Determinação de resíduos de agrotóxicos em mel empregando método QuEChERS modificado e GC-ECD
Autor(a) principal: | |
---|---|
Data de Publicação: | 2011 |
Tipo de documento: | Dissertação |
Idioma: | por |
Título da fonte: | Repositório Institucional Manancial UFSM |
Texto Completo: | http://repositorio.ufsm.br/handle/1/10490 |
Resumo: | The production of honey has been increasing continuously in the world in function of the greatest consume of natural products. It is related directly to human health, and stimulated by its therapeutics and nutritious qualities. Due to this, it is necessary the verification of the features related to honey quality as: physical-chemical characteristics and identification of the floral and geographic origin of this product. For such intention emerges the importance of the residues analysis and monitoring to ensure its supply. In this study was developed and validated a method for the determination of 23 pesticide residues in honey using modified QuEChERS method and Gas Chromatography with Electron Capture Detection (GC-ECD). The fortification of honey samples was preformed, with a solution containing the 23 pesticides, in 3 levels of concentration (10.0; 20.0 and 50.0 μg kg-1), 6 extractions of each level was realized, and the modified QuEChERS method was applied. This extraction method consisted to weight 2.5 g of honey and the addiction of 5 mL of a Na2EDTA solution 0.1 mol L-1 and 5 mL of acetonitrile followed by vortex shaking, for 3 min. Partition consisted of the addiction of 6.0 g of anhydrous magnesium sulfate and 1.5 g of sodium chloride shaked for 1 min, followed by centrifugation for 8 min. The purification of the extract was realized through a dispersive clean up step in which 2 mL of the extract was transferred to another tube, previously added 120 mg anhydrous magnesium sulfate and 100 mg of primary secondary amine (PSA) followed by vortex shaking and centrifugation. Finally the extracts were analyzed by GC-ECD. The linearity of the analytical curves (6 levels of concentration and 6 injections of each level), detection limit (LOD), quantification limit (LOQ), matrix effects, accuracy and precision of the analytical method were evaluated. In general the linear range of the analytical curves prepared in acetonitrile and matrix matched were between 5.0 or 10.0 to 100 μg L-1 with values of r2 > 0.99. The GC-ECD technique enables the quantification of 95.6% of the compounds and method LOQ of 3.0 or 6.0 μg kg-1. Therefore, the method proved appropriated for pesticide multiresidue determination in honey, as well, effective purification technique for honey extracts combining good sensitivity and selectivity. All the parameters evaluated are in agreement to limits suggested for chromatographic methods validation. |
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2017-05-122017-05-122011-08-03ORSO, Débora. Determination of pesticide residues in honey by modified QuEChERS method and GC-ECD. 2011. 118 f. Dissertação (Mestrado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2011.http://repositorio.ufsm.br/handle/1/10490The production of honey has been increasing continuously in the world in function of the greatest consume of natural products. It is related directly to human health, and stimulated by its therapeutics and nutritious qualities. Due to this, it is necessary the verification of the features related to honey quality as: physical-chemical characteristics and identification of the floral and geographic origin of this product. For such intention emerges the importance of the residues analysis and monitoring to ensure its supply. In this study was developed and validated a method for the determination of 23 pesticide residues in honey using modified QuEChERS method and Gas Chromatography with Electron Capture Detection (GC-ECD). The fortification of honey samples was preformed, with a solution containing the 23 pesticides, in 3 levels of concentration (10.0; 20.0 and 50.0 μg kg-1), 6 extractions of each level was realized, and the modified QuEChERS method was applied. This extraction method consisted to weight 2.5 g of honey and the addiction of 5 mL of a Na2EDTA solution 0.1 mol L-1 and 5 mL of acetonitrile followed by vortex shaking, for 3 min. Partition consisted of the addiction of 6.0 g of anhydrous magnesium sulfate and 1.5 g of sodium chloride shaked for 1 min, followed by centrifugation for 8 min. The purification of the extract was realized through a dispersive clean up step in which 2 mL of the extract was transferred to another tube, previously added 120 mg anhydrous magnesium sulfate and 100 mg of primary secondary amine (PSA) followed by vortex shaking and centrifugation. Finally the extracts were analyzed by GC-ECD. The linearity of the analytical curves (6 levels of concentration and 6 injections of each level), detection limit (LOD), quantification limit (LOQ), matrix effects, accuracy and precision of the analytical method were evaluated. In general the linear range of the analytical curves prepared in acetonitrile and matrix matched were between 5.0 or 10.0 to 100 μg L-1 with values of r2 > 0.99. The GC-ECD technique enables the quantification of 95.6% of the compounds and method LOQ of 3.0 or 6.0 μg kg-1. Therefore, the method proved appropriated for pesticide