Determinação de resíduos de agrotóxicos em azeite de oliva e azeitonas empregando método QuEChERS e UHPLC-MS/MS
Autor(a) principal: | |
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Data de Publicação: | 2019 |
Tipo de documento: | Tese |
Idioma: | por |
Título da fonte: | Manancial - Repositório Digital da UFSM |
dARK ID: | ark:/26339/001300000z2qr |
Texto Completo: | http://repositorio.ufsm.br/handle/1/20737 |
Resumo: | Commonly used in the Mediterranean diet, olive oils and table olives have become more frequent in the everyday meals of the Brazilian consumer. Despite the small consumption per capita, the country is already the second biggest importer of the fruit. The main provider is Argentina, followed by Spain, Portugal and Chile. In the last years, Brazil has been increasing olive growing, mainly in the Rio Grande do Sul state. However, there is not stablished law for olive trees cultivation and only one insecticide is permitted for olives. Therefore, many producers have to apply restricted pesticides, in the need to fight pests, like the olive fly, olive tree moth, rust and others. Therefore, the need to develop an analytical method to determine pesticide residues from different classes in olive oils and table olives, to guarantee that the produce brought to the consumer are not contaminated. This research developed and validated an analytical method for the determination of 80 different pesticides in olive oil and table olives employing QuEChERS and ultra-high performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS). The extracts were analysed by UHPLC-MS/MS according to the validation criteria stablished by SANTE. The proposed method showed adequate for the determination of 80 pesticides in olive oil and table olives. LOQ ranged from 0.5 to 10 μg L-1 and the LOD from 0.15 to 3 μg L-1 with adequate accuracy (70 to 120%) and precision (RSD ≤20%). The proposed method was applied in 23 samples of olive oils and 11 table olives from national and imported brands. From those, six samples of olive oils and all samples of table olives showed at least one pesticide above the LOQ. The compounds allowed by the Brazilian law were not detected in the samples. However, the fungicide difenoconazole, allowed for olive growing by Codex Alimentarius, showed concentration below the maximum residues limit. |
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Determinação de resíduos de agrotóxicos em azeite de oliva e azeitonas empregando método QuEChERS e UHPLC-MS/MSDetermination of pesticides residuoes in olive and olive oil using QuEChERS METHOD and UHPLC-MS/MSAzeitonaAzeite de olivaQuEChERSUHPLC-MS/MSAgrotóxicosOliveOlive oilPesticidesCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICACommonly used in the Mediterranean diet, olive oils and table olives have become more frequent in the everyday meals of the Brazilian consumer. Despite the small consumption per capita, the country is already the second biggest importer of the fruit. The main provider is Argentina, followed by Spain, Portugal and Chile. In the last years, Brazil has been increasing olive growing, mainly in the Rio Grande do Sul state. However, there is not stablished law for olive trees cultivation and only one insecticide is permitted for olives. Therefore, many producers have to apply restricted pesticides, in the need to fight pests, like the olive fly, olive tree moth, rust and others. Therefore, the need to develop an analytical method to determine pesticide residues from different classes in olive oils and table olives, to guarantee that the produce brought to the consumer are not contaminated. This research developed and validated an analytical method for the determination of 80 different pesticides in olive oil and table olives employing QuEChERS and ultra-high performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS). The extracts were analysed by UHPLC-MS/MS according to the validation criteria stablished by SANTE. The proposed method showed adequate for the determination of 80 pesticides in olive oil and table olives. LOQ ranged from 0.5 to 10 μg L-1 and the LOD from 0.15 to 3 μg L-1 with adequate accuracy (70 to 120%) and precision (RSD ≤20%). The proposed method was applied in 23 samples of olive oils and 11 table olives from national and imported brands. From those, six samples of olive oils and all samples of table olives showed