Determinação multirresíduo de agrotóxicos em bebidas à base de soja empregando método QuEChERS e UHPLC-MS/MS
Ano de defesa: | 2016 |
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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/1/10617 |
Resumo: | Soy beverages are aqueous extracts of soybeans which are a source of high quality protein and no contains cholesterol or lactose, can be considered functional foods. These beverages have a large acceptance among consumers and due to they are extracted from the grain, the beneficial components are preserved, but may also contain residues of pesticides used to control pest infestation during the growing of the grains. This study aimed to develop and validate a multiresidue method based on QuEChERS extraction for the simultaneous determination of 41 pesticides in soy-based beverages using ultra-high performance liquid chromatography coupled with tandem mass spectrometry (UHPLC-MS/MS). In the sample preparation step, it was used 10 mL of sample and 10 mL of acetonitrile and addition of salts. The clean-up procedure was optimized by experimental design, evaluating different quantities of the sorbents primary secondary amine (PSA) and octadecylsilane (C18).The clean-up step was performed with magnesium sulfate anhydrous and C18. To assess the accuracy of the method, blank samples were spiked at 10, 25 and 50 μg L-1 with n = 6. To evaluate the matrix effect, inclinations of curves in acetonitrile and blank extract of the matrix were compared. The results of the validation are satisfactory, since the method presented optimized recoveries between 70 and 112% with RSD less than 19%. Curves were prepared in the matrix extract, due to some compounds presented pronounced matrix effect. The curves showed r² ≥ 0,99 for all compounds in the range between the respective limit of quantification and 50 μg L-1. The method proved to be suitable for the determination of the compounds and may be used for routine analysis. |
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2017-05-192017-05-192016-02-26MAY, Marília Melina. Multiresidue determination of pesticides in soy-based beverages using a QuEChERS method and UHPLC-MS/MS. 2016. 99 f. Dissertação (Mestrado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2016.http://repositorio.ufsm.br/handle/1/10617Soy beverages are aqueous extracts of soybeans which are a source of high quality protein and no contains cholesterol or lactose, can be considered functional foods. These beverages have a large acceptance among consumers and due to they are extracted from the grain, the beneficial components are preserved, but may also contain residues of pesticides used to control pest infestation during the growing of the grains. This study aimed to develop and validate a multiresidue method based on QuEChERS extraction for the simultaneous determination of 41 pesticides in soy-based beverages using ultra-high performance liquid chromatography coupled with tandem mass spectrometry (UHPLC-MS/MS). In the sample preparation step, it was used 10 mL of sample and 10 mL of acetonitrile and addition of salts. The clean-up procedure was optimized by experimental design, evaluating different quantities of the sorbents primary secondary amine (PSA) and octadecylsilane (C18).The clean-up step was performed with magnesium sulfate anhydrous and C18. To assess the accuracy of the method, blank samples were spiked at 10, 25 and 50 μg L-1 with n = 6. To evaluate the matrix effect, inclinations of curves in acetonitrile and blank extract of the matrix were compared. The results of the validation are satisfactory, since the method presented optimized recoveries between 70 and 112% with RSD less than 19%. Curves were prepared in the matrix extract, due to some compounds presented pronounced matrix effect. The curves showed r² ≥ 0,99 for all compounds in the range between the respective limit of quantification and 50 μg L-1. The method proved to be suitable for the determination of the compounds and may be used for routine analysis.Bebidas à base de soja são extratos aquosos do grão de soja, que representam uma fonte de proteínas de alta qualidade e não contém colesterol ou lactose, podendo ser consideradas alimentos funcionais. Essas bebidas têm grande aceitabilidade entre consumidores e por serem extraídas do grão, os componentes benéficos são preservados, mas também podem conter resíduos de agrotóxicos