Estudo dos par?metros de otimiza??o e aplica??o da micro-extra??o em fase s?lida para determina??o de agrot?xicos organoclorados em alface (Lactuva sativa L.) e ?gua
Ano de defesa: | 2004 |
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Autor(a) principal: | |
Orientador(a): | |
Banca de defesa: | , , , , |
Tipo de documento: | Tese |
Tipo de acesso: | Acesso aberto |
Idioma: | por |
Instituição de defesa: |
Universidade Federal Rural do Rio de Janeiro
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Programa de Pós-Graduação: |
Programa de P?s-Gradua??o em Qu?mica
|
Departamento: |
Instituto de Ci?ncias Exatas
|
País: |
Brasil
|
Palavras-chave em Português: | |
Área do conhecimento CNPq: | |
Link de acesso: | https://tede.ufrrj.br/jspui/handle/jspui/4309 |
Resumo: | Predatory practice of agricultural production has led to the accumulation of agricultural pesticides in the environment, contaminating the ground, water resources and even virgin areas, those that never received application agrochemicals. Although many of the carcinogenic, toxic agrochemicals, considered as highly persistent pollutants have already been forbidden in Brazil (DDT, BHC, etc), there are others, less persistent, that can be degraded into others, as toxic, or even more toxic. Currently, the quality of all the foodstuffs is defined not only by its nutritional composition and state of conservation, but also by the levels of residual substances, toxic to man. It is important to develop and apply the philosophy of the good agronomic practices; environmental education; consumer education; legislation with strong repression for the infractors; routine fiscal analyses by competent official agencies, control of levels of the maximum residual limits (MRL) in foodstuffs and water for human consumption. With this end, a simple methodology, efficient and economic, was developed, based in the use of solid phase micro-extraction (SPME) for determination of pesticides (Lindane?, Aldrin?, DDE, Dieldrin?, TDE and Mirex?) in samples of water and of lettuce, using gas chromatography with electron capture detector (GC-ECD). This method can be applied in small volumes of sample (ca. 1,0 mL), it does no need the use of solvents and, in the multi-residue analysis there is no need to modify the ionic force or pH of the matrix. Of the analyzed samples, after screening, the organochlorine pesticide DDE was found only in the samples of lettuce, in the range 29 ? 262 ng/g, with RSD average of 13 %. The accuracy of the quantification of DDE in the samples of lettuce was tested by % of recovery and comparison with an official method for determination of pesticides, when recoveries in the range 93 ? 96 % with average RSD of 14 % were obtained. Using ELL extraction (official method) a value for the DDE in the four samples of lettuce in the band of 25 ? 240 ng/g was found, with average RSD of 14 %, and recovery between 92 and 98 %, with RSD average of 12 %. The two methods do not differ statistically, to a level of confidence of 95 %. The presence of DDE as contaminant can be related with the application of DDT instead of DDE itself, since DDT was used world-wide in wide scale up to 1985, when its use was forbidden in Brazil. The results obtained for the lettuce samples are indicative of the environmental persistence of organochlorine pesticides |
