Determinação de resíduos de agrotóxicos em uva empregando método QuEChERS e UHPLC-MS/MS
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/1/20253 |
Resumo: | Grapes, classified as fruits play important role in human diet and nutrition. They are sources of vitamins, polyphenols, essential amino acids, and a wide range of health benefits. Grapes are extremely rich in pigments, such as anthocyanins and anthocyanidins, responsible for conferring color, a characteristic used as a parameter of maturity and quality. The instinctive preferences and the search for a healthier life lead to the practice of eating naturally colored foods. Although, like many other crops, grapes are susceptible to pest attack, such as fungi and other diseases, and the application of plant health products is a common practice in agriculture to circumvent this problem and increase productivity. Therefore, it is necessary to monitor the products intended for consumption, which may pose risks to human health, resulting from chronic dietary exposure. However, the sample matrix contains abundant quantities of anthocyanins, requiring a preliminary sample preparation step capable of providing clean extracts and suitable recoveries of the compounds of interest. The main objective of this work was to optimize the cleaning of sample preparation through the use of different dilution volumes through the dilution and shoot technique for the removal of pigments derived from the different anthocyanins present in extracts from grape samples. The experiments were evaluated by gravimetric tests, and qualitative analysis by the GC-MS / MS chromatographic system and by high performance liquid chromatography with ultraviolet / visible detection (HPLC-UV / Vis). After optimization, a multi-residue method was developed and validated for the determination of 36 agrochemicals in grapes using modified QuEChERS citrate method and evaluated by ultra high-performance liquid chromatography coupled to mass-mass spectrometry (UHPLC-MS / MS). allowed the accomplishment of the analyzes with high selectivity and sensitivity. The extracts were cleaned using the dilution and shoot technique, applying different dilutions of the extract in 2, 5, 10, 20 and 40x, the latter being the method that presented better efficiency in the removal of coextractives and adequate recoveries of the compounds. The validation results were satisfactory with recoveries between 70 and 120% and RSDs ≤20%. The curves were prepared in the matrix extract, due to the presence of a strong matrix effect for most of the compounds. The limits of detection and quantification were 7 and 25 μg kg-1, respectively. The proposed method proved to be adequate for the determination of multi-residues of pesticides in grapes, as well as, the dilution stage of the extracts demonstrated satisfactory efficiency, detectability and selectivity to the method and also in the application of 20 samples since all the parameters suggested for the validation chromatographic methods are within the limits. |
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2021-01-15T11:06:14Z2021-01-15T11:06:14Z2019-02-28http://repositorio.ufsm.br/handle/1/20253Grapes, classified as fruits play important role in human diet and nutrition. They are sources of vitamins, polyphenols, essential amino acids, and a wide range of health benefits. Grapes are extremely rich in pigments, such as anthocyanins and anthocyanidins, responsible for conferring color, a characteristic used as a parameter of maturity and quality. The instinctive preferences and the search for a healthier life lead to the practice of eating naturally colored foods. Although, like many other crops, grapes are susceptible to pest attack, such as fungi and other diseases, and the application of plant health products is a common practice in agriculture to circumvent this problem and increase productivity. Therefore, it is necessary to monitor the products intended for consumption, which may pose risks to human health, resulting from chronic dietary exposure. However, the sample matrix contains abundant quantities of anthocyanins, requiring a preliminary sample preparation step capable of providing clean extracts and suitable recoveries of the compounds of interest. The main objective of this work was to optimize the cleaning of sample preparation through the use of different dilution volumes through the dilution and shoot technique for the removal of pigments derived from the different anthocyanins present in extracts from grape samples. The experiments were evaluated by gravimetric tests, and qualitative analysis by the GC-MS / MS chromatographic system and by high performance liquid chromatography with ultraviolet / visible detection (HPLC-UV / Vis). After optimization, a multi-residue method was developed and validated for the determination of 36 agrochemicals in grapes using modified QuEChERS citrate method and evaluated by ultra high-performance liquid chromatography coupled to mass-mass spectrometry (UHPLC-MS / MS). allowed the accomplishment of the analyzes with high selectivity and sensitivity. The extracts were cleaned using the dilution and shoot technique, applying different dilutions of the extract in 2, 5, 10, 20 and 40x, the latter being the method that presented better efficiency in the removal of coextractives and adequate recoveries of the compounds. The