empregados para controlar a infestação de pragas durante o cultivo dos grãos. O presente trabalho teve por objetivo desenvolver e validar um método multirresíduo baseado na extração por QuEChERS para a determinação simultânea de 41 agrotóxicos em bebidas à base de soja por meio de cromatografia líquida de ultra alta eficiência acoplada à espectrometria de massas em série (UHPLC-MS/MS). Na etapa de preparo de amostra, utilizou-se 10 mL de amostra e 10 mL de acetonitrila e adição de sais. O procedimento de limpeza dos extratos foi otimizado a partir de planejamento experimental, avaliando diferentes quantidades dos sorventes amina primária secundária (PSA) e octadecilsilano (C18). A etapa de limpeza dos extratos foi realizada com sulfato de magnésio anidro e C18. Para avaliar a exatidão do método, amostras branco foram fortificadas nos níveis de 10, 25 e 50 μg L-1, com n = 6. Para avaliação do efeito matriz foram comparadas as inclinações de curvas em acetonitrila e no extrato branco da matriz. Os resultados da validação foram satisfatórios, já que o método otimizado apresentou recuperações entre 70 e 112%, com RSD menor que 19%. As curvas foram preparadas no extrato da matriz, devido a alguns compostos apresentarem efeito matriz acentuado. Foi obtido r² ≥ 0,99 para todos os compostos, na faixa entre os respectivos limites de quantificação e 50 μg L-1. O método provou ser adequado para a determinação dos compostos e pode ser utilizado para análises de rotina.Conselho Nacional de Desenvolvimento Científico e Tecnológicoapplication/pdfporUniversidade Federal de Santa MariaPrograma de Pós-Graduação em QuímicaUFSMBRQuímicaBebidas à base de sojaAgrotóxicosQuEChERSPlanejamento experimentalUHPLC-MS/MSSoy-based beveragesPesticidesQuEChERSExperimental designUHPLC-MS/MSCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICADeterminação multirresíduo de agrotóxicos em bebidas à base de soja empregando método QuEChERS e UHPLC-MS/MSMultiresidue determination of pesticides in soy-based beverages using a QuEChERS method and UHPLC-MS/MSinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisAdaime, Martha Bohrerhttp://lattes.cnpq.br/4385786922516848Friedrich, Maria Terezahttp://lattes.cnpq.br/4262267680099526Zanella, Renatohttp://lattes.cnpq.br/2541865299438479http://lattes.cnpq.br/0702121937232751May, Marília Melina1006000000004005003003005007a851b28-0ef7-4e7d-9bed-bfbacf6d9791df8d58b3-8fe0-48b3-91a5-daa8cfa84ce58a3791e5-69f3-40a3-88f2-da6decbf4cdf91ca9a05-efa0-482c-9364-32cd291280e8info:eu-repo/semantics/openAccessreponame:Manancial - Repositório Digital da UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMORIGINALMAY, MARILIA MELINA.pdfapplication/pdf3868338http://repositorio.ufsm.br/bitstream/1/10617/1/MAY%2c%20MARILIA%20MELINA.pdf220a1bda99afd647e8c8877a246f1bf2MD51TEXTMAY, MARILIA MELINA.pdf.txtMAY, MARILIA MELINA.pdf.txtExtracted texttext/plain151892http://repositorio.ufsm.br/bitstream/1/10617/2/MAY%2c%20MARILIA%20MELINA.pdf.txtd68031d693e592f182f9a0f6d2674d72MD52THUMBNAILMAY, MARILIA MELINA.pdf.jpgMAY, MARILIA MELINA.pdf.jpgIM Thumbnailimage/jpeg4462http://repositorio.ufsm.br/bitstream/1/10617/3/MAY%2c%20MARILIA%20MELINA.pdf.jpga01c44baf3d0de8219902d5f57675b12MD531/106172021-09-16 09:05:33.793oai:repositorio.ufsm.br:1/10617Repositório Institucionalhttp://repositorio.ufsm.br/PUBhttp://repositorio.ufsm.br/oai/requestopendoar:39132021-09-16T12:05:33Manancial - Repositório Digital da UFSM - Universidade Federal de Santa Maria (UFSM)false |
dc.title.por.fl_str_mv |
Determinação multirresíduo de agrotóxicos em bebidas à base de soja empregando método QuEChERS e UHPLC-MS/MS |
dc.title.alternative.eng.fl_str_mv |
Multiresidue determination of pesticides in soy-based beverages using a QuEChERS method and UHPLC-MS/MS |
title |
Determinação multirresíduo de agrotóxicos em bebidas à base de soja empregando método QuEChERS e UHPLC-MS/MS |
spellingShingle |
Determinação multirresíduo de agrotóxicos em bebidas à base de soja empregando método QuEChERS e UHPLC-MS/MS May, Marília Melina Bebidas à base de soja Agrotóxicos QuEChERS Planejamento experimental UHPLC-MS/MS Soy-based beverages Pesticides QuEChERS Experimental design UHPLC-MS/MS CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Determinação multirresíduo de agrotóxicos em bebidas à base de soja empregando método QuEChERS e UHPLC-MS/MS |
title_full |
Determinação multirresíduo de agrotóxicos em bebidas à base de soja empregando método QuEChERS e UHPLC-MS/MS |