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Ferreira, Aur?lio Baird Buarquehttp://lattes.cnpq.br/5526484175547597Godoy, Ronoel Luiz De OliveiraFerreira, Aur?lio Baird BuarqueGodoy, Ronoel Luiz de OliveiraBarra, Cristina MariaCastro, Izabela Miranda deMaria, Carlos Alberto B. dehttp://lattes.cnpq.br/7401298194086731Quinteiro, Leila Martins da Costa2020-12-29T17:41:59Z2004-10-29QUJINTEIRo, Leila Martins da Costa. Estudo dos par?metros de otimiza??o e aplica??o da micro-extra??o em fase s?lida para determina??o de agrot?xicos organoclorados em alface (Lactuva sativa L.) e ?gua. 2004. 167 f. Tese (Doutorado em Qu?mica) - Instituto de Ci?ncias Exatas, Universidade Federal Rural do Rio de Janeiro, Serop?dica - RJ, 2004.https://tede.ufrrj.br/jspui/handle/jspui/4309Predatory practice of agricultural production has led to the accumulation of agricultural pesticides in the environment, contaminating the ground, water resources and even virgin areas, those that never received application agrochemicals. Although many of the carcinogenic, toxic agrochemicals, considered as highly persistent pollutants have already been forbidden in Brazil (DDT, BHC, etc), there are others, less persistent, that can be degraded into others, as toxic, or even more toxic. Currently, the quality of all the foodstuffs is defined not only by its nutritional composition and state of conservation, but also by the levels of residual substances, toxic to man. It is important to develop and apply the philosophy of the good agronomic practices; environmental education; consumer education; legislation with strong repression for the infractors; routine fiscal analyses by competent official agencies, control of levels of the maximum residual limits (MRL) in foodstuffs and water for human consumption. With this end, a simple methodology, efficient and economic, was developed, based in the use of solid phase micro-extraction (SPME) for determination of pesticides (Lindane?, Aldrin?, DDE, Dieldrin?, TDE and Mirex?) in samples of water and of lettuce, using gas chromatography with electron capture detector (GC-ECD). This method can be applied in small volumes of sample (ca. 1,0 mL), it does no need the use of solvents and, in the multi-residue analysis there is no need to modify the ionic force or pH of the matrix. Of the analyzed samples, after screening, the organochlorine pesticide DDE was found only in the samples of lettuce, in the range 29 ? 262 ng/g, with RSD average of 13 %. The accuracy of the quantification of DDE in the samples of lettuce was tested by % of recovery and comparison with an official method for determination of pesticides, when recoveries in the range 93 ? 96 % with average RSD of 14 % were obtained. Using ELL extraction (official method) a value for the DDE in the four samples of lettuce in the band of 25 ? 240 ng/g was found, with average RSD of 14 %, and recovery between 92 and 98 %, with RSD average of 12 %. The two methods do not differ statistically, to a level of confidence of 95 %. The presence of DDE as contaminant can be related with the application of DDT instead of DDE itself, since DDT was used world-wide in wide scale up to 1985, when its use was forbidden in Brazil. The results obtained for the lettuce samples are indicative of the environmental persistence of organochlorine pesticidesA pr?tica predat?ria da produ??o agr?cola tem levado ao a c?mulo de defensivos agr?colas no meio ambiente, contaminando o solo, os espelhos d??gua e at? as ?reas virgens, ou seja, aquelas que nunca receberam aplica??o de pesticidas. Embora os agrot?xicos mais carcinog?nicos, considerados poluentes de grande persist?ncia, j? tenham sido proibidos no Brasil (DDT, BHC, etc), existem ainda outros, menos persistentes, que podem se degradar originando outros t?o ou mais t?xicos. Atualmente, a qualidade de todos os alimentos est? intrinsecamente ligada, n?o s? ? composi??o nutricional e ao estado de conserva??o, mas tamb?m aos n?veis residuais de elementos t?xicos ao homem. ? importante procurar desenvolver e aplicar a filosofia das boas t?cnicas agron?micas; educa??o ambiental; educa??o do consumidor; legisla??o com repress?o pesada sobre os infratores; an?lises