Estudo de método para determinação de resíduos de agrotóxicos em uva por GC-MS
Ano de defesa: | 2013 |
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Autor(a) principal: | |
Orientador(a): | |
Banca de defesa: | , |
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/1/10551 |
Resumo: | The regulatory agencies are becoming increasingly stringent as regards the quality of the food. Thus, the development of analytical methods that help monitoring of pesticide residues, and it is essential in routine laboratories. This study aimed at the development and validation of an analytical method for sample preparation and determination of multiclass pesticide residues in grape variety Isabel. The sample preparation was based on the QuEChERS procedure with determination by gas chromatography coupled to mass spectrometry. Several sorbent materials were tested in the cleaning step of the sample preparation, such as PSA, C18, Florisil, alumina and active carbon, with the sorbent with the highest efficiency in cleaning the extract was the Florisil. The method was defined as follows: 10 g of the sample, peel, pulp and seeds, processed in a blender was added 10 mL of acetonitrile with 1% acetic acid, 4 g of magnesium sulfate and 1 g of sodium acetate. This mixture was stirred manually for 1 minute, centrifuged at 3,000 rpm for 20 minutes. 2 mL of the supernatant was collected and mixed with 300 mg of magnesium sulfate and 400 mg of florisil, which were agitated and centrifuged again. 1 mL of the supernatant was pipetted and brought to a concentrator and the volume reduced to 200l. The efficiency of the method was proven through validation, with detection limits below the maximum residue limits allowed by regulators and recoveries between 70 and 120% with RSD lower than 20% for most pesticides studied, except for trifloxystrobin, tebuconazole and tetradifon. Using the technique matrix matched is extremely important, since it was observed that there was a large positive influence on the performance of the array analysis by increasing the signal chromatographic all analytes studied. |
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2017-05-162017-05-162013-07-29VOLPATTO, Fernanda. Study method for determination of pesticide residues in grape by GC-MS. 2013. 130 f. Dissertação (Mestrado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2013.http://repositorio.ufsm.br/handle/1/10551The regulatory agencies are becoming increasingly stringent as regards the quality of the food. Thus, the development of analytical methods that help monitoring of pesticide residues, and it is essential in routine laboratories. This study aimed at the development and validation of an analytical method for sample preparation and determination of multiclass pesticide residues in grape variety Isabel. The sample preparation was based on the QuEChERS procedure with determination by gas chromatography coupled to mass spectrometry. Several sorbent materials were tested in the cleaning step of the sample preparation, such as PSA, C18, Florisil, alumina and active carbon, with the sorbent with the highest efficiency in cleaning the extract was the Florisil. The method was defined as follows: 10 g of the sample, peel, pulp and seeds, processed in a blender was added 10 mL of acetonitrile with 1% acetic acid, 4 g of magnesium sulfate and 1 g of sodium acetate. This mixture was stirred manually for 1 minute, centrifuged at 3,000 rpm for 20 minutes. 2 mL of the supernatant was collected and mixed with 300 mg of magnesium sulfate and 400 mg of florisil, which were agitated and centrifuged again. 1 mL of the supernatant was pipetted and brought to a concentrator and the volume reduced to 200l. The efficiency of the method was proven through validation, with detection limits below the maximum residue limits allowed by regulators and recoveries between 70 and 120% with RSD lower than 20% for most pesticides studied, except for trifloxystrobin, tebuconazole and tetradifon. Using the technique matrix matched is extremely important, since it was observed that there was a large positive influence on the performance of the array analysis by increasing the signal chromatographic all analytes studied.Os órgãos regulamentadores estão se