Determinação de micotoxinas por UPLC-MS/MS em grãos armazenados sob condições de temperatura e atmosfera controlada
Ano de defesa: | 2019 |
---|---|
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
Centro de Ciências Naturais e Exatas |
Programa de Pós-Graduação: |
Programa de Pós-Graduação em Química
|
Departamento: |
Química
|
País: |
Brasil
|
Palavras-chave em Português: | |
Palavras-chave em Inglês: | |
Área do conhecimento CNPq: | |
Link de acesso: | http://repositorio.ufsm.br/handle/1/17190 |
Resumo: | This work aimed to develop and validate analytical methods for the determination of mycotoxins in beans, corn and soybean using UPLC-MS/MS and to evaluate the occurrence of mycotoxins in samples of these grains after six months of storage under controlled atmosphere. The extraction of mycotoxins was performed using the QuEChERS method, which was optimized so that the highest number of mycotoxins were extracted with recoveries between 70 and 120% and RSD ≤ 20%. Subsequently, the optimized methods were validated for beans and soybeans based on three guidance documents. Samples (5 g) were extracted with 10 mL of acetonitrile containing 1% formic acid for beans and maize, and 5% formic acid for soybean, followed by partitioning with MgSO4 and diluting the extract 1: 1 (v / v) with methanol directly into vial. Samples submitted to 15 controlled atmosphere treatments for four bean cultivars (Fepagro 26, Garapia, Cowpea white and red beans), four soybean cultivars (Brasmax Ultra IPRO, Brasmax Desafio RR, Brasmax Bonus IPRO and Tec IRGA 6070) were analyzed and 6 treatments for maize. Treatments were carried out at three temperature (20, 25 and 30 ºC) and at atmosphere with control of the partial pressures of O2 and CO2. There was no occurrence of mycotoxins in the cultivars Cowpea white and red beans, and soybean cultivars Brasmax Desafio RR and Brasmax Ultra IPRO. Aflatoxin B1 (AF B1) was detected in the other bean and soybean cultivars. For the cultivars Fepagro 26 and Garapia, no mycotoxins were detected in the grains stored at temperatures ≤ 20 ºC. For the cultivars Brasmax Bonus IPRO and Tec IRGA, AF B1 was detected in all the studied samples, indicating that the storage conditions were not effective to prevent the contamination of the samples. AF B1, fumonisins B1 and B2 (FM B1 and FM B2, respectively) were detected in all maize samples, although FM B1 was not detected in grain stored with moisture content at 14% at 30 ºC and ambient atmosphere. |
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Biblioteca Digital de Teses e Dissertações do UFSM |
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2019-06-28T11:45:53Z2019-06-28T11:45:53Z2019-02-28http://repositorio.ufsm.br/handle/1/17190This work aimed to develop and validate analytical methods for the determination of mycotoxins in beans, corn and soybean using UPLC-MS/MS and to evaluate the occurrence of mycotoxins in samples of these grains after six months of storage under controlled atmosphere. The extraction of mycotoxins was performed using the QuEChERS method, which was optimized so that the highest number of mycotoxins were extracted with recoveries between 70 and 120% and RSD ≤ 20%. Subsequently, the optimized methods were validated for beans and soybeans based on three guidance documents. Samples (5 g) were extracted with 10 mL of acetonitrile containing 1% formic acid for beans and maize, and 5% formic acid for soybean, followed by partitioning with MgSO4 and diluting the extract 1: 1 (v / v) with methanol directly into vial. Samples submitted to 15 controlled atmosphere treatments for four bean cultivars (Fepagro 26, Garapia, Cowpea white and red beans), four soybean cultivars (Brasmax Ultra IPRO, Brasmax Desafio RR, Brasmax Bonus IPRO