multiresidue determination in honey, as well, effective purification technique for honey extracts combining good sensitivity and selectivity. All the parameters evaluated are in agreement to limits suggested for chromatographic methods validation.A produção mundial de mel vem crescendo continuamente em função do maior consumo de produtos naturais, estando relacionado diretamente com a saúde dos consumidores e estimulado pelas suas qualidades terapêuticas e nutricionais. Torna-se necessário, portanto, a verificação da adequação das características relacionadas à qualidade do mel, tais como, as suas características físico-químicas e a identificação da origem floral e geográfica deste produto. Para tal finalidade, surge a importância da análise de resíduos e o necessário monitoramento destes, para que o seu suprimento seja garantido. Neste estudo, foi desenvolvido e validado um método para a determinação de resíduos de 23 agrotóxicos em mel, analisados pela utilização do método de extração QuEChERS modificado e Cromatografia Gasosa com Detector por Captura de Elétrons (GC-ECD). Dessa forma, efetuou-se a fortificação da amostra de mel, com soluções contendo os 23 agrotóxicos, em 3 níveis de fortificação (10,0; 20,0 e 50,0 μg kg-1), 6 réplicas para cada nível, e aplicou-se o método QuEChERS modificado. Este método de extração consistiu em pesar 2,5 g da matriz, adição de 5 mL da solução Na2EDTA 0,1 mol L-1 e 5 mL de acetonitrila, após efetuouse a agitação em vortex, por 3 min. Acrescentou-se 6,0 g de sulfato de magnésio anidro e 1,5 g de cloreto de sódio, agitando-se novamente por 1 min. Posteriormente, ocorreu a centrifugação por 8 min. A purificação dos extratos foi realizada através da etapa de clean-up dispersivo, em que 2 mL do extrato foram transferidos para outro tubo contendo 120 mg de sulfato de magnésio anidro e 100 mg de amina primária secundária (PSA), repetindo-se a agitação e centrifugação e, em seguida, os extratos foram analisados por GC-ECD. Avaliou-se a linearidade das curvas analíticas (6 níveis de concentração e seis injeções de cada nível), limite de detecção (LOD), limite de quantificação (LOQ), efeito matriz, exatidão e precisão do método analítico. Em geral, a faixa linear de concentração das curvas analíticas, preparadas em acetonitrila e no extrato da matriz, situou-se entre 5,0 ou 10,0 a 100 μg L-1 com valores de r2 > 0,99. A técnica GC-ECD promoveu a quantificação de 95,6% dos compostos que apresentaram LOQ do método de 3,0 ou 6,0 μg kg-1. Portanto, conclui-se que o método mostrou-se adequado à determinação multirresíduo dos agrotóxicos em mel, bem como, a técnica de purificação dos extratos de mel foi eficiente, conciliando sensibilidade e seletividade adequadas, e todos os parâmetros de validação encontram-se dentro dos limites sugeridos para validação de métodos cromatográficos.application/pdfporUniversidade Federal de Santa MariaPrograma de Pós-Graduação em QuímicaUFSMBRQuímicaMelAgrotóxicosMétodo QuEChERSGC-ECDHoneyPesticidesQuEChERS methodGC-ECDCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICADeterminação de resíduos de agrotóxicos em mel empregando método QuEChERS modificado e GC-ECDDetermination of pesticide residues in honey by modified QuEChERS method and GC-ECDinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisZanella, Renatohttp://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4781698T9Mazutti, Marcio Antoniohttp://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4770663T7Prestes, Osmar Damianhttp://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4702776A6http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4291420U0Orso, Débora1006000000004005003005005000aa2baab-94e8-4d3d-bbb2-85495ba77db5d4d8e623-61bf-4f45-99e6-5f27e691123b67e239f9-31ad-4d6b-9c76-bea8273292994eef7b33-113c-470f-8729-f99c250df028info:eu-repo/semantics/openAccessreponame:Repositório Institucional Manancial UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMORIGINALORSO, DEBORA.pdfapplication/pdf1126381http://repositorio.ufsm.br/bitstream/1/10490/1/ORSO%2c%20DEBORA.pdf8bce957f117bbc70bb61f7deb9ea0aa3MD51TEXTORSO, DEBORA.pdf.txtORSO, DEBORA.pdf.txtExtracted texttext/plain222328http://repositorio.ufsm.br/bitstream/1/10490/2/ORSO%2c%20DEBORA.pdf.txt9c52dd3bedc8ae3a85ed0117a0e8ff25MD52THUMBNAILORSO, DEBORA.pdf.jpgORSO, DEBORA.pdf.jpgIM Thumbnailimage/jpeg5701http://repositorio.ufsm.br/bitstream/1/10490/3/ORSO%2c%20DEBORA.pdf.jpg3b9ea4f46cccb25d24ad895f1f8868a4MD531/104902017-07-25 12:05:09.477oai:repositorio.ufsm.br:1/10490Repositório Institucionalhttp://repositorio.ufsm.br/PUBhttp://repositorio.ufsm.br/oai/requestouvidoria@ufsm.bropendoar:39132017-07-25T15:05:09Repositório Institucional Manancial UFSM - Universidade Federal de Santa Maria (UFSM)false |
dc.title.por.fl_str_mv |
Determinação de resíduos de agrotóxicos em mel empregando método QuEChERS modificado e GC-ECD |
dc.title.alternative.eng.fl_str_mv |
Determination of pesticide residues in honey by modified QuEChERS method and GC-ECD |
title |
Determinação de resíduos de agrotóxicos em mel empregando método QuEChERS modificado e GC-ECD |
spellingShingle |
Determinação de resíduos de agrotóxicos em mel empregando método QuEChERS modificado e GC-ECD Orso, Débora Mel Agrotóxicos Método QuEChERS GC-ECD Honey Pesticides QuEChERS method GC-ECD CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Determinação de resíduos de agrotóxicos em mel empregando método QuEChERS modificado e GC-ECD |