title_fullStr |
Determinação multirresíduo de agrotóxicos em bebidas à base de soja empregando método QuEChERS e UHPLC-MS/MS |
title_full_unstemmed |
Determinação multirresíduo de agrotóxicos em bebidas à base de soja empregando método QuEChERS e UHPLC-MS/MS |
title_sort |
Determinação multirresíduo de agrotóxicos em bebidas à base de soja empregando método QuEChERS e UHPLC-MS/MS |
author |
May, Marília Melina |
author_facet |
May, Marília Melina |
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 |
Friedrich, Maria Tereza |
dc.contributor.referee1Lattes.fl_str_mv |
http://lattes.cnpq.br/4262267680099526 |
dc.contributor.referee2.fl_str_mv |
Zanella, Renato |
dc.contributor.referee2Lattes.fl_str_mv |
http://lattes.cnpq.br/2541865299438479 |
dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/0702121937232751 |
dc.contributor.author.fl_str_mv |
May, Marília Melina |
contributor_str_mv |
Adaime, Martha Bohrer Friedrich, Maria Tereza Zanella, Renato |
dc.subject.por.fl_str_mv |
Bebidas à base de soja Agrotóxicos QuEChERS Planejamento experimental UHPLC-MS/MS |
topic |
Bebidas à base de soja Agrotóxicos QuEChERS Planejamento experimental UHPLC-MS/MS Soy-based beverages Pesticides QuEChERS Experimental design UHPLC-MS/MS CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.eng.fl_str_mv |
Soy-based beverages Pesticides QuEChERS Experimental design UHPLC-MS/MS |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
Soy beverages are aqueous extracts of soybeans which are a source of high quality protein and no contains cholesterol or lactose, can be considered functional foods. These beverages have a large acceptance among consumers and due to they are extracted from the grain, the beneficial components are preserved, but may also contain residues of pesticides used to control pest infestation during the growing of the grains. This study aimed to develop and validate a multiresidue method based on QuEChERS extraction for the simultaneous determination of 41 pesticides in soy-based beverages using ultra-high performance liquid chromatography coupled with tandem mass spectrometry (UHPLC-MS/MS). In the sample preparation step, it was used 10 mL of sample and 10 mL of acetonitrile and addition of salts. The clean-up procedure was optimized by experimental design, evaluating different quantities of the sorbents primary secondary amine (PSA) and octadecylsilane (C18).The clean-up step was performed with magnesium sulfate anhydrous and C18. To assess the accuracy of the method, blank samples were spiked at 10, 25 and 50 μg L-1 with n = 6. To evaluate the matrix effect, inclinations of curves in acetonitrile and blank extract of the matrix were compared. The results of the validation are satisfactory, since the method presented optimized recoveries between 70 and 112% with RSD less than 19%. Curves were prepared in the matrix extract, due to some compounds presented pronounced matrix effect. The curves showed r² ≥ 0,99 for all compounds in the range between the respective limit of quantification and 50 μg L-1. The method proved to be suitable for the determination of the compounds and may be used for routine analysis. |
publishDate |
2016 |
dc.date.issued.fl_str_mv |
2016-02-26 |
dc.date.accessioned.fl_str_mv |
2017-05-19 |
dc.date.available.fl_str_mv |
2017-05-19 |
dc.type.status.fl_str_mv |
info:eu-repo/semantics/publishedVersion |
dc.type.driver.fl_str_mv |
info:eu-repo/semantics/masterThesis |
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masterThesis |
status_str |
publishedVersion |
dc.identifier.citation.fl_str_mv |
MAY, Marília Melina. Multiresidue determination of pesticides in soy-based beverages using a QuEChERS method and UHPLC-MS/MS. 2016. 99 f. Dissertação (Mestrado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2016. |
dc.identifier.uri.fl_str_mv |
http://repositorio.ufsm.br/handle/1/10617 |
identifier_str_mv |
MAY, Marília Melina. Multiresidue determination of pesticides in soy-based beverages using a QuEChERS method and UHPLC-MS/MS. 2016. 99 f. Dissertação (Mestrado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2016. |
url |
http://repositorio.ufsm.br/handle/1/10617 |
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100600000000 |
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Universidade Federal de Santa Maria |
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