validation results were satisfactory with recoveries between 70 and 120% and RSDs ≤20%. The curves were prepared in the matrix extract, due to the presence of a strong matrix effect for most of the compounds. The limits of detection and quantification were 7 and 25 μg kg-1, respectively. The proposed method proved to be adequate for the determination of multi-residues of pesticides in grapes, as well as, the dilution stage of the extracts demonstrated satisfactory efficiency, detectability and selectivity to the method and also in the application of 20 samples since all the parameters suggested for the validation chromatographic methods are within the limits.As uvas, classificadas como frutas desempenham importante papel na dieta e nutrição humana. São fontes de vitaminas, polifenóis, aminoácidos essenciais, além de uma vasta gama de benefícios a saúde. As uvas são extremamente ricas em pigmentos, como as antocianinas e as antocianidinas, responsáveis por conferir cor, característica utilizada como parâmetro de maturidade e qualidade. As preferências instintivas e a busca por uma vida mais saudável levam a prática do consumo de alimentos coloridos naturalmente. Embora, assim como muitas outras culturas, as uvas são susceptíveis a ataque de pragas, como fungos e outras doenças, sendo a aplicação de produtos fitossanitários uma prática comum na agricultura para contornar este problema e aumentar a produtividade. Assim, é necessário monitorar os produtos destinados ao consumo, os quais possam oferecer riscos para a saúde humana, resultantes da exposição dietética crônica. No entanto, a matriz da amostra contém abundantes quantidades de antocianinas, exigindo uma etapa preliminar de preparo de amostras capaz de fornecer extratos limpos e recuperações adequadas dos compostos de interesse. Este trabalho teve como objetivo principal otimizar a etapa de limpeza do preparo de amostras, através do uso de diferentes volumes de diluição através da técnica de dilute and shoot para a remoção de pigmentos, derivados das diferentes antocianinas presentes em extratos de amostras de uva. Os experimentos foram avaliados por testes gravimétricos, e análise qualitativa pelo sistema cromatográfico GC-MS/MS e por cromatografia líquida de alta eficiência com detecção no ultravioleta/visível (HPLC-UV/Vis). Após a otimização, foi desenvolvido e validado um método multirresíduos para a determinação de 36 agrotóxicos em uvas empregando método QuEChERS citrato modificado e avaliados por cromatografia liquida de ultraalta eficiência acoplada à espectrometria de massas em série (UHPLC-MS/MS) o que permitiu a realização das análises com alta seletividade e sensibilidade. A limpeza dos extratos foi realizada pela técnica de dilute and shoot, aplicando diferentes diluições do extrato em 2, 5, 10, 20 e 40x sendo este último o método que apresentou melhor eficiência na remoção de coextrativos e recuperações adequadas dos compostos. Os resultados da validação foram satisfatórios com recuperações entre 70 e 120% e RSDs ≤20%. As curvas foram preparadas no extrato da matriz, devido à presença de efeito matriz acentuado para a maioria dos compostos. Os limites de detecção e quantificação foram de 7 e 25 μg kg-1, respectivamente. O método proposto mostrouse adequado à determinação multirresíduos de agrotóxicos em uvas, bem como, a etapa de diluição dos extratos demonstrou, eficiência, detectabilidade e seletividade satisfatórias ao método e também na aplicação de 20 amostras visto que todos os parâmetros sugeridos para a validação de métodos cromatográficos encontram-se dentro dos limites.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/openAccessPreparo de amostraUvaResíduos de agrotóxicosDilute and shootSample preparationGrapePesticide residuesCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICADeterminação de resíduos de agrotóxicos em uva empregando método QuEChERS e UHPLC-MS/MSDetermination of pesticides residues in grape empregating QuEChERS and METHOD UHPLC-MS / MSinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisPrestes, Osmar Damianhttp://lattes.cnpq.br/9632234955509028Peixoto, Sandra Cadorehttp://lattes.cnpq.br/0051729840313401Müller, Aline Lima Hermeshttp://lattes.cnpq.br/6859286861380431http://lattes.cnpq.br/7077500969280525Cassól, Ricardo Ramos Corrêa100600000000600f79cc0c9-c923-4244-9c1f-c80d74674410a67112b2-3ab0-4aff-8cd7-02464833d02437d33bad-e676-436f-86c5-984dfc4cc2e668a7f309-90a3-4221-a8b2-fe09d8f1e28ereponame:Biblioteca Digital de Teses e Dissertações do UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMORIGINALDIS_PPGQUIMICA_2019_CASSOL_RICARDO.pdfDIS_PPGQUIMICA_2019_CASSOL_RICARDO.pdfDissertação de Mestradoapplication/pdf2715278http://repositorio.ufsm.br/bitstream/1/20253/1/DIS_PPGQUIMICA_2019_CASSOL_RICARDO.pdf48684561e43b62dd1a731d7fbd153757MD51CC-LICENSElicense_rdflicense_rdfapplication/rdf+xml; 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dc.title.por.fl_str_mv |
Determinação de resíduos de agrotóxicos em uva empregando método QuEChERS e UHPLC-MS/MS |
dc.title.alternative.eng.fl_str_mv |
Determination of pesticides residues in grape empregating QuEChERS and METHOD UHPLC-MS / MS |
title |
Determinação de resíduos de agrotóxicos em uva empregando método QuEChERS e UHPLC-MS/MS |
spellingShingle |