at least one pesticide above the LOQ. The compounds allowed by the Brazilian law were not detected in the samples. However, the fungicide difenoconazole, allowed for olive growing by Codex Alimentarius, showed concentration below the maximum residues limit.Muito usados na dieta mediterrânea os azeites de oliva e azeitonas de mesa têm se tornado cada dia mais frequentes na mesa do consumidor brasileiro. Apesar do consumo per capta ainda ser pequeno, o país já se configura no cenário internacional como o segundo maior importador do azeite. O principal fornecedor de azeite de oliva é a Espanha ede azeitona é a Argentina, seguida por Espanha, Portugal e Chile. Nos últimos anos a olivicultura vem crescendo no Brasil, principalmente no estado do Rio Grande do Sul. No entanto, ainda não há uma legislação bem estabelecida para o cultivo das oliveiras e apenas um inseticida apresenta LMR para azeitonas. Assim, agrotóxicos não permitidos acabam sendo utilizados para o combate de pragas. Por isso, desenvolver um método analítico que permita determinar agrotóxicos de diferentes classes em azeites de oliva e azeitonas de mesa é fundamental para garantir que os produtos levados à mesa do consumidor não estejam contaminados. Portanto, essa pesquisa desenvolveu e validou um método analítico para determinação de 80 diferentes agrotóxicos em azeite de oliva e azeitonas de mesa empregando o método QuEChERS e a Cromatografia Líquida de ultra eficiência acoplada a espectrometria sequencial (UHPLC-MS/MS). Os extratos foram submetidos à análise cromatográfica por UHPLC-MS/MS obedecendo aos critérios de validação estabelecidos pela SANTE (2017). O método proposto mostrou-se adequado para a determinação de 80 agrotóxicos de diferentes classes em azeite de oliva e azeitonas. O LOQ variou de 0,5 a 10 μg L-1 e o LOD de 0,15 a 3 μg L-1 dentro da faixa de aceitação utilizada que foi de 70 a 120% com RSD <20%. Aplicou-se o método proposto para 23 amostras de azeites de oliva e 11 de azeitonas nacionais e importadas. Dessas, seis azeites de oliva e todas as azeitonas de mesa apresentaram pelo menos um dos agrotóxicos avaliados acima do LOQ. Os compostos permitidos pela legislação brasileira não foram detectados nas amostras. Já o fungicida difenoconazol, permitido para a cultura pelo Codex Alimentarius, apresentou concentração abaixo do limite máximo de resíduos.Universidade Federal de Santa MariaBrasilQuímicaUFSMPrograma de Pós-Graduação em QuímicaCentro de Ciências Naturais e ExatasAdaime, Martha Bohrerhttp://lattes.cnpq.br/4385786922516848Cabrera, Liziara da CostaXXXXXXXXXXXXXXXXXXXOrso, DéboraXXXXXXXXXXXXXXBallus, Cristiano AugustoXXXXXXXXXXXXPrestes, Osmar DamianXXXXXXXXXXXXXXXFerronato, Giovana2021-04-30T10:17:29Z2021-04-30T10:17:29Z2019-08-03info:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/doctoralThesisapplication/pdfhttp://repositorio.ufsm.br/handle/1/20737ark:/26339/001300000z2qrporAttribution-NonCommercial-NoDerivatives 4.0 Internationalhttp://creativecommons.org/licenses/by-nc-nd/4.0/info:eu-repo/semantics/openAccessreponame:Manancial - Repositório Digital da UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSM2021-05-01T06:03:31Zoai:repositorio.ufsm.br:1/20737Biblioteca Digital de Teses e Dissertaçõeshttps://repositorio.ufsm.br/ONGhttps://repositorio.ufsm.br/oai/requestatendimento.sib@ufsm.br||tedebc@gmail.comopendoar:2021-05-01T06:03:31Manancial - Repositório Digital da UFSM - Universidade Federal de Santa Maria (UFSM)false |
dc.title.none.fl_str_mv |
Determinação de resíduos de agrotóxicos em azeite de oliva e azeitonas empregando método QuEChERS e UHPLC-MS/MS Determination of pesticides residuoes in olive and olive oil using QuEChERS METHOD and UHPLC-MS/MS |
title |
Determinação de resíduos de agrotóxicos em azeite de oliva e azeitonas empregando método QuEChERS e UHPLC-MS/MS |
spellingShingle |
Determinação de resíduos de agrotóxicos em azeite de oliva e azeitonas empregando método QuEChERS e UHPLC-MS/MS Ferronato, Giovana Azeitona Azeite de oliva QuEChERS UHPLC-MS/MS Agrotóxicos Olive Olive oil Pesticides CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Determinação de resíduos de agrotóxicos em azeite de oliva e azeitonas empregando método QuEChERS e UHPLC-MS/MS |
title_full |
Determinação de resíduos de agrotóxicos em azeite de oliva e azeitonas empregando método QuEChERS e UHPLC-MS/MS |
title_fullStr |