fiscais rotineiras por ?rg?os oficiais competentes, para controle dos teores dos limites residuais m?ximos (LMR) em alimentos e em ?guas de consumo humano. Com este fim foi desenvolvida uma metodologia simples, eficiente e econ?mica baseada na utiliza??o de micro-extra??o em fase s?lida (MFES) para determina??o dos agrot?xicos (Lindane?, Aldrin?, DDE, Dieldrin?, TDE and Mirex?) em amostras de ?gua e alface por cromatografia gasosa com detector de captura de el?trons(CG-DCE). Este m?todo pode ser aplicado em pequenos volumes de amostra (em torno de 1,0 mL) e na necessita de uso de solventes e na an?lise de multi-res?duo n?o h? necessidade de modificar a for?a i?nica ou o pH da matriz. Das amostras analisadas, ap?s screening, foi encontrado o agrot?xico organoclorado DDE somente nas amostras de alface, na faixa entre 29- 262 ng/g, com % CV m?dio de 13 %. A exatid?o da quantifica??o de DDE nas amostras de alface foi testada pela % de recupera??o e compara??o com um m?todo oficial para determina??o de agrot?xicos, obtendo-se uma recupera??o entre 93- 96 % com %CV m?dio de 14 %. Pela extra??o ELL (oficial) foi encontrado um valor de para o DDE nas quatro amostras de alface na faixa de 25 ? 240 ng/g, com %CV m?dio de 14 %, e recupera??o entre 92 ? 98 %, com CV m?dio de 12 %. Os dois m?todos n?o diferem estatisticamente entre si, a um n?vel da confian?a de 95 %. A presen?a de DDE como contaminante pode estar relacionada com a aplica??o de DDT em vez do pr?prio DDE, pois o DDT foi utilizado mundialmente em larga escala at? 1985, quando o seu uso foi proibido no Brasil. O resultado obtido para as amostras de alface ? indicativo de persist?ncia ambiental de agrot?xicos organoclorados.Submitted by Celso Magalhaes (celsomagalhaes@ufrrj.br) on 2020-12-29T17:41:59Z No. of bitstreams: 1 2004 - Leila Martins da Costa Quinteiro.pdf: 948696 bytes, checksum: ee5d43ffd8de2a89e2ed68b26eee9f25 (MD5)Made available in DSpace on 2020-12-29T17:41:59Z (GMT). No. of bitstreams: 1 2004 - Leila Martins da Costa Quinteiro.pdf: 948696 bytes, checksum: ee5d43ffd8de2a89e2ed68b26eee9f25 (MD5) Previous issue date: 2004-10-29application/pdfhttps://tede.ufrrj.br/retrieve/63675/2004%20-%20Leila%20Martins%20da%20Costa%20Quinteiro.pdf.jpgporUniversidade Federal Rural do Rio de JaneiroPrograma de P?s-Gradua??o em Qu?micaUFRRJBrasilInstituto de Ci?ncias ExatasAGUILAR, A.; PE?ALVER, E.; POCURULL, E.; FERR?, F.; BORRULL, R.M. MARC?. Optimization of spme conditions using a response methodology to determine organochlorine pesticides surface methodology to detrmine organochlorine pesticides in water by gas chromatography ande electron-capture detection. Journal of Chromatography A, v.844, n.425-432, 1999. ANALYTIVAL METHODS COMMITTEE. Principles of Data Quality Control in Chemical Analysis. Analyst, v.114, p. 1497 ? 1503, 1989. BOYD-BOLAND, A.; MAGDIC S.; PAWLISZYN, J. B. Simultaneous determinations of 60 pesticides in water using solid-phase microextraction and gas chromatographymass spectrometry. Analyst, v.121, p.929-938, 1996. BRASIL. Minist?rio da Sa?de. Ag?ncia Nacional de Vigil?ncia Sanit?ria (ANVISA). [2004]. Dispon?vel em:<http:// www.anvisa.gov.br>.Acesso em: 05 ab. 2004. COLLINS C. H.; BRAGA, G. L.; BONATO, S. P. Introdu??o a m?todos cromatogr?ficos.6.ed. Campinas: Ed. Unicamp,1996. 279 p. GOMES, F.P. Curso de estat?stica experimental.14. Ed. Piracicaba: Ed. Universidade de S?o Paulo, Escola Superior de Agricultura Luiz de Queiroz, 2000.477p. HOLANDA. Ministery of Public Health, Welfare and Sport. Analytical methods for pesticide residues in foodstuffs. 6.Ed. Netherland: Ed. Van Zoonen, P. Part I, p.4. 1996. INMETRO - Instituto Nacional de Metrologia e Qualidade Industrial, Orienta??o sobre valida??o de m?todos de ensaios qu?micos. DOQ-CGCRE-008. 