Determinação de resíduos de agrotóxicos no leite bovino empregando método QuEChERS modificado e GC-MS/MS
Autor(a) principal: | |
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Data de Publicação: | 2012 |
Tipo de documento: | Dissertação |
Idioma: | por |
Título da fonte: | Manancial - Repositório Digital da UFSM |
Texto Completo: | http://repositorio.ufsm.br/handle/1/10504 |
Resumo: | For providing a balanced composition, among fresh food, the milk is considered one of the most nutritionally complete, being a product very well accepted in the market with consumers of all ages. Thus, the analysis of milk quality is great importance for consumer information and verification of the parameters required by law. Considering all the problems involving the many chemicals used for several purposes in agriculture, and the possibility of these compounds directly or indirectly the milk and cause damage to population health, this work aimed to develope and validate a method for a multiresidue determination of 48 pesticides in cattle milk, using modified QuEChERS method and GC-MS/MS. The extraction procedure consisted of 5.0 mL of sample (milk) extracted with 5.0 mL of acetonitrile, acidified with 1% of acetic acid (v/v), followed by manual shaking for 1 min for partition step was used 2.0 g of anhydrous MgSO4 and 0.85 g of anhydrous sodium acetate. Manual agitation was repeated for 1 min, and subsequently it was performed centrifugation at 3400 rpm for 8 min. The dispersive clean up step consisted in add 1.0 mL of supernatant extract, 150.0 mg of anhydrous MgSO4, 125.0 mg of C18 and 62.0 mg of PSA in an eppendorf tube, which was shaked in a vortex for 1 min, centrifuged at 10000 rpm for 3 min. After centrifugation, the extract was transferred to a glass insert for the injection into the GC-MS/MS system. It was evaluated the linearity, limits of detection (LOD) and quantitation (LOQ), the matrix effect, accuracy and precision of the analytical method. The method proved to be efficient, with satisfactory results for recoveries, with values in a range between 71.1 and 117.4% for 45 of the 48 compounds analyzed. RSD values lowerd than 17,3%, values of LODi and LODm ranged between 0.3 to 3.0 μg L-1 and LOQi and LOQm ranged between 1.0 to 10.0 μg L-1. The validated method was applied for the determination of residues of 45 pesticides/degradation products in samples of milk UHT. The method developed was adequate for the analysis of pesticide residues in cattle milk, as all the validation parameters were within the limits required for validation of chromatographic methods, achieving satisfactorily the objectives outlined in this paper. |
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Determinação de resíduos de agrotóxicos no leite bovino empregando método QuEChERS modificado e GC-MS/MSDetermination of pesticide residues in cattle milk using modified QuEChERS method and GC-MS/MSLeiteAgrotóxicosQuEChERS modificadoGC-MS/MSPesticideMilkModified QuEChERSGC-MS/MSCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICAFor providing a balanced composition, among fresh food, the milk is considered one of the most nutritionally complete, being a product very well accepted in the market with consumers of all ages. Thus, the analysis of milk quality is great importance for consumer information and verification of the parameters required by law. Considering all the problems involving the many chemicals used for several purposes in agriculture, and the possibility of these compounds directly or indirectly the milk and cause damage to population health, this work aimed to develope and validate a method for a multiresidue determination of 48 pesticides in cattle milk, using modified QuEChERS method and GC-MS/MS. The extraction procedure consisted of 5.0 mL of sample (milk) extracted with 5.0 mL of acetonitrile, acidified with 1% of acetic acid (v/v), followed by manual shaking for 1 min for partition step was used 2.0 g of anhydrous MgSO4 and 0.85 g of anhydrous sodium acetate. Manual agitation was repeated for 1 min, and subsequently it was performed centrifugation at 3400 rpm for 8 min. The dispersive clean up step consisted in add 1.0 mL of supernatant extract, 150.0 mg of anhydrous MgSO4, 125.0 mg of C18 and 62.0 mg of PSA in an eppendorf tube, which was shaked in a vortex for 1 min, centrifuged at 10000 rpm for 3 min. After centrifugation, the extract was transferred to a glass insert for the injection into the GC-MS/MS system. It was evaluated the linearity, limits of detection (LOD) and quantitation (LOQ), the matrix effect, accuracy and precision of the analytical method. The method proved to be efficient, with satisfactory results for recoveries, with values in a range between 71.1 and 