Determinação de resíduos de ditiocarbamatos, empregando cromatografia gasosa acoplada a espectrometria de massas, em erva-mate (Ilex paraguariensis) produzida na América do Sul
Ano de defesa: | 2022 |
---|---|
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/1/24607 |
Resumo: | Dithiocarbamates (DTC) fungicides have characteristics related to high instability when in the presence of moisture and oxygen, thus requiring special preparation of the sample to be worked on, as well as the development and validation of an individual method for analysis of the generated compounds. In this work, an individual method for the determination of DTC in yerba mate was miniaturized and validated, based on the acid hydrolysis of the sample in the presence of tin chloride II, purification of the extract and subsequent analysis of the carbon disulfide (CS2) generated using gas chromatography–mass spectrometry (GC-MS). The optimization conditions were evaluated through miniaturization in the sample extraction process, based on the amount of sample, volume of extracting solvent and acid solution and the stirring time during the hot bath. These conditions were compared to those already described in the literature. As it is a complex matrix, an extract purification step was carried out through the dispersive solid phase extraction (d-SPE) process using primary and secondary amine (PSA) as sorbents, graphitized carbon (GCB) in addition to magnesium sulfate (MgSO4) as a drier. For the method validation study, the following parameters were evaluated: linearity, matrix effect, limit of detection (LOD) and limit of quantification (LOQ), precision and accuracy. Within the results obtained in the validation study, the LOD was established at 0.05 mg L-1 CS2, and the LOQ at 0.1 mg kg-1 CS2. The coefficient of determination (r2) obtained through the analytical curves was r2 > 0.99. The results obtained through the precision study were acceptable values with RSDr ≤11.2% and RSDpi ≤19.4% and, as well as the recoveries, in the range of 71.3 to 118.2%. The matrix effect calculated was -5.1%, which is within acceptable values for determining trace levels of contaminants. The validation parameters are in accordance with those described in DG-SANTE (2019) and, therefore, suitable for the determination of DTC in yerba mate. The validated method proved to be faster, simpler, and cheaper when compared to the traditional method described in the literature and quite effective for determining DTC in yerba mate. The miniaturized method was applied to 58 samples produced and sold in southern Brazil, 3 produced in Brazil and exported to Uruguay, and 4 produced in Argentina and sold in Brazil. Of the 65 herb samples that were used for the monitoring study, 33.8% had detectable levels of CS2, and 14% had concentration levels higher than the LOQ. |
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2022-05-31T17:54:07Z2022-05-31T17:54:07Z2022-02-28http://repositorio.ufsm.br/handle/1/24607Dithiocarbamates (DTC) fungicides have characteristics related to high instability when in the presence of moisture and oxygen, thus requiring special preparation of the sample to be worked on, as well as the development and validation of an individual method for analysis of the generated compounds. In this work, an individual method for the determination of DTC in yerba mate was miniaturized and validated, based on the acid hydrolysis of the sample in the presence of tin chloride II, purification of the extract and subsequent analysis of the carbon disulfide (CS2) generated using gas chromatography–mass spectrometry (GC-MS). The optimization conditions were evaluated through miniaturization in the sample extraction process, based on the amount of sample, volume of extracting solvent and acid solution and the stirring time during the hot bath. These conditions were compared to those already described in the literature. As it is a complex matrix, an extract purification step was carried out through the dispersive solid phase extraction (d-SPE) process using primary and secondary amine (PSA) as sorbents, graphitized carbon (GCB) in addition