Estudo da estabilidade a campo dos pesticidas carbofurano e quincloraque em água de lavoura de arroz irrigado empregando SPE e HPLC-DAD

Detalhes bibliográficos
Ano de defesa: 2007
Autor(a) principal: Peixoto, Sandra Cadore lattes
Orientador(a): Zanella, Renato lattes
Banca de defesa: Primel, Ednei Gilberto lattes, Machado, Sérgio Luiz de Oliveira lattes
Tipo de documento: Dissertação
Tipo de acesso: Acesso aberto
Idioma: por
Instituição de defesa: Universidade Federal de Santa Maria
Programa de Pós-Graduação: Programa de Pós-Graduação em Química
Departamento: Química
País: BR
Palavras-chave em Português:
Palavras-chave em Inglês:
Área do conhecimento CNPq:
Link de acesso: http://repositorio.ufsm.br/handle/1/10378
Resumo: The use of pesticides to control pests, diseases and weeds in crops of agricultural interest aims at the increase of production. The degradation of applied compounds or their conversion into other products, does not necessarily mean the loss of biological activity, and many times, this conversion can result in even more toxic and active products. The study of the pesticides persistence in crops is of great importance in order to evaluate the risks of environmental contamination. In this study, an analytical method for the residual determination of the insecticide carbofuran and the herbicide quinclorac in the water of irrigated rice farming, using SPE and HPLC-DAD, was developed and validated. The method consists of the pre-concentration of the water samples in SPE cartridges with 500 mg of C18 followed by elution with methanol. The extracts were analyzed by HPLC-DAD with a Gemini C18 column and detection at 220 nm for carbofuran and 270 nm for quinclorac. In the method validation, LOD, LOQ, linearity, precision (repeatability and intermediate precision) and accuracy (from the recovery) were evaluated. The LOQ values for the method were 2 μg L-1 for carbofuran and 0.6 μg L-1 for quinclorac. The analytical curves presented linearity between 0.5 and 10.0 mg L-1 for carbofuran and 0.05 and 10.0 mg L-1 for quinclorac, with coefficient of determination values higher than 0.995. The method presented good precision, with RSD values lower than 17.1%, and good accuracy, with recoveries between 82 and 112%. The detection by diode array allowed an adequate confirmation and quantification of the pesticides in study. After validation, the method was applied to analyze samples of water from irrigated rice crops from an experiment carried out at the Campus of the UFSM, where the pesticides, carbofuran and quinclorac, were applied, separately, in the 2006/2007 harvests. The herbicide quinclorac presented greater persistence, with a half life time of approximately 12 days, and residues were found up to 42 days after the application. The insecticide carbofuran was well less persistent, observing residues only up to 5 days after application. For carbofuran, it was not possible to determine the half life time and its metabolite, 3-hydroxycarbofuran, was not found in the samples analyzed.
