applied to the study of the residual concentration of pesticides in rice plants, from rice crops irrigated with an experiment carried through at the UFSM Campus; where the pesticides azoxystrobin, bifenthrin, lambda-cyhalothrin, and trifloxystrobin were individually applied in 2007/2008 harvest. All pesticides in this study were detected up to approximately twenty (20) days after being applied. |
publishDate |
2008 |
dc.date.none.fl_str_mv |
2008-12-19 2017-05-18 2017-05-18 |
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.uri.fl_str_mv |
COGO, Juliana Pivetta. Determination of pesticide residues in rice plants using modified QuEChERS and GC-ECD. 2008. 113 f. Dissertação (Mestrado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2008. http://repositorio.ufsm.br/handle/1/10439 |
identifier_str_mv |
COGO, Juliana Pivetta. Determination of pesticide residues in rice plants using modified QuEChERS and GC-ECD. 2008. 113 f. Dissertação (Mestrado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2008. |
url |
http://repositorio.ufsm.br/handle/1/10439 |
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 application/pdf |
dc.publisher.none.fl_str_mv |
Universidade Federal de Santa Maria BR Química UFSM Programa de Pós-Graduação em Química |
publisher.none.fl_str_mv |
Universidade Federal de Santa Maria BR Química UFSM Programa de Pós-Graduação em Química |
dc.source.none.fl_str_mv |
reponame:Manancial - Repositório Digital da UFSM instname:Universidade Federal de Santa Maria (UFSM) instacron:UFSM |
instname_str |
Universidade Federal de Santa Maria (UFSM) |
instacron_str |
UFSM |
institution |
UFSM |
reponame_str |
Manancial - Repositório Digital da UFSM |
collection |
Manancial - Repositório Digital da UFSM |
repository.name.fl_str_mv |
Manancial - Repositório Digital da UFSM - Universidade Federal de Santa Maria (UFSM) |
repository.mail.fl_str_mv |
atendimento.sib@ufsm.br||tedebc@gmail.com |
_version_ |
1805922178379546624 |