to magnesium sulfate (MgSO4) as a drier. For the method validation study, the following parameters were evaluated: linearity, matrix effect, limit of detection (LOD) and limit of quantification (LOQ), precision and accuracy. Within the results obtained in the validation study, the LOD was established at 0.05 mg L-1 CS2, and the LOQ at 0.1 mg kg-1 CS2. The coefficient of determination (r2) obtained through the analytical curves was r2 > 0.99. The results obtained through the precision study were acceptable values with RSDr ≤11.2% and RSDpi ≤19.4% and, as well as the recoveries, in the range of 71.3 to 118.2%. The matrix effect calculated was -5.1%, which is within acceptable values for determining trace levels of contaminants. The validation parameters are in accordance with those described in DG-SANTE (2019) and, therefore, suitable for the determination of DTC in yerba mate. The validated method proved to be faster, simpler, and cheaper when compared to the traditional method described in the literature and quite effective for determining DTC in yerba mate. The miniaturized method was applied to 58 samples produced and sold in southern Brazil, 3 produced in Brazil and exported to Uruguay, and 4 produced in Argentina and sold in Brazil. Of the 65 herb samples that were used for the monitoring study, 33.8% had detectable levels of CS2, and 14% had concentration levels higher than the LOQ.Os fungicidas da classe dos ditiocarbamatos (DTC) apresentam características particulares relacionadas à alta instabilidade quando em presença de umidade e oxigênio, necessitando assim, de preparo especial da amostra a ser trabalhada, bem como desenvolvimento e validação de método individual para análise dos compostos gerados. Neste trabalho, um método individual para determinação de DTC em ervamate foi miniaturizado e validado, com base na hidrólise ácida da amostra em presença de cloreto de estanho II (SnCl2), purificação do extrato e posterior análise do dissulfeto de carbono (CS2) gerado utilizando Cromatografia Gasosa acoplada a Espectrometria de Massas (GC-MS, do inglês Gas Chromatography–mass Spectrometry). As condições de otimização foram avaliadas através da miniaturização no processo de extração das amostras, com base na quantidade de amostra, volume de solvente extrator e solução ácida e o tempo de agitação durante o banho quente. Essas condições foram comparadas às já descritas na literatura. Por se tratar de uma matriz complexa, foi realizada uma etapa de purificação do extrato através do processo de extração em fase sólida dispersiva (d-SPE, do inglês Dispersive Solid Phase Extraction) utilizando como sorventes amina primária e secundária (PSA, do inglês, Primary Secundary Amine) e carvão grafitizado (GCB, do inglês Grahitized Carbon Black) além de sulfato de magnésio (MgSO4) como secante. Para o estudo de validação do método, foram avaliados os seguintes parâmetros: linearidade, efeito matriz, limite de detecção (LOD, do inglês Limit of Detection) e limite de quantificação (LOQ, do inglês Limit of Quantification), precisão e exatidão. Dentro dos resultados obtidos no estudo de validação, o LOD foi estabelecido em 0,05 mg L-1 CS2, e o LOQ 0,1 mg kg-1 CS2. O coeficiente de determinação (r2) obtido através das curvas analíticas foi r2>0,99. Os resultados obtidos através do estudo de precisão foram valores aceitáveis com RSDr ≤11,2% e RSDpi≤19,4% e, assim como as recuperações, na faixa de 71,3 a 118,2%. O efeito matriz calculado foi de -5,1%, estando dentro dos valores aceitáveis para determinação de contaminantes em níveis traço. Os parâmetros de validação estão em acordo com descrito no DG-SANTE (2019) e, portanto, apropriados à determinação de DTC em erva-mate. O método validado mostrou ser mais rápido, simples e barato quando comparado ao método tradicional descrito na literatura e bastante eficaz para determinação de DTC em erva-mate. O método miniaturizado foi aplicado a 58 amostras produzidas e comercializadas no sul do Brasil, 3 produzidas no Brasil e exportadas ao Uruguai, e 4 produzidas na Argentina e comercializadas no Brasil. Das 65 amostras de erva que foram utilizadas