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spelling 2017-05-252017-05-252007-07-24PEIXOTO, Sandra Cadore. Study of field pesticide stability of carbofuran and quinclorac in the water of irrigated rice crops using SPE and HPLC-DAD. 2007. 129 f. Dissertação (Mestrado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2007.http://repositorio.ufsm.br/handle/1/10378The use of pesticides to control pests, diseases and weeds in crops of agricultural interest aims at the increase of production. The degradation of applied compounds or their conversion into other products, does not necessarily mean the loss of biological activity, and many times, this conversion can result in even more toxic and active products. The study of the pesticides persistence in crops is of great importance in order to evaluate the risks of environmental contamination. In this study, an analytical method for the residual determination of the insecticide carbofuran and the herbicide quinclorac in the water of irrigated rice farming, using SPE and HPLC-DAD, was developed and validated. The method consists of the pre-concentration of the water samples in SPE cartridges with 500 mg of C18 followed by elution with methanol. The extracts were analyzed by HPLC-DAD with a Gemini C18 column and detection at 220 nm for carbofuran and 270 nm for quinclorac. In the method validation, LOD, LOQ, linearity, precision (repeatability and intermediate precision) and accuracy (from the recovery) were evaluated. The LOQ values for the method were 2 μg L-1 for carbofuran and 0.6 μg L-1 for quinclorac. The analytical curves presented linearity between 0.5 and 10.0 mg L-1 for carbofuran and 0.05 and 10.0 mg L-1 for quinclorac, with coefficient of determination values higher than 0.995. The method presented good precision, with RSD values lower than 17.1%, and good accuracy, with recoveries between 82 and 112%. The detection by diode array allowed an adequate confirmation and quantification of the pesticides in study. After validation, the method was applied to analyze samples of water from irrigated rice crops from an experiment carried out at the Campus of the UFSM, where the pesticides, carbofuran and quinclorac, were applied, separately, in the 2006/2007 harvests. The herbicide quinclorac presented greater persistence, with a half life time of approximately 12 days, and residues were found up to 42 days after the application. The insecticide carbofuran was well less persistent, observing residues only up to 5 days after application. For carbofuran, it was not possible to determine the half life time and its metabolite, 3-hydroxycarbofuran, was not found in the samples analyzed.O uso de pesticidas no controle de pragas,doenças e ervas daninhas que prejudicam culturas de interesse agronômico visa o aumento da produção. A degradação dos compostos aplicados ou sua conversão em outros produtos, não significa necessariamente perda da atividade biológica, e muitas vezes, essa conversão pode resultar em produtos ainda mais tóxicos e ativos. O estudo da persistência dos pesticidas nas lavouras é de grande importância para avaliar os riscos de contaminação ambiental. Neste trabalho desenvolveu-se e validou-se um método analítico, utilizando SPE e HPLC-DAD, para a determinação residual do inseticida carbofurano e do herbicida quincloraque em água de lavoura de arroz irrigado. O método consiste na pré-concentração das amostras de água em cartuchos de SPE contendo 500 mg de C18 seguida da eluição com metanol. Os extratos foram analisados por HPLC-DAD com coluna Gemini C18 e detecção em 220 nm para o carbofurano e 270 nm para o quincloraque. Na validação do método avaliou-se LOD, LOQ, linearidade, precisão (repetitividade e precisão intermediária) e exatidão, avaliada pela recuperação. Os valores de LOQ para o método foram 2 μg L-1 para o carbofurano e 0,6 μg L-1 para o quincloraque. As curvas analíticas apresentaram linearidade entre 0,5 e 10,0 mg L-1 para o carbofurano e 0,05 e 10,0 mg L-1 para o quincloraque, com valores de coeficiente de determinação maiores que 0,995. O método apresentou boa precisão, com valores de RSD inferiores a 17,1%, e boa exatidão, com recuperações entre 82 e 112%. A