Determinação de resíduos de agrotóxicos em uva empregando método QuEChERS e UHPLC-MS/MS Cassól, Ricardo Ramos Corrêa Preparo de amostra Uva Resíduos de agrotóxicos Dilute and shoot Sample preparation Grape Pesticide residues CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Determinação de resíduos de agrotóxicos em uva empregando método QuEChERS e UHPLC-MS/MS |
title_full |
Determinação de resíduos de agrotóxicos em uva empregando método QuEChERS e UHPLC-MS/MS |
title_fullStr |
Determinação de resíduos de agrotóxicos em uva empregando método QuEChERS e UHPLC-MS/MS |
title_full_unstemmed |
Determinação de resíduos de agrotóxicos em uva empregando método QuEChERS e UHPLC-MS/MS |
title_sort |
Determinação de resíduos de agrotóxicos em uva empregando método QuEChERS e UHPLC-MS/MS |
author |
Cassól, Ricardo Ramos Corrêa |
author_facet |
Cassól, Ricardo Ramos Corrêa |
author_role |
author |
dc.contributor.advisor1.fl_str_mv |
Prestes, Osmar Damian |
dc.contributor.advisor1Lattes.fl_str_mv |
http://lattes.cnpq.br/9632234955509028 |
dc.contributor.referee1.fl_str_mv |
Peixoto, Sandra Cadore |
dc.contributor.referee1Lattes.fl_str_mv |
http://lattes.cnpq.br/0051729840313401 |
dc.contributor.referee2.fl_str_mv |
Müller, Aline Lima Hermes |
dc.contributor.referee2Lattes.fl_str_mv |
http://lattes.cnpq.br/6859286861380431 |
dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/7077500969280525 |
dc.contributor.author.fl_str_mv |
Cassól, Ricardo Ramos Corrêa |
contributor_str_mv |
Prestes, Osmar Damian Peixoto, Sandra Cadore Müller, Aline Lima Hermes |
dc.subject.por.fl_str_mv |
Preparo de amostra Uva Resíduos de agrotóxicos |
topic |
Preparo de amostra Uva Resíduos de agrotóxicos Dilute and shoot Sample preparation Grape Pesticide residues CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.eng.fl_str_mv |
Dilute and shoot Sample preparation Grape Pesticide residues |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
Grapes, classified as fruits play important role in human diet and nutrition. They are sources of vitamins, polyphenols, essential amino acids, and a wide range of health benefits. Grapes are extremely rich in pigments, such as anthocyanins and anthocyanidins, responsible for conferring color, a characteristic used as a parameter of maturity and quality. The instinctive preferences and the search for a healthier life lead to the practice of eating naturally colored foods. Although, like many other crops, grapes are susceptible to pest attack, such as fungi and other diseases, and the application of plant health products is a common practice in agriculture to circumvent this problem and increase productivity. Therefore, it is necessary to monitor the products intended for consumption, which may pose risks to human health, resulting from chronic dietary exposure. However, the sample matrix contains abundant quantities of anthocyanins, requiring a preliminary sample preparation step capable of providing clean extracts and suitable recoveries of the compounds of interest. The main objective of this work was to optimize the cleaning of sample preparation through the use of different dilution volumes through the dilution and shoot technique for the removal of pigments derived from the different anthocyanins present in extracts from grape samples. The experiments were evaluated by gravimetric tests, and qualitative analysis by the GC-MS / MS chromatographic system and by high performance liquid chromatography with ultraviolet / visible detection (HPLC-UV / Vis). After optimization, a multi-residue method was developed and validated for the determination of 36 agrochemicals in grapes using modified QuEChERS citrate method and evaluated by ultra high-performance liquid chromatography coupled to mass-mass spectrometry (UHPLC-MS / MS). allowed the accomplishment of the analyzes with high selectivity and sensitivity. The extracts were cleaned using the dilution and shoot technique, applying different dilutions of the extract in 2, 5, 10, 20 and 40x, the latter being the method that presented better efficiency in the removal of coextractives and adequate recoveries of the compounds. The validation results were satisfactory with recoveries between 70 and 120% and RSDs ≤20%. The curves were prepared in the matrix extract, due to the presence of a strong matrix effect for most of the compounds. The limits of detection and quantification were 7 and 25 μg kg-1, respectively. The proposed method proved to be adequate for the determination of multi-residues of pesticides in grapes, as well as, the dilution stage of the extracts demonstrated satisfactory efficiency, detectability and selectivity to the method and also in the application of 20 samples since all the parameters suggested for the validation chromatographic methods are within the limits. |
publishDate |
2019 |
dc.date.issued.fl_str_mv |
2019-02-28 |
dc.date.accessioned.fl_str_mv |
2021-01-15T11:06:14Z |
dc.date.available.fl_str_mv |
2021-01-15T11:06:14Z |
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/1/20253 |
url |
http://repositorio.ufsm.br/handle/1/20253 |
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 |
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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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Biblioteca Digital de Teses e Dissertações do UFSM - Universidade Federal de Santa Maria (UFSM) |
repository.mail.fl_str_mv |
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