117.4% for 45 of the 48 compounds analyzed. RSD values lowerd than 17,3%, values of LODi and LODm ranged between 0.3 to 3.0 μg L-1 and LOQi and LOQm ranged between 1.0 to 10.0 μg L-1. The validated method was applied for the determination of residues of 45 pesticides/degradation products in samples of milk UHT. The method developed was adequate for the analysis of pesticide residues in cattle milk, as all the validation parameters were within the limits required for validation of chromatographic methods, achieving satisfactorily the objectives outlined in this paper.Por oferecer uma composição equilibrada, o leite é considerado um dos alimentos in natura mais completos nutricionalmente, sendo um produto muito bem aceito no mercado e tendo consumidores de todas as idades. Sendo assim, a análise da qualidade do leite é de grande importância para informação do consumidor e verificação dos parâmetros exigidos pela legislação. Considerando toda a problemática envolvendo as inúmeras substâncias químicas utilizadas com finalidades diversas na agropecuária, e a possibilidade destas chegarem direta ou indiretamente até o leite e causarem danos a saúde da população, neste trabalho foi desenvolvido e validado um método multirresíduo para a determinação de 48 agrotóxicos em leite de vaca, empregando método QuEChERS modificado e GCMS/ MS. O procedimento de extração consistiu em 5,0 mL de amostra (leite integral) extraída com 5,0 mL de acetonitrila acidificada com 1% de ácido acético (v/v), seguido de agitação manual por 1 min, para a etapa de partição utilizou-se 2,0 g de MgSO4 anidro e 0,85 g de acetato de sódio. Repetiu-se a agitação manual por 1 min, e posteriormente foi realizada a etapa de centrifugação a 3400 rpm, durante 8 min. A etapa de limpeza dispersiva, consistiu em 1,0 mL de extrato sobrenadante, 150 mg de MgSO4 anidro, 125 mg de C18 e 62 mg de PSA em tubo eppendorf, os quais foram agitados em vortex por 1 min centrifugados a 10000 rpm por 3 min. Após a centrifugação, o extrato foi transferido para o insert de vidro para injeção no sistema GC-MS/MS. Avaliou-se a linearidade, os limites de detecção (LOD) e quantificação (LOQ), o efeito matriz, a exatidão e a precisão do método analítico. O método demonstrou ser eficiente, apresentando resultados satisfatórios para recuperações, as quais se situaram na faixa entre 71,1 e 117,4%, para 45 dos 48 compostos avaliados, com valores de RSD ≤ 17,3%, os valores de LODi bem como o LODm variaram entre 0,3 e 3,0 μg L-1 e o LOQi e o LOQm variaram entre 1,0 e 10 μg L-1. O método validado foi aplicado para a determinação de resíduos de 45 agrotóxicos/produtos de degradação em amostras de leite UHT. O método desenvolvido mostrou-se adequado a análise de resíduos de agrotóxicos em leite, pois todos os parâmetros de validação encontraram-se dentro dos limites exigidos para validação de métodos cromatográficos, atendendo satisfatoriamente os objetivos traçados neste trabalho.Universidade Federal de Santa MariaBRQuímicaUFSMPrograma de Pós-Graduação em QuímicaAdaime, Martha Bohrerhttp://lattes.cnpq.br/4385786922516848Richards, Neila Silvia Pereira dos Santoshttp://lattes.cnpq.br/0618653776990780Prestes, Osmar Damianhttp://lattes.cnpq.br/9632234955509028Bandeira, Danieli Daiani2017-05-122017-05-122012-03-26info:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisapplication/pdfapplication/pdfBANDEIRA, Danieli Daiani. Determination of pesticide residues in cattle milk using modified QuEChERS method and GC-MS/MS. 2012. 126 f. Dissertação (Mestrado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2012.http://repositorio.ufsm.br/handle/1/10504porinfo:eu-repo/semantics/openAccessreponame:Manancial - Repositório Digital da UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSM2021-09-16T11:42:17Zoai:repositorio.ufsm.br:1/10504Biblioteca Digital de Teses e Dissertaçõeshttps://repositorio.ufsm.br/ONGhttps://repositorio.ufsm.br/oai/requestatendimento.sib@ufsm.br||tedebc@gmail.comopendoar:2021-09-16T11:42:17Manancial - Repositório Digital da UFSM - Universidade Federal de Santa Maria (UFSM)false |
dc.title.none.fl_str_mv |
Determinação de resíduos de agrotóxicos no leite bovino empregando método QuEChERS modificado e GC-MS/MS Determination of pesticide residues in cattle milk using modified QuEChERS method and GC-MS/MS |
title |
Determinação de resíduos de agrotóxicos no leite bovino empregando método QuEChERS modificado e GC-MS/MS |
spellingShingle |
Determinação de resíduos de agrotóxicos no leite bovino empregando método QuEChERS modificado e GC-MS/MS Bandeira, Danieli Daiani Leite Agrotóxicos QuEChERS modificado GC-MS/MS Pesticide Milk Modified QuEChERS GC-MS/MS CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Determinação de resíduos de agrotóxicos no leite bovino empregando método QuEChERS modificado e GC-MS/MS |