detecção por arranjo de diodos permitiu confirmação e a quantificação de forma adequada dos pesticidas em estudo. Após validado, o método foi aplicado para analisar amostras de água de lavoura de arroz irrigado de um experimento realizado no Campus da UFSM, onde foram aplicados separadamente os pesticidas carbofurano e quincloraque, nas safras 2006/2007. O herbicida quincloraque apresentou maior persistência, com tempo de meia-vida de aproximadamente 12 dias, e foram encontrados resíduos até o 42º dia após aplicação. O inseticida carbofurano foi bem menos persistente, observando-se resíduos apenas até 5 dias após aplicação. Para carbofurano não foi possível determinar o tempo de meia-vida e o seu metabólito, 3-hidroxicarbofurano, não foi encontrado nas amostras analisadas.application/pdfporUniversidade Federal de Santa MariaPrograma de Pós-Graduação em QuímicaUFSMBRQuímicaPesticidasÁguaHPLC-DADPesticidesWaterHPLC-DADCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICAEstudo da estabilidade a campo dos pesticidas carbofurano e quincloraque em água de lavoura de arroz irrigado empregando SPE e HPLC-DADStudy of field pesticide stability of carbofuran and quinclorac in the water of irrigated rice crops using SPE and HPLC-DADinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisZanella, Renatohttp://lattes.cnpq.br/2541865299438479Primel, Ednei Gilbertohttp://lattes.cnpq.br/3259602390948297Machado, Sérgio Luiz de Oliveirahttp://lattes.cnpq.br/0360886006002113http://lattes.cnpq.br/0051729840313401Peixoto, Sandra Cadore1006000000004005005005005000aa2baab-94e8-4d3d-bbb2-85495ba77db575bc22d9-7d4a-4784-8060-4a6377bc8db1baeb8541-95af-4405-96c9-db07639f33f6d76f65d6-31b5-4a33-a150-b5891e3e81d4info:eu-repo/semantics/openAccessreponame:Biblioteca Digital de Teses e Dissertações do UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMORIGINALSANDRA PEIXOTO.pdfapplication/pdf2405739http://repositorio.ufsm.br/bitstream/1/10378/1/SANDRA%20PEIXOTO.pdf9d5592d3fb4c36c95736279ef057c1b5MD51TEXTSANDRA PEIXOTO.pdf.txtSANDRA PEIXOTO.pdf.txtExtracted texttext/plain178594http://repositorio.ufsm.br/bitstream/1/10378/2/SANDRA%20PEIXOTO.pdf.txt10f0bb2ec93518322133f111f0d442cfMD52THUMBNAILSANDRA PEIXOTO.pdf.jpgSANDRA PEIXOTO.pdf.jpgIM Thumbnailimage/jpeg6363http://repositorio.ufsm.br/bitstream/1/10378/3/SANDRA%20PEIXOTO.pdf.jpgc9a191538eea5d92a9c0cbc3fbeae8bbMD531/103782023-02-01 13:27:33.305oai:repositorio.ufsm.br:1/10378Biblioteca Digital de Teses e Dissertaçõeshttps://repositorio.ufsm.br/ONGhttps://repositorio.ufsm.br/oai/requestatendimento.sib@ufsm.br||tedebc@gmail.comopendoar:2023-02-01T16:27:33Biblioteca Digital de Teses e Dissertações do UFSM - Universidade Federal de Santa Maria (UFSM)false
dc.title.por.fl_str_mv Estudo da estabilidade a campo dos pesticidas carbofurano e quincloraque em água de lavoura de arroz irrigado empregando SPE e HPLC-DAD
dc.title.alternative.eng.fl_str_mv Study of field pesticide stability of carbofuran and quinclorac in the water of irrigated rice crops using SPE and HPLC-DAD
title Estudo da estabilidade a campo dos pesticidas carbofurano e quincloraque em água de lavoura de arroz irrigado empregando SPE e HPLC-DAD
spellingShingle Estudo da estabilidade a campo dos pesticidas carbofurano e quincloraque em água de lavoura de arroz irrigado empregando SPE e HPLC-DAD
Peixoto, Sandra Cadore
Pesticidas
Água
HPLC-DAD
Pesticides
Water
HPLC-DAD
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA
title_short Estudo da estabilidade a campo dos pesticidas carbofurano e quincloraque em água de lavoura de arroz irrigado empregando SPE e HPLC-DAD
title_full Estudo da estabilidade a campo dos pesticidas carbofurano e quincloraque em água de lavoura de arroz irrigado empregando SPE e HPLC-DAD
title_fullStr Estudo da estabilidade a campo dos pesticidas carbofurano e quincloraque em água de lavoura de arroz irrigado empregando SPE e HPLC-DAD
title_full_unstemmed Estudo da estabilidade a campo dos pesticidas carbofurano e quincloraque em água de lavoura de arroz irrigado empregando SPE e HPLC-DAD
title_sort Estudo da estabilidade a campo dos pesticidas carbofurano e quincloraque em água de lavoura de arroz irrigado empregando SPE e HPLC-DAD