and Tec IRGA 6070) were analyzed and 6 treatments for maize. Treatments were carried out at three temperature (20, 25 and 30 ºC) and at atmosphere with control of the partial pressures of O2 and CO2. There was no occurrence of mycotoxins in the cultivars Cowpea white and red beans, and soybean cultivars Brasmax Desafio RR and Brasmax Ultra IPRO. Aflatoxin B1 (AF B1) was detected in the other bean and soybean cultivars. For the cultivars Fepagro 26 and Garapia, no mycotoxins were detected in the grains stored at temperatures ≤ 20 ºC. For the cultivars Brasmax Bonus IPRO and Tec IRGA, AF B1 was detected in all the studied samples, indicating that the storage conditions were not effective to prevent the contamination of the samples. AF B1, fumonisins B1 and B2 (FM B1 and FM B2, respectively) were detected in all maize samples, although FM B1 was not detected in grain stored with moisture content at 14% at 30 ºC and ambient atmosphere.Este trabalho teve como objetivos desenvolver e validar métodos analíticos para a determinação de micotoxinas em grãos de feijão, milho e soja empregando UPLC-MS/MS e avaliar a ocorrência de micotoxinas em amostras desses grãos após seis meses de armazenamento em atmosfera controlada. A extração das micotoxinas foi realizada com o método QuEChERS, o qual foi otimizado de forma que o maior número de micotoxinas fosse extraído com recuperações entre 70 e 120% e RSD ≤ 20%. Posteriormente, os métodos foram validados para as matrizes feijão e soja com base em três documentos orientativos. As amostras (5 g) foram extraídas com 10 mL de acetonitrila contendo 1% de ácido fórmico para feijão e milho, e 5% de ácido fórmico para soja, seguido de partição com MgSO4 e diluição do extrato 1:1 (v/v) com metanol diretamente em vial. Foram analisadas amostras submetidas a 15 tratamentos em atmosfera controlada para quatro cultivares de feijão (Fepagro 26, Garapiá, Caupi branco e Caupi vermelho), quatro cultivares de soja (Brasmax Ultra IPRO, Brasmax Desafio RR, Brasmax Bônus IPRO e Tec IRGA 6070) e 6 tratamentos para milho. Os tratamentos foram realizados em três faixas de temperatura (20, 25 e 30 ºC) e em atmosfera com controle das pressões parciais de O2 e CO2. Não houve ocorrência de micotoxinas nos cultivares feijão Caupi branco e vermelho, e nos cultivares de soja Brasmax Desafio RR e Brasmax Ultra IPRO. Nos demais cultivares de feijão e soja detectou-se a presença de aflatoxina B1 (AF B1). Para os cultivares Fepagro 26 e Garapiá, não foram detectadas micotoxinas nos grãos armazenados em temperaturas ≤ 20 ºC. Para os cultivares Brasmax Bônus IPRO e Tec IRGA, detectou-se a presença de AF B1 em todas amostras estudadas, indicando que as condições de armazenamento não foram efetivas para impedir a contaminação das amostras. Nas amostras de milho detectou-se a presença das micotoxinas AF B1, fumonisinas B1 e B2 (FM B1 e FM B2, respectivamente) sendo que FM B1 não foi detectada no armazenamento dos grãos com teor de umidade 14%, à 30 ºC e em atmosfera ambiente.Coordenação de Aperfeiçoamento de Pessoal de Nível Superior - CAPESporUniversidade Federal de Santa MariaCentro de Ciências Naturais e ExatasPrograma de Pós-Graduação em QuímicaUFSMBrasilQuímicaAttribution-NonCommercial-NoDerivatives 4.0 Internationalhttp://creativecommons.org/licenses/by-nc-nd/4.0/info:eu-repo/semantics/openAccessMicotoxinasQuEChERSEspectrometria de massasFeijãoMilhoSojaAtmosfera controladaCromatografia líquidaMycotoxinsLiquid chromatographyMass spectrometryBeansMaizeSoybeansControlled atmosphereCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICADeterminação de micotoxinas por UPLC-MS/MS em grãos armazenados sob condições de temperatura e atmosfera controladaDetermination of mycotoxins by UPLC-MS/MS in grains stored under