tornando cada vez mais rigorosos no que se refere à qualidade dos alimentos. Assim, o desenvolvimento de métodos analíticos, que auxiliem monitoramento de resíduos de agrotóxicos, e torna-se fundamental em laboratórios de rotina. Este estudo objetivou o desenvolvimento e validação de um método analítico para o preparo da amostra e determinação multiclasse de resíduos de agrotóxicos em uva da variedade Isabel. O preparo de amostra baseou-se no procedimento QuEChERS com determinação por Cromatografia Gasosa acoplada à Espectrometria de Massas. Diversos materiais sorventes foram testados na etapa de limpeza do preparo da amostra, como PSA, C18, Florisil, Carvão ativo e alumina, sendo que o sorvente que apresentou maior eficiência na limpeza do extrato foi o Florisil. O método ficou assim definido: a 10 g da amostra, casca, polpa e sementes, processada em liquidificador foram adicionados 10 mL de acetonitrila com 1% de ácido acético, 4 g de sulfato de magnésio e 1 g de acetato de sódio. Essa mistura foi agitada manualmente por 1 minuto, centrifugada a 3.000 rpm por 20 minutos. 2 mL do sobrenadante foram coletados e misturados com 300 mg de sulfato de magnésio e 400 mg de Florisil, que foram novamente agitados e centrifugados. 1 mL do sobrenadante foi pipetado e levado a um concentrador e o volume reduzido a 200 μL. A eficiência do método foi comprovada através da validação, apresentando limites de detecção abaixo dos Limites Máximos de Resíduos permitidos pelos órgãos reguladores e recuperações entre 70 e 120% com RSD menor que 20%, para a maioria dos agrotóxicos estudados, com exceção para trifloxistrobina, tebuconazol e tetradifona. A utilização da técnica matrix matched é de extrema importância, uma vez que foi observado que houve grande influência positiva da matriz na realização da análise, aumentando o sinal cromatográfico de todos os analitos estudados.application/pdfporUniversidade Federal de Santa MariaPrograma de Pós-Graduação em QuímicaUFSMBRQuímicaQuEChERSUvaAgrotóxicosGC-MSQuEChERSGrapePesticidesGC-MSCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICAEstudo de método para determinação de resíduos de agrotóxicos em uva por GC-MSStudy method for determination of pesticide residues in grape by GC-MSinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisAdaime, Martha Bohrerhttp://lattes.cnpq.br/4385786922516848Pizzolato, Tânia Marahttp://lattes.cnpq.br/6392594590302380Martins, Manoel Leonardohttp://lattes.cnpq.br/4404290090180984http://lattes.cnpq.br/5306436314128202Volpatto, Fernanda1006000000004005003003003007a851b28-0ef7-4e7d-9bed-bfbacf6d9791e24fe78b-dca9-40e3-b325-e63e5b9bfe7602daebba-0379-470c-a256-d94daca9b11972f05bf0-a74b-4221-b1e1-573a89d1841einfo:eu-repo/semantics/openAccessreponame:Manancial - Repositório Digital da UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMORIGINALVOLPATTO, FERNANDA.pdfapplication/pdf1807712http://repositorio.ufsm.br/bitstream/1/10551/1/VOLPATTO%2c%20FERNANDA.pdf412530aafaa7085f063d36bb835cc3e8MD51TEXTVOLPATTO, FERNANDA.pdf.txtVOLPATTO, FERNANDA.pdf.txtExtracted texttext/plain221986http://repositorio.ufsm.br/bitstream/1/10551/2/VOLPATTO%2c%20FERNANDA.pdf.txtf12ff9f251af6c7f73fcbc28418a1196MD52THUMBNAILVOLPATTO, FERNANDA.pdf.jpgVOLPATTO, FERNANDA.pdf.jpgIM Thumbnailimage/jpeg4502http://repositorio.ufsm.br/bitstream/1/10551/3/VOLPATTO%2c%20FERNANDA.pdf.jpg62ea08c3392481cf8b8b111aab672812MD531/105512022-01-26 10:56:15.359oai:repositorio.ufsm.br:1/10551Repositório Institucionalhttp://repositorio.ufsm.br/PUBhttp://repositorio.ufsm.br/oai/requestopendoar:39132022-01-26T13:56:15Manancial - Repositório Digital da UFSM - Universidade Federal de Santa Maria (UFSM)false |
dc.title.por.fl_str_mv |
Estudo de método para determinação de resíduos de agrotóxicos em uva por GC-MS |
dc.title.alternative.eng.fl_str_mv |
Study method for determination of pesticide residues in grape by GC-MS |
title |
Estudo de método para determinação de resíduos de agrotóxicos em uva por GC-MS |
spellingShingle |
Estudo de método para determinação de resíduos de agrotóxicos em uva por GC-MS Volpatto, Fernanda QuEChERS Uva Agrotóxicos GC-MS QuEChERS Grape Pesticides GC-MS CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Estudo de método para determinação de resíduos de agrotóxicos em uva por GC-MS |