35p. Mar. 2003. IUPAC. Analytical methods committee ? Recommendations for definitions, estimation and used of the detection limits. Analyst, v.112, p.199-204, 1987. LEITE, F. Valida??o em an?lise qu?mica. 3.ed.Campinas:Ed.?tomo, 1998, 224p. MAGDIC, S.; PAWLISZYN, J. Analysis of organochlorine pesticides using SPME, Journal of Chromatography A, v.723, p.111-122, 1996. MILLER, J.C.; MILLER, J.N. Estad?stica para qu?mica anal?tica. 2.ed. Delaware: Ed. Addison-Wesley Iberoamerican, 1993, 211p. NOBRE, A. LR. Determina??o de metais em m?is por voltametria de redissolu??o an?dica e adsortiva. 1990. 182p. Disserta??o (Mestrado) - Departamento de Qu?mica e F?sica Molecular, Universidade de S?o Paulo, S?o Carlos,1990. PAWLISZYN, J. Solid phase microextraction ? Theory and practice. New York: John Wiley & Sons, Inc, 1997.247p. 166 SIMPL?CIO, A. L.; VILAS BOAS, L. Validation of a SPME method for the determination of organophosphorus pesticides in fruitsand fruit juice. Journal of Chromatography A, v.833, p.35-42, 1999. SOUZA CRUZ. Protocolo m?nimo para valida??o de m?todos anal?ticos. Centro de Pesquisa e Desenvolvimento. Fev. 2003, 11p. SUPELCO. Manual de instru??es.2003. YOKOMIZO, Y.; LARA, W. H.; PUGA, F.; BATISTA, G.; CARVALHO, P. R. N.; BARRETO, H. C.; MALTONE, C. A.; DOEGE, M. Res?duos de pesticidas em alimentos. 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dc.title.por.fl_str_mv |
Estudo dos par?metros de otimiza??o e aplica??o da micro-extra??o em fase s?lida para determina??o de agrot?xicos organoclorados em alface (Lactuva sativa L.) e ?gua |
title |
Estudo dos par?metros de otimiza??o e aplica??o da micro-extra??o em fase s?lida para determina??o de agrot?xicos organoclorados em alface (Lactuva sativa L.) e ?gua |
spellingShingle |
Estudo dos par?metros de otimiza??o e aplica??o da micro-extra??o em fase s?lida para determina??o de agrot?xicos organoclorados em alface (Lactuva sativa L.) e ?gua Quinteiro, Leila Martins da Costa Qu?mica Qu?mica |
title_short |
Estudo dos par?metros de otimiza??o e aplica??o da micro-extra??o em fase s?lida para determina??o de agrot?xicos organoclorados em alface (Lactuva sativa L.) e ?gua |
title_full |
Estudo dos par?metros de otimiza??o e aplica??o da micro-extra??o em fase s?lida para determina??o de agrot?xicos organoclorados em alface (Lactuva sativa L.) e ?gua |
title_fullStr |
Estudo dos par?metros de otimiza??o e aplica??o da micro-extra??o em fase s?lida para determina??o de agrot?xicos organoclorados em alface (Lactuva sativa L.) e ?gua |
title_full_unstemmed |
Estudo dos par?metros de otimiza??o e aplica??o da micro-extra??o em fase s?lida para determina??o de agrot?xicos organoclorados em alface (Lactuva sativa L.) e ?gua |
title_sort |
Estudo dos par?metros de otimiza??o e aplica??o da micro-extra??o em fase s?lida para determina??o de agrot?xicos organoclorados em alface (Lactuva sativa L.) e ?gua |
author |
Quinteiro, Leila Martins da Costa |
author_facet |
Quinteiro, Leila Martins da Costa |
author_role |
author |
dc.contributor.advisor1.fl_str_mv |
Ferreira, Aur?lio Baird Buarque |
dc.contributor.advisor1Lattes.fl_str_mv |
http://lattes.cnpq.br/5526484175547597 |
dc.contributor.advisor-co1.fl_str_mv |
Godoy, Ronoel Luiz De Oliveira |
dc.contributor.referee1.fl_str_mv |
Ferreira, Aur?lio Baird Buarque |
dc.contributor.referee2.fl_str_mv |
Godoy, Ronoel Luiz de Oliveira |
dc.contributor.referee3.fl_str_mv |
Barra, Cristina Maria |
dc.contributor.referee4.fl_str_mv |
Castro, Izabela Miranda de |
dc.contributor.referee5.fl_str_mv |
Maria, Carlos Alberto B. de |
dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/7401298194086731 |
dc.contributor.author.fl_str_mv |
Quinteiro, Leila Martins da Costa |
contributor_str_mv |