temperature and controlled atmosphereinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisPizzutti, Ionara Reginahttp://lattes.cnpq.br/3883506164936996Brackmann, Aurihttp://lattes.cnpq.br/1305840929832646Silva, Rosselei Caiél dahttp://lattes.cnpq.br/2187197138622302http://lattes.cnpq.br/3127277855964895Nunes, Maria da Graça Pereira100600000000600961b4a4a-1465-4d87-b4e8-6428b5a3ad38713f01f2-70d9-4c0a-872d-777c1c4e24f040e57e71-6060-40b2-bf11-2ecccf5e9c3d76bfa5a6-c0a0-46b7-aac3-616d4fe00e63reponame:Biblioteca Digital de Teses e Dissertações do UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMORIGINALDIS_PPGQUIMICA_2019_NUNES_MARIA.pdfDIS_PPGQUIMICA_2019_NUNES_MARIA.pdfDissertação de Mestradoapplication/pdf3248574http://repositorio.ufsm.br/bitstream/1/17190/1/DIS_PPGQUIMICA_2019_NUNES_MARIA.pdffa553e4adba61d571eea9becd8a46cf4MD51CC-LICENSElicense_rdflicense_rdfapplication/rdf+xml; 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dc.title.por.fl_str_mv |
Determinação de micotoxinas por UPLC-MS/MS em grãos armazenados sob condições de temperatura e atmosfera controlada |
dc.title.alternative.eng.fl_str_mv |
Determination of mycotoxins by UPLC-MS/MS in grains stored under temperature and controlled atmosphere |
title |
Determinação de micotoxinas por UPLC-MS/MS em grãos armazenados sob condições de temperatura e atmosfera controlada |
spellingShingle |
Determinação de micotoxinas por UPLC-MS/MS em grãos armazenados sob condições de temperatura e atmosfera controlada Nunes, Maria da Graça Pereira Micotoxinas QuEChERS Espectrometria de massas Feijão Milho Soja Atmosfera controlada Cromatografia líquida Mycotoxins Liquid chromatography Mass spectrometry Beans Maize Soybeans Controlled atmosphere CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Determinação de micotoxinas por UPLC-MS/MS em grãos armazenados sob condições de temperatura e atmosfera controlada |
title_full |
Determinação de micotoxinas por UPLC-MS/MS em grãos armazenados sob condições de temperatura e atmosfera controlada |
title_fullStr |
Determinação de micotoxinas por UPLC-MS/MS em grãos armazenados sob condições de temperatura e atmosfera controlada |
title_full_unstemmed |
Determinação de micotoxinas por UPLC-MS/MS em grãos armazenados sob condições de temperatura e atmosfera controlada |
title_sort |
Determinação de micotoxinas por UPLC-MS/MS em grãos armazenados sob condições de temperatura e atmosfera controlada |
author |
Nunes, Maria da Graça Pereira |
author_facet |
Nunes, Maria da Graça Pereira |
author_role |
author |
dc.contributor.advisor1.fl_str_mv |
Pizzutti, Ionara Regina |
dc.contributor.advisor1Lattes.fl_str_mv |
http://lattes.cnpq.br/3883506164936996 |
dc.contributor.referee1.fl_str_mv |
Brackmann, Auri |
dc.contributor.referee1Lattes.fl_str_mv |
http://lattes.cnpq.br/1305840929832646 |
dc.contributor.referee2.fl_str_mv |
Silva, Rosselei Caiél da |
dc.contributor.referee2Lattes.fl_str_mv |
http://lattes.cnpq.br/2187197138622302 |
dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/3127277855964895 |
dc.contributor.author.fl_str_mv |
Nunes, Maria da Graça Pereira |
contributor_str_mv |
Pizzutti, Ionara Regina Brackmann, Auri Silva, Rosselei Caiél da |
dc.subject.por.fl_str_mv |
Micotoxinas QuEChERS Espectrometria de massas Feijão Milho Soja Atmosfera controlada |
topic |
Micotoxinas QuEChERS Espectrometria de massas Feijão Milho Soja Atmosfera controlada Cromatografia líquida Mycotoxins Liquid chromatography Mass spectrometry Beans Maize Soybeans Controlled atmosphere CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.eng.fl_str_mv |
Cromatografia líquida Mycotoxins Liquid chromatography Mass spectrometry Beans Maize Soybeans Controlled atmosphere |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