para o estudo de monitoramento, 33,8% com níveis detectáveis de CS2, sendo que, 14% apresentaram níveis de concentração maior que o LOQ.porUniversidade 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/openAccessCromatografia gasosaDitiocarbamatosErva-mateFungicidasGas chromatographyDithiocarbamatesYerba mateFungicidesCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICADeterminação de resíduos de ditiocarbamatos, empregando cromatografia gasosa acoplada a espectrometria de massas, em erva-mate (Ilex paraguariensis) produzida na América do SulDetermination of dithiocarbamates residues, using gas chromatography coupled to mass spectrometry, in yerba mate (Ilex paraguariensis) produced in South Americainfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisPizzutti, Ionara Reginahttp://lattes.cnpq.br/3883506164936996Silva, Rosselei Caiel daHoffmann, Jessicahttp://lattes.cnpq.br/2472238156682970Balbinot, Priscila Dotto Rosa100600000000600600600600600961b4a4a-1465-4d87-b4e8-6428b5a3ad38425c84f8-1fbf-4495-94ee-b0e1ba803a06da7f2087-b65c-4e4e-9655-413f0a415b571fa752b8-0fa2-4647-a28d-cfffd58501dereponame:Manancial - Repositório Digital da UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMORIGINALDIS_PPGQUÍMICA_2022_BALBINOT_PRISCILA.PDFDIS_PPGQUÍMICA_2022_BALBINOT_PRISCILA.PDFDissertação de mestradoapplication/pdf2379257http://repositorio.ufsm.br/bitstream/1/24607/1/DIS_PPGQU%c3%8dMICA_2022_BALBINOT_PRISCILA.PDFa018af330f526aea3dce8c21c6a00ea7MD51CC-LICENSElicense_rdflicense_rdfapplication/rdf+xml; charset=utf-8805http://repositorio.ufsm.br/bitstream/1/24607/2/license_rdf4460e5956bc1d1639be9ae6146a50347MD52LICENSElicense.txtlicense.txttext/plain; charset=utf-81956http://repositorio.ufsm.br/bitstream/1/24607/3/license.txt2f0571ecee68693bd5cd3f17c1e075dfMD531/246072022-05-31 14:56:40.002oai:repositorio.ufsm.br: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ório Institucionalhttp://repositorio.ufsm.br/PUBhttp://repositorio.ufsm.br/oai/requestopendoar:39132022-05-31T17:56:40Manancial - Repositório Digital da UFSM - Universidade Federal de Santa Maria (UFSM)false |
dc.title.por.fl_str_mv |
Determinação de resíduos de ditiocarbamatos, empregando cromatografia gasosa acoplada a espectrometria de massas, em erva-mate (Ilex paraguariensis) produzida na América do Sul |
dc.title.alternative.eng.fl_str_mv |
Determination of dithiocarbamates residues, using gas chromatography coupled to mass spectrometry, in yerba mate (Ilex paraguariensis) produced in South America |
title |
Determinação de resíduos de ditiocarbamatos, empregando cromatografia gasosa acoplada a espectrometria de massas, em erva-mate (Ilex paraguariensis) produzida na América do Sul |
spellingShingle |
Determinação de resíduos de ditiocarbamatos, empregando cromatografia gasosa acoplada a espectrometria de massas, em erva-mate (Ilex paraguariensis) produzida na América do Sul Balbinot, Priscila Dotto Rosa Cromatografia gasosa Ditiocarbamatos Erva-mate Fungicidas Gas chromatography Dithiocarbamates Yerba mate Fungicides CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Determinação de resíduos de ditiocarbamatos, empregando cromatografia gasosa acoplada a espectrometria de massas, em erva-mate (Ilex paraguariensis) produzida na América do Sul |
title_full |
Determinação de resíduos de ditiocarbamatos, empregando cromatografia gasosa acoplada a espectrometria de massas, em erva-mate (Ilex paraguariensis) produzida na América do Sul |
title_fullStr |
Determinação de resíduos de ditiocarbamatos, empregando cromatografia gasosa acoplada a espectrometria de massas, em erva-mate (Ilex paraguariensis) produzida na América do Sul |
title_full_unstemmed |
Determinação de resíduos de ditiocarbamatos, empregando cromatografia gasosa acoplada a espectrometria de massas, em erva-mate (Ilex paraguariensis) produzida na América do Sul |
title_sort |
Determinação de resíduos de ditiocarbamatos, empregando cromatografia gasosa acoplada a espectrometria de massas, em erva-mate (Ilex paraguariensis) produzida na América do Sul |
author |
Balbinot, Priscila Dotto Rosa |
author_facet |
Balbinot, Priscila Dotto Rosa |