author Peixoto, Sandra Cadore
author_facet Peixoto, Sandra Cadore
author_role author
dc.contributor.advisor1.fl_str_mv Zanella, Renato
dc.contributor.advisor1Lattes.fl_str_mv http://lattes.cnpq.br/2541865299438479
dc.contributor.referee1.fl_str_mv Primel, Ednei Gilberto
dc.contributor.referee1Lattes.fl_str_mv http://lattes.cnpq.br/3259602390948297
dc.contributor.referee2.fl_str_mv Machado, Sérgio Luiz de Oliveira
dc.contributor.referee2Lattes.fl_str_mv http://lattes.cnpq.br/0360886006002113
dc.contributor.authorLattes.fl_str_mv http://lattes.cnpq.br/0051729840313401
dc.contributor.author.fl_str_mv Peixoto, Sandra Cadore
contributor_str_mv Zanella, Renato
Primel, Ednei Gilberto
Machado, Sérgio Luiz de Oliveira
dc.subject.por.fl_str_mv Pesticidas
Água
HPLC-DAD
topic Pesticidas
Água
HPLC-DAD
Pesticides
Water
HPLC-DAD
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA
dc.subject.eng.fl_str_mv Pesticides
Water
HPLC-DAD
dc.subject.cnpq.fl_str_mv CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA
description The use of pesticides to control pests, diseases and weeds in crops of agricultural interest aims at the increase of production. The degradation of applied compounds or their conversion into other products, does not necessarily mean the loss of biological activity, and many times, this conversion can result in even more toxic and active products. The study of the pesticides persistence in crops is of great importance in order to evaluate the risks of environmental contamination. In this study, an analytical method for the residual determination of the insecticide carbofuran and the herbicide quinclorac in the water of irrigated rice farming, using SPE and HPLC-DAD, was developed and validated. The method consists of the pre-concentration of the water samples in SPE cartridges with 500 mg of C18 followed by elution with methanol. The extracts were analyzed by HPLC-DAD with a Gemini C18 column and detection at 220 nm for carbofuran and 270 nm for quinclorac. In the method validation, LOD, LOQ, linearity, precision (repeatability and intermediate precision) and accuracy (from the recovery) were evaluated. The LOQ values for the method were 2 μg L-1 for carbofuran and 0.6 μg L-1 for quinclorac. The analytical curves presented linearity between 0.5 and 10.0 mg L-1 for carbofuran and 0.05 and 10.0 mg L-1 for quinclorac, with coefficient of determination values higher than 0.995. The method presented good precision, with RSD values lower than 17.1%, and good accuracy, with recoveries between 82 and 112%. The detection by diode array allowed an adequate confirmation and quantification of the pesticides in study. After validation, the method was applied to analyze samples of water from irrigated rice crops from an experiment carried out at the Campus of the UFSM, where the pesticides, carbofuran and quinclorac, were applied, separately, in the 2006/2007 harvests. The herbicide quinclorac presented greater persistence, with a half life time of approximately 12 days, and residues were found up to 42 days after the application. The insecticide carbofuran was well less persistent, observing residues only up to 5 days after application. For carbofuran, it was not possible to determine the half life time and its metabolite, 3-hydroxycarbofuran, was not found in the samples analyzed.
publishDate 2007
dc.date.issued.fl_str_mv 2007-07-24
dc.date.accessioned.fl_str_mv 2017-05-25
dc.date.available.fl_str_mv 2017-05-25
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dc.identifier.citation.fl_str_mv PEIXOTO, Sandra Cadore. Study of field pesticide stability of carbofuran and quinclorac in the water of irrigated rice crops using SPE and HPLC-DAD. 2007. 129 f. Dissertação (Mestrado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2007.
dc.identifier.uri.fl_str_mv http://repositorio.ufsm.br/handle/1/10378
identifier_str_mv PEIXOTO, Sandra Cadore. Study of field pesticide stability of carbofuran and quinclorac in the water of irrigated rice crops using SPE and HPLC-DAD. 2007. 129 f. Dissertação (Mestrado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2007.
url http://repositorio.ufsm.br/handle/1/10378
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