Ferreira, Aur?lio Baird Buarque Godoy, Ronoel Luiz De Oliveira Ferreira, Aur?lio Baird Buarque Godoy, Ronoel Luiz de Oliveira Barra, Cristina Maria Castro, Izabela Miranda de Maria, Carlos Alberto B. de |
dc.subject.por.fl_str_mv |
Qu?mica |
topic |
Qu?mica Qu?mica |
dc.subject.cnpq.fl_str_mv |
Qu?mica |
description |
Predatory practice of agricultural production has led to the accumulation of agricultural pesticides in the environment, contaminating the ground, water resources and even virgin areas, those that never received application agrochemicals. Although many of the carcinogenic, toxic agrochemicals, considered as highly persistent pollutants have already been forbidden in Brazil (DDT, BHC, etc), there are others, less persistent, that can be degraded into others, as toxic, or even more toxic. Currently, the quality of all the foodstuffs is defined not only by its nutritional composition and state of conservation, but also by the levels of residual substances, toxic to man. It is important to develop and apply the philosophy of the good agronomic practices; environmental education; consumer education; legislation with strong repression for the infractors; routine fiscal analyses by competent official agencies, control of levels of the maximum residual limits (MRL) in foodstuffs and water for human consumption. With this end, a simple methodology, efficient and economic, was developed, based in the use of solid phase micro-extraction (SPME) for determination of pesticides (Lindane?, Aldrin?, DDE, Dieldrin?, TDE and Mirex?) in samples of water and of lettuce, using gas chromatography with electron capture detector (GC-ECD). This method can be applied in small volumes of sample (ca. 1,0 mL), it does no need the use of solvents and, in the multi-residue analysis there is no need to modify the ionic force or pH of the matrix. Of the analyzed samples, after screening, the organochlorine pesticide DDE was found only in the samples of lettuce, in the range 29 ? 262 ng/g, with RSD average of 13 %. The accuracy of the quantification of DDE in the samples of lettuce was tested by % of recovery and comparison with an official method for determination of pesticides, when recoveries in the range 93 ? 96 % with average RSD of 14 % were obtained. Using ELL extraction (official method) a value for the DDE in the four samples of lettuce in the band of 25 ? 240 ng/g was found, with average RSD of 14 %, and recovery between 92 and 98 %, with RSD average of 12 %. The two methods do not differ statistically, to a level of confidence of 95 %. The presence of DDE as contaminant can be related with the application of DDT instead of DDE itself, since DDT was used world-wide in wide scale up to 1985, when its use was forbidden in Brazil. The results obtained for the lettuce samples are indicative of the environmental persistence of organochlorine pesticides |
publishDate |
2004 |
dc.date.issued.fl_str_mv |
2004-10-29 |
dc.date.accessioned.fl_str_mv |
2020-12-29T17:41:59Z |
dc.type.status.fl_str_mv |
info:eu-repo/semantics/publishedVersion |
dc.type.driver.fl_str_mv |
info:eu-repo/semantics/doctoralThesis |
format |
doctoralThesis |
status_str |
publishedVersion |
dc.identifier.citation.fl_str_mv |
QUJINTEIRo, Leila Martins da Costa. Estudo dos par?metros de otimiza??o e aplica??o da micro-extra??o em fase s?lida para determina??o de agrot?xicos organoclorados em alface (Lactuva sativa L.) e ?gua. 2004. 167 f. Tese (Doutorado em Qu?mica) - Instituto de Ci?ncias Exatas, Universidade Federal Rural do Rio de Janeiro, Serop?dica - RJ, 2004. |
dc.identifier.uri.fl_str_mv |
https://tede.ufrrj.br/jspui/handle/jspui/4309 |
identifier_str_mv |