title_full |
Estudo de método para determinação de resíduos de agrotóxicos em uva por GC-MS |
title_fullStr |
Estudo de método para determinação de resíduos de agrotóxicos em uva por GC-MS |
title_full_unstemmed |
Estudo de método para determinação de resíduos de agrotóxicos em uva por GC-MS |
title_sort |
Estudo de método para determinação de resíduos de agrotóxicos em uva por GC-MS |
author |
Volpatto, Fernanda |
author_facet |
Volpatto, Fernanda |
author_role |
author |
dc.contributor.advisor1.fl_str_mv |
Adaime, Martha Bohrer |
dc.contributor.advisor1Lattes.fl_str_mv |
http://lattes.cnpq.br/4385786922516848 |
dc.contributor.referee1.fl_str_mv |
Pizzolato, Tânia Mara |
dc.contributor.referee1Lattes.fl_str_mv |
http://lattes.cnpq.br/6392594590302380 |
dc.contributor.referee2.fl_str_mv |
Martins, Manoel Leonardo |
dc.contributor.referee2Lattes.fl_str_mv |
http://lattes.cnpq.br/4404290090180984 |
dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/5306436314128202 |
dc.contributor.author.fl_str_mv |
Volpatto, Fernanda |
contributor_str_mv |
Adaime, Martha Bohrer Pizzolato, Tânia Mara Martins, Manoel Leonardo |
dc.subject.por.fl_str_mv |
QuEChERS Uva Agrotóxicos GC-MS |
topic |
QuEChERS Uva Agrotóxicos GC-MS QuEChERS Grape Pesticides GC-MS CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.eng.fl_str_mv |
QuEChERS Grape Pesticides GC-MS |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
The regulatory agencies are becoming increasingly stringent as regards the quality of the food. Thus, the development of analytical methods that help monitoring of pesticide residues, and it is essential in routine laboratories. This study aimed at the development and validation of an analytical method for sample preparation and determination of multiclass pesticide residues in grape variety Isabel. The sample preparation was based on the QuEChERS procedure with determination by gas chromatography coupled to mass spectrometry. Several sorbent materials were tested in the cleaning step of the sample preparation, such as PSA, C18, Florisil, alumina and active carbon, with the sorbent with the highest efficiency in cleaning the extract was the Florisil. The method was defined as follows: 10 g of the sample, peel, pulp and seeds, processed in a blender was added 10 mL of acetonitrile with 1% acetic acid, 4 g of magnesium sulfate and 1 g of sodium acetate. This mixture was stirred manually for 1 minute, centrifuged at 3,000 rpm for 20 minutes. 2 mL of the supernatant was collected and mixed with 300 mg of magnesium sulfate and 400 mg of florisil, which were agitated and centrifuged again. 1 mL of the supernatant was pipetted and brought to a concentrator and the volume reduced to 200l. The efficiency of the method was proven through validation, with detection limits below the maximum residue limits allowed by regulators and recoveries between 70 and 120% with RSD lower than 20% for most pesticides studied, except for trifloxystrobin, tebuconazole and tetradifon. Using the technique matrix matched is extremely important, since it was observed that there was a large positive influence on the performance of the array analysis by increasing the signal chromatographic all analytes studied. |
publishDate |
2013 |
dc.date.issued.fl_str_mv |
2013-07-29 |
dc.date.accessioned.fl_str_mv |
2017-05-16 |
dc.date.available.fl_str_mv |
2017-05-16 |
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 |
VOLPATTO, Fernanda. Study method for determination of pesticide residues in grape by GC-MS. 2013. 130 f. Dissertação (Mestrado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2013. |
dc.identifier.uri.fl_str_mv |
http://repositorio.ufsm.br/handle/1/10551 |
identifier_str_mv |
VOLPATTO, Fernanda. Study method for determination of pesticide residues in grape by GC-MS. 2013. 130 f. Dissertação (Mestrado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2013. |
url |
http://repositorio.ufsm.br/handle/1/10551 |
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100600000000 |
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Universidade Federal de Santa Maria |
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Química |
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