Determinação de resíduos de agrotóxicos em azeite de oliva e azeitonas empregando método QuEChERS e UHPLC-MS/MS |
title_full_unstemmed |
Determinação de resíduos de agrotóxicos em azeite de oliva e azeitonas empregando método QuEChERS e UHPLC-MS/MS |
title_sort |
Determinação de resíduos de agrotóxicos em azeite de oliva e azeitonas empregando método QuEChERS e UHPLC-MS/MS |
author |
Ferronato, Giovana |
author_facet |
Ferronato, Giovana |
author_role |
author |
dc.contributor.none.fl_str_mv |
Adaime, Martha Bohrer http://lattes.cnpq.br/4385786922516848 Cabrera, Liziara da Costa XXXXXXXXXXXXXXXXXXX Orso, Débora XXXXXXXXXXXXXX Ballus, Cristiano Augusto XXXXXXXXXXXX Prestes, Osmar Damian XXXXXXXXXXXXXXX |
dc.contributor.author.fl_str_mv |
Ferronato, Giovana |
dc.subject.por.fl_str_mv |
Azeitona Azeite de oliva QuEChERS UHPLC-MS/MS Agrotóxicos Olive Olive oil Pesticides CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
topic |
Azeitona Azeite de oliva QuEChERS UHPLC-MS/MS Agrotóxicos Olive Olive oil Pesticides CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
Commonly used in the Mediterranean diet, olive oils and table olives have become more frequent in the everyday meals of the Brazilian consumer. Despite the small consumption per capita, the country is already the second biggest importer of the fruit. The main provider is Argentina, followed by Spain, Portugal and Chile. In the last years, Brazil has been increasing olive growing, mainly in the Rio Grande do Sul state. However, there is not stablished law for olive trees cultivation and only one insecticide is permitted for olives. Therefore, many producers have to apply restricted pesticides, in the need to fight pests, like the olive fly, olive tree moth, rust and others. Therefore, the need to develop an analytical method to determine pesticide residues from different classes in olive oils and table olives, to guarantee that the produce brought to the consumer are not contaminated. This research developed and validated an analytical method for the determination of 80 different pesticides in olive oil and table olives employing QuEChERS and ultra-high performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS). The extracts were analysed by UHPLC-MS/MS according to the validation criteria stablished by SANTE. The proposed method showed adequate for the determination of 80 pesticides in olive oil and table olives. LOQ ranged from 0.5 to 10 μg L-1 and the LOD from 0.15 to 3 μg L-1 with adequate accuracy (70 to 120%) and precision (RSD ≤20%). The proposed method was applied in 23 samples of olive oils and 11 table olives from national and imported brands. From those, six samples of olive oils and all samples of table olives showed at least one pesticide above the LOQ. The compounds allowed by the Brazilian law were not detected in the samples. However, the fungicide difenoconazole, allowed for olive growing by Codex Alimentarius, showed concentration below the maximum residues limit. |
publishDate |
2019 |
dc.date.none.fl_str_mv |
2019-08-03 2021-04-30T10:17:29Z 2021-04-30T10:17:29Z |
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.uri.fl_str_mv |
http://repositorio.ufsm.br/handle/1/20737 |
dc.identifier.dark.fl_str_mv |
ark:/26339/001300000z2qr |
url |
http://repositorio.ufsm.br/handle/1/20737 |
identifier_str_mv |
ark:/26339/001300000z2qr |
dc.language.iso.fl_str_mv |
por |
language |
por |
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.format.none.fl_str_mv |
application/pdf |
dc.publisher.none.fl_str_mv |
Universidade Federal de Santa Maria Brasil Química UFSM Programa de Pós-Graduação em Química Centro de Ciências Naturais e Exatas |
publisher.none.fl_str_mv |
Universidade Federal de Santa Maria Brasil Química UFSM Programa de Pós-Graduação em Química Centro de Ciências Naturais e Exatas |
dc.source.none.fl_str_mv |
reponame:Manancial - Repositório Digital da UFSM instname:Universidade Federal de Santa Maria (UFSM) instacron:UFSM |
instname_str |
Universidade Federal de Santa Maria (UFSM) |
instacron_str |
UFSM |
institution |
UFSM |
reponame_str |
Manancial - Repositório Digital da UFSM |
collection |
Manancial - Repositório Digital da UFSM |
repository.name.fl_str_mv |
Manancial - Repositório Digital da UFSM - Universidade Federal de Santa Maria (UFSM) |
repository.mail.fl_str_mv |
atendimento.sib@ufsm.br||tedebc@gmail.com |
_version_ |
1815172416461078528 |