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Master's Dissertation
DOI
https://doi.org/10.11606/D.11.1981.tde-20240301-152652
Document
Author
Full name
José Poleze Soares Novo
Institute/School/College
Date of Defense
Published
Piracicaba, 1981
Supervisor
Title in Portuguese
Resíduos de DDT e endrin em folhas, caroços, óleos e farelos de algodoeiro (Gossypium hirsutm L., cultivar IAC - 17), determinados por cromatografia em fase gasosa
Keywords in Portuguese
ALGODÃO
CROMATOGRAFIA GASOSA
RESÍDUOS DE INSETICIDAS
Abstract in Portuguese
Procurou-se estudar o comportamento dos resduos de DDT e endrin em folhas de algodoeiro e determinar os resíduos desses inseticidas em caroços de algodão na ocasião da colheita, bem como sua distribuição nos produtos do processamento dos caroços. O experimento foi instalado no município de Tietê, SP, utilizando algodão do cultivar IAC-17. Foram realizadas três pulverizações (76, 56 e 31 dias antes da colheita) nas dosagens de 2000g de i.a. DDT/ha (500g de DDT 50% PM/ 100 litros de água) e 800g de i.a. endrin/ha (600ml de Endrex 20, CE/100 litros de água). As folhas foram amostradas 3 dias após cada aplicação e 20, 25 e 31 dias após as 1ª, 2ª e 3ª aplicações, respectivamente. Os caroços foram colhidos 31 dias após a 3ª aplicação. O método de análise de resíduos em materiais não gordurosos (folhas e farelos) constou de extração com acetonitrilo e água, e purificação através de partição em éter de petróleo e limpeza em coluna de florisil, eluida com uma mistura de éter etílico e éter de petróleo. O método para materiais gordurosos (caroços e Óleos) constou de extração com ace tonitrilo, água e Óxido de alumínio neutro, partição em éter de petróleo e limpeza em coluna de florisil eluida com uma mistura de éter de petróleo, diclorometano e acetonitrilo. Os extratos foram concentrados e injetados em cromatógrafo a gás equipado com coluna de vidro (2,5% de SE-30/Chromosorb WHP) e detector de captura de elétrons (Ni63). Os limites de detecção obtidos foram 0,005ppm para DDT e 0,002ppm para endrin em mate riais não gordurosos e 0,005 ppm para ambos em materiais gordurosos. O DDT foi menos persistente em folhas, apresentando depósitos iniciais muito sensíveis a fatores climáticos, principalmente chuva e vento. Na Última amostragem, os resíduos em folhas foram 4,208ppm de DDT total (soma de p,p’-DDE , o,p’-DDT e p,p’-DDT) e 7,92ppm de endrin. Em caroços, a persistência dos dois inseticidas foi semelhante, considerando a quantidade aplicada e o resíduo final, que foi 0,09lppm de DDT total e 0,035ppm de endrin. O Óleo bruto apresentou resíduos mais altos, 0,200ppm de DDT e 0,086ppm de endrin, o que representa cerca de metade do total dos inseticidas contidos nos caroços. No farelo os resíduos foram menores, 0,025ppm de DDT total e 0,010 ppm de endrin. Os resultados em caroços, respeitado o período de carência de 30 dias, estiveram abaixo dos limites de tolerância (1,0 ppm para DDT e 0,1 ppm para endrin) estabelecidos pela legislação vigente no Brasil.
Title in English
DDT and endrin residues in leaves, seeds, oil and meal of cotton cultivar IAC-17 (Gossypium hirsutm L.) determined by gas chromatography
Abstract in English
The residues behaviour of DDT and endrin in/on cotton leaves were studied. Determinations of these residues were also made in cotton seeds, oil and meal, after the harvest and the processing of the seeds. The experiment was installed in Tietê County, State of São Paulo, Brazil, with cotton seeds of IAC-17 cultivar. At 76, 56 and 31 days before the harvesting, the plants were sprayed at the rates of 2,000g a.i. DDT/ha (500 g DDT 50% WP/100 1 water ) and 800 g a.i. endrin/ha ( 600 ml Endrex 20% EC/ 100 1 water ). Samples of leaves were collected 3 days after each application and 20, 25 and 31 days after the 1st, 2nd and 3rd application, respectively. Cotton see d s were harvested 31 days after the 3rd application. The residues in nonfatty materials ( leaves and meal) were extracted with acetonitrile and distilled water and purified by solvent partition with petroleum ether plus florisil column, eluted with a mixture of ethyl ether and petroleum ether. The residues in fatty materials (cotton seeds and oil) were extracted with acetonitrile, distilled water and neutral aluminium oxide and purified by solvent partition with petroleum ether plus florisil column eluted with a mixture of petroleum ether, dichloromethane and acetonitrile. The ex tract was concentrated and injected in a gas chromatograph e quiped with a 2.5% SE-30 coated on chromosorb WHP glass column and electron capture detector (Ni63). The limit of detectability obtained was 0.005 ppm for DDT and 0.002 ppm for endrin ln nonfatty materials and 0.005 ppm for both insecticides in fatty materials. DDT residues were less persistent in leaves than endrin residues, with initial deposits easily removed by weathering agents, particularly rain and wind. In the last sampling the residue levels in leaves were 4.208 ppm for DDT (p,p’-DDE, o,p’-DDT and p,p’-DDT) and 7.92 ppm for endrin. The persistence of both insecticides in cotton seeds was similar, considering the amount applied and the final residues, which were 0.091 ppm and 0.035 ppm for DDT and endrin respectively. The crude oil showed higher residue J.evels, 0.20 ppm and 0.086 ppm for DDT and endrin, which represents approximately 50% of these insecticides contained in the cotton seeds. The meal showed lower residue levels, 0.025 pprn and 0.010 ppm for DDT and endrin. The residue levels found in cotton seeds were in accordance with the official tolerances, which are 1.0 ppm for DDT residues and 0.1 ppm for endrin residues,with a safety interval of 30 days.
 
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Publishing Date
2024-03-14
 
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