title_full |
Determinação de resíduos de agrotóxicos em mel empregando método QuEChERS modificado e GC-ECD |
title_fullStr |
Determinação de resíduos de agrotóxicos em mel empregando método QuEChERS modificado e GC-ECD |
title_full_unstemmed |
Determinação de resíduos de agrotóxicos em mel empregando método QuEChERS modificado e GC-ECD |
title_sort |
Determinação de resíduos de agrotóxicos em mel empregando método QuEChERS modificado e GC-ECD |
author |
Orso, Débora |
author_facet |
Orso, Débora |
author_role |
author |
dc.contributor.advisor1.fl_str_mv |
Zanella, Renato |
dc.contributor.advisor1Lattes.fl_str_mv |
http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4781698T9 |
dc.contributor.referee1.fl_str_mv |
Mazutti, Marcio Antonio |
dc.contributor.referee1Lattes.fl_str_mv |
http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4770663T7 |
dc.contributor.referee2.fl_str_mv |
Prestes, Osmar Damian |
dc.contributor.referee2Lattes.fl_str_mv |
http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4702776A6 |
dc.contributor.authorLattes.fl_str_mv |
http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4291420U0 |
dc.contributor.author.fl_str_mv |
Orso, Débora |
contributor_str_mv |
Zanella, Renato Mazutti, Marcio Antonio Prestes, Osmar Damian |
dc.subject.por.fl_str_mv |
Mel Agrotóxicos Método QuEChERS GC-ECD |
topic |
Mel Agrotóxicos Método QuEChERS GC-ECD Honey Pesticides QuEChERS method GC-ECD CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.eng.fl_str_mv |
Honey Pesticides QuEChERS method GC-ECD |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
The production of honey has been increasing continuously in the world in function of the greatest consume of natural products. It is related directly to human health, and stimulated by its therapeutics and nutritious qualities. Due to this, it is necessary the verification of the features related to honey quality as: physical-chemical characteristics and identification of the floral and geographic origin of this product. For such intention emerges the importance of the residues analysis and monitoring to ensure its supply. In this study was developed and validated a method for the determination of 23 pesticide residues in honey using modified QuEChERS method and Gas Chromatography with Electron Capture Detection (GC-ECD). The fortification of honey samples was preformed, with a solution containing the 23 pesticides, in 3 levels of concentration (10.0; 20.0 and 50.0 μg kg-1), 6 extractions of each level was realized, and the modified QuEChERS method was applied. This extraction method consisted to weight 2.5 g of honey and the addiction of 5 mL of a Na2EDTA solution 0.1 mol L-1 and 5 mL of acetonitrile followed by vortex shaking, for 3 min. Partition consisted of the addiction of 6.0 g of anhydrous magnesium sulfate and 1.5 g of sodium chloride shaked for 1 min, followed by centrifugation for 8 min. The purification of the extract was realized through a dispersive clean up step in which 2 mL of the extract was transferred to another tube, previously added 120 mg anhydrous magnesium sulfate and 100 mg of primary secondary amine (PSA) followed by vortex shaking and centrifugation. Finally the extracts were analyzed by GC-ECD. The linearity of the analytical curves (6 levels of concentration and 6 injections of each level), detection limit (LOD), quantification limit (LOQ), matrix effects, accuracy and precision of the analytical method were evaluated. In general the linear range of the analytical curves prepared in acetonitrile and matrix matched were between 5.0 or 10.0 to 100 μg L-1 with values of r2 > 0.99. The GC-ECD technique enables the quantification of 95.6% of the compounds and method LOQ of 3.0 or 6.0 μg kg-1. Therefore, the method proved appropriated for pesticide multiresidue determination in honey, as well, effective purification technique for honey extracts combining good sensitivity and selectivity. All the parameters evaluated are in agreement to limits suggested for chromatographic methods validation. |
publishDate |
2011 |
dc.date.issued.fl_str_mv |
2011-08-03 |
dc.date.accessioned.fl_str_mv |
2017-05-12 |
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2017-05-12 |
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info:eu-repo/semantics/masterThesis |
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masterThesis |
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publishedVersion |
dc.identifier.citation.fl_str_mv |
ORSO, Débora. Determination of pesticide residues in honey by modified QuEChERS method and GC-ECD. 2011. 118 f. Dissertação (Mestrado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2011. |
dc.identifier.uri.fl_str_mv |
http://repositorio.ufsm.br/handle/1/10490 |
identifier_str_mv |
ORSO, Débora. Determination of pesticide residues in honey by modified QuEChERS method and GC-ECD. 2011. 118 f. Dissertação (Mestrado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2011. |
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http://repositorio.ufsm.br/handle/1/10490 |
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Química |
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