QUJINTEIRo, Leila Martins da Costa. Estudo dos par?metros de otimiza??o e aplica??o da micro-extra??o em fase s?lida para determina??o de agrot?xicos organoclorados em alface (Lactuva sativa L.) e ?gua. 2004. 167 f. Tese (Doutorado em Qu?mica) - Instituto de Ci?ncias Exatas, Universidade Federal Rural do Rio de Janeiro, Serop?dica - RJ, 2004. |
url |
https://tede.ufrrj.br/jspui/handle/jspui/4309 |
dc.language.iso.fl_str_mv |
por |
language |
por |
dc.relation.references.por.fl_str_mv |
AGUILAR, A.; PE?ALVER, E.; POCURULL, E.; FERR?, F.; BORRULL, R.M. MARC?. Optimization of spme conditions using a response methodology to determine organochlorine pesticides surface methodology to detrmine organochlorine pesticides in water by gas chromatography ande electron-capture detection. Journal of Chromatography A, v.844, n.425-432, 1999. ANALYTIVAL METHODS COMMITTEE. Principles of Data Quality Control in Chemical Analysis. Analyst, v.114, p. 1497 ? 1503, 1989. BOYD-BOLAND, A.; MAGDIC S.; PAWLISZYN, J. B. Simultaneous determinations of 60 pesticides in water using solid-phase microextraction and gas chromatographymass spectrometry. Analyst, v.121, p.929-938, 1996. BRASIL. Minist?rio da Sa?de. Ag?ncia Nacional de Vigil?ncia Sanit?ria (ANVISA). [2004]. Dispon?vel em:<http:// www.anvisa.gov.br>.Acesso em: 05 ab. 2004. COLLINS C. H.; BRAGA, G. L.; BONATO, S. P. Introdu??o a m?todos cromatogr?ficos.6.ed. Campinas: Ed. Unicamp,1996. 279 p. GOMES, F.P. Curso de estat?stica experimental.14. Ed. Piracicaba: Ed. Universidade de S?o Paulo, Escola Superior de Agricultura Luiz de Queiroz, 2000.477p. HOLANDA. Ministery of Public Health, Welfare and Sport. Analytical methods for pesticide residues in foodstuffs. 6.Ed. Netherland: Ed. Van Zoonen, P. Part I, p.4. 1996. INMETRO - Instituto Nacional de Metrologia e Qualidade Industrial, Orienta??o sobre valida??o de m?todos de ensaios qu?micos. DOQ-CGCRE-008. 35p. Mar. 2003. IUPAC. Analytical methods committee ? Recommendations for definitions, estimation and used of the detection limits. Analyst, v.112, p.199-204, 1987. LEITE, F. Valida??o em an?lise qu?mica. 3.ed.Campinas:Ed.?tomo, 1998, 224p. MAGDIC, S.; PAWLISZYN, J. Analysis of organochlorine pesticides using SPME, Journal of Chromatography A, v.723, p.111-122, 1996. MILLER, J.C.; MILLER, J.N. Estad?stica para qu?mica anal?tica. 2.ed. Delaware: Ed. Addison-Wesley Iberoamerican, 1993, 211p. NOBRE, A. LR. Determina??o de metais em m?is por voltametria de redissolu??o an?dica e adsortiva. 1990. 182p. Disserta??o (Mestrado) - Departamento de Qu?mica e F?sica Molecular, Universidade de S?o Paulo, S?o Carlos,1990. PAWLISZYN, J. Solid phase microextraction ? Theory and practice. New York: John Wiley & Sons, Inc, 1997.247p. 166 SIMPL?CIO, A. L.; VILAS BOAS, L. Validation of a SPME method for the determination of organophosphorus pesticides in fruitsand fruit juice. Journal of Chromatography A, v.833, p.35-42, 1999. SOUZA CRUZ. Protocolo m?nimo para valida??o de m?todos anal?ticos. Centro de Pesquisa e Desenvolvimento. Fev. 2003, 11p. SUPELCO. Manual de instru??es.2003. YOKOMIZO, Y.; LARA, W. H.; PUGA, F.; BATISTA, G.; CARVALHO, P. R. N.; BARRETO, H. C.; MALTONE, C. A.; DOEGE, M. Res?duos de pesticidas em alimentos. Campinas:Ital, 1985. 226p. |
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info:eu-repo/semantics/openAccess |
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openAccess |
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Universidade Federal Rural do Rio de Janeiro |
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Programa de P?s-Gradua??o em Qu?mica |
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UFRRJ |
dc.publisher.country.fl_str_mv |
Brasil |
dc.publisher.department.fl_str_mv |
Instituto de Ci?ncias Exatas |
publisher.none.fl_str_mv |
Universidade Federal Rural do Rio de Janeiro |
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