This work aimed to develop and validate analytical methods for the determination of mycotoxins in beans, corn and soybean using UPLC-MS/MS and to evaluate the occurrence of mycotoxins in samples of these grains after six months of storage under controlled atmosphere. The extraction of mycotoxins was performed using the QuEChERS method, which was optimized so that the highest number of mycotoxins were extracted with recoveries between 70 and 120% and RSD ≤ 20%. Subsequently, the optimized methods were validated for beans and soybeans based on three guidance documents. Samples (5 g) were extracted with 10 mL of acetonitrile containing 1% formic acid for beans and maize, and 5% formic acid for soybean, followed by partitioning with MgSO4 and diluting the extract 1: 1 (v / v) with methanol directly into vial. Samples submitted to 15 controlled atmosphere treatments for four bean cultivars (Fepagro 26, Garapia, Cowpea white and red beans), four soybean cultivars (Brasmax Ultra IPRO, Brasmax Desafio RR, Brasmax Bonus IPRO and Tec IRGA 6070) were analyzed and 6 treatments for maize. Treatments were carried out at three temperature (20, 25 and 30 ºC) and at atmosphere with control of the partial pressures of O2 and CO2. There was no occurrence of mycotoxins in the cultivars Cowpea white and red beans, and soybean cultivars Brasmax Desafio RR and Brasmax Ultra IPRO. Aflatoxin B1 (AF B1) was detected in the other bean and soybean cultivars. For the cultivars Fepagro 26 and Garapia, no mycotoxins were detected in the grains stored at temperatures ≤ 20 ºC. For the cultivars Brasmax Bonus IPRO and Tec IRGA, AF B1 was detected in all the studied samples, indicating that the storage conditions were not effective to prevent the contamination of the samples. AF B1, fumonisins B1 and B2 (FM B1 and FM B2, respectively) were detected in all maize samples, although FM B1 was not detected in grain stored with moisture content at 14% at 30 ºC and ambient atmosphere. |
publishDate |
2019 |
dc.date.accessioned.fl_str_mv |
2019-06-28T11:45:53Z |
dc.date.available.fl_str_mv |
2019-06-28T11:45:53Z |
dc.date.issued.fl_str_mv |
2019-02-28 |
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 |
http://repositorio.ufsm.br/handle/1/17190 |
url |
http://repositorio.ufsm.br/handle/1/17190 |
dc.language.iso.fl_str_mv |
por |
language |
por |
dc.relation.cnpq.fl_str_mv |
100600000000 |
dc.relation.confidence.fl_str_mv |
600 |
dc.relation.authority.fl_str_mv |
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dc.rights.driver.fl_str_mv |
Attribution-NonCommercial-NoDerivatives 4.0 International http://creativecommons.org/licenses/by-nc-nd/4.0/ info:eu-repo/semantics/openAccess |
rights_invalid_str_mv |
Attribution-NonCommercial-NoDerivatives 4.0 International http://creativecommons.org/licenses/by-nc-nd/4.0/ |
eu_rights_str_mv |
openAccess |
dc.publisher.none.fl_str_mv |
Universidade Federal de Santa Maria Centro de Ciências Naturais e Exatas |
dc.publisher.program.fl_str_mv |
Programa de Pós-Graduação em Química |
dc.publisher.initials.fl_str_mv |
UFSM |
dc.publisher.country.fl_str_mv |
Brasil |
dc.publisher.department.fl_str_mv |
Química |
publisher.none.fl_str_mv |
Universidade Federal de Santa Maria Centro de Ciências Naturais e Exatas |
dc.source.none.fl_str_mv |
reponame:Biblioteca Digital de Teses e Dissertações do UFSM instname:Universidade Federal de Santa Maria (UFSM) instacron:UFSM |
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Universidade Federal de Santa Maria (UFSM) |
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UFSM |
institution |
UFSM |
reponame_str |
Biblioteca Digital de Teses e Dissertações do UFSM |
collection |
Biblioteca Digital de Teses e Dissertações do UFSM |
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