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 |
Silva, Rosselei Caiel da |
dc.contributor.referee2.fl_str_mv |
Hoffmann, Jessica |
dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/2472238156682970 |
dc.contributor.author.fl_str_mv |
Balbinot, Priscila Dotto Rosa |
contributor_str_mv |
Pizzutti, Ionara Regina Silva, Rosselei Caiel da Hoffmann, Jessica |
dc.subject.por.fl_str_mv |
Cromatografia gasosa Ditiocarbamatos Erva-mate Fungicidas |
topic |
Cromatografia gasosa Ditiocarbamatos Erva-mate Fungicidas Gas chromatography Dithiocarbamates Yerba mate Fungicides CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.eng.fl_str_mv |
Gas chromatography Dithiocarbamates Yerba mate Fungicides |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
Dithiocarbamates (DTC) fungicides have characteristics related to high instability when in the presence of moisture and oxygen, thus requiring special preparation of the sample to be worked on, as well as the development and validation of an individual method for analysis of the generated compounds. In this work, an individual method for the determination of DTC in yerba mate was miniaturized and validated, based on the acid hydrolysis of the sample in the presence of tin chloride II, purification of the extract and subsequent analysis of the carbon disulfide (CS2) generated using gas chromatography–mass spectrometry (GC-MS). The optimization conditions were evaluated through miniaturization in the sample extraction process, based on the amount of sample, volume of extracting solvent and acid solution and the stirring time during the hot bath. These conditions were compared to those already described in the literature. As it is a complex matrix, an extract purification step was carried out through the dispersive solid phase extraction (d-SPE) process using primary and secondary amine (PSA) as sorbents, graphitized carbon (GCB) in addition to magnesium sulfate (MgSO4) as a drier. For the method validation study, the following parameters were evaluated: linearity, matrix effect, limit of detection (LOD) and limit of quantification (LOQ), precision and accuracy. Within the results obtained in the validation study, the LOD was established at 0.05 mg L-1 CS2, and the LOQ at 0.1 mg kg-1 CS2. The coefficient of determination (r2) obtained through the analytical curves was r2 > 0.99. The results obtained through the precision study were acceptable values with RSDr ≤11.2% and RSDpi ≤19.4% and, as well as the recoveries, in the range of 71.3 to 118.2%. The matrix effect calculated was -5.1%, which is within acceptable values for determining trace levels of contaminants. The validation parameters are in accordance with those described in DG-SANTE (2019) and, therefore, suitable for the determination of DTC in yerba mate. The validated method proved to be faster, simpler, and cheaper when compared to the traditional method described in the literature and quite effective for determining DTC in yerba mate. The miniaturized method was applied to 58 samples produced and sold in southern Brazil, 3 produced in Brazil and exported to Uruguay, and 4 produced in Argentina and sold in Brazil. Of the 65 herb samples that were used for the monitoring study, 33.8% had detectable levels of CS2, and 14% had concentration levels higher than the LOQ. |
publishDate |
2022 |
dc.date.accessioned.fl_str_mv |
2022-05-31T17:54:07Z |
dc.date.available.fl_str_mv |
2022-05-31T17:54:07Z |
dc.date.issued.fl_str_mv |
2022-02-28 |
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/1/24607 |
url |
http://repositorio.ufsm.br/handle/1/24607 |
dc.language.iso.fl_str_mv |
por |
language |
por |
dc.relation.cnpq.fl_str_mv |
100600000000 |
dc.relation.confidence.fl_str_mv |
600 600 600 600 600 |
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:Manancial - Repositório Digital da UFSM instname:Universidade Federal de Santa Maria (UFSM) instacron:UFSM |
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UFSM |
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collection |
Manancial - Repositório Digital da UFSM |
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