title_full |
Determinação de resíduos de agrotóxicos no leite bovino empregando método QuEChERS modificado e GC-MS/MS |
title_fullStr |
Determinação de resíduos de agrotóxicos no leite bovino empregando método QuEChERS modificado e GC-MS/MS |
title_full_unstemmed |
Determinação de resíduos de agrotóxicos no leite bovino empregando método QuEChERS modificado e GC-MS/MS |
title_sort |
Determinação de resíduos de agrotóxicos no leite bovino empregando método QuEChERS modificado e GC-MS/MS |
author |
Bandeira, Danieli Daiani |
author_facet |
Bandeira, Danieli Daiani |
author_role |
author |
dc.contributor.none.fl_str_mv |
Adaime, Martha Bohrer http://lattes.cnpq.br/4385786922516848 Richards, Neila Silvia Pereira dos Santos http://lattes.cnpq.br/0618653776990780 Prestes, Osmar Damian http://lattes.cnpq.br/9632234955509028 |
dc.contributor.author.fl_str_mv |
Bandeira, Danieli Daiani |
dc.subject.por.fl_str_mv |
Leite Agrotóxicos QuEChERS modificado GC-MS/MS Pesticide Milk Modified QuEChERS GC-MS/MS CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
topic |
Leite Agrotóxicos QuEChERS modificado GC-MS/MS Pesticide Milk Modified QuEChERS GC-MS/MS CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
For providing a balanced composition, among fresh food, the milk is considered one of the most nutritionally complete, being a product very well accepted in the market with consumers of all ages. Thus, the analysis of milk quality is great importance for consumer information and verification of the parameters required by law. Considering all the problems involving the many chemicals used for several purposes in agriculture, and the possibility of these compounds directly or indirectly the milk and cause damage to population health, this work aimed to develope and validate a method for a multiresidue determination of 48 pesticides in cattle milk, using modified QuEChERS method and GC-MS/MS. The extraction procedure consisted of 5.0 mL of sample (milk) extracted with 5.0 mL of acetonitrile, acidified with 1% of acetic acid (v/v), followed by manual shaking for 1 min for partition step was used 2.0 g of anhydrous MgSO4 and 0.85 g of anhydrous sodium acetate. Manual agitation was repeated for 1 min, and subsequently it was performed centrifugation at 3400 rpm for 8 min. The dispersive clean up step consisted in add 1.0 mL of supernatant extract, 150.0 mg of anhydrous MgSO4, 125.0 mg of C18 and 62.0 mg of PSA in an eppendorf tube, which was shaked in a vortex for 1 min, centrifuged at 10000 rpm for 3 min. After centrifugation, the extract was transferred to a glass insert for the injection into the GC-MS/MS system. It was evaluated the linearity, limits of detection (LOD) and quantitation (LOQ), the matrix effect, accuracy and precision of the analytical method. The method proved to be efficient, with satisfactory results for recoveries, with values in a range between 71.1 and 117.4% for 45 of the 48 compounds analyzed. RSD values lowerd than 17,3%, values of LODi and LODm ranged between 0.3 to 3.0 μg L-1 and LOQi and LOQm ranged between 1.0 to 10.0 μg L-1. The validated method was applied for the determination of residues of 45 pesticides/degradation products in samples of milk UHT. The method developed was adequate for the analysis of pesticide residues in cattle milk, as all the validation parameters were within the limits required for validation of chromatographic methods, achieving satisfactorily the objectives outlined in this paper. |
publishDate |
2012 |
dc.date.none.fl_str_mv |
2012-03-26 2017-05-12 2017-05-12 |
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 |
BANDEIRA, Danieli Daiani. Determination of pesticide residues in cattle milk using modified QuEChERS method and GC-MS/MS. 2012. 126 f. Dissertação (Mestrado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2012. http://repositorio.ufsm.br/handle/1/10504 |
identifier_str_mv |
BANDEIRA, Danieli Daiani. Determination of pesticide residues in cattle milk using modified QuEChERS method and GC-MS/MS. 2012. 126 f. Dissertação (Mestrado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2012. |
url |
http://repositorio.ufsm.br/handle/1/10504 |
dc.language.iso.fl_str_mv |
por |
language |
por |
dc.rights.driver.fl_str_mv |
info:eu-repo/semantics/openAccess |
eu_rights_str_mv |
openAccess |
dc.format.none.fl_str_mv |
application/pdf application/pdf |
dc.publisher.none.fl_str_mv |
Universidade Federal de Santa Maria BR Química UFSM Programa de Pós-Graduação em Química |
publisher.none.fl_str_mv |
Universidade Federal de Santa Maria BR Química UFSM Programa de Pós-Graduação em Química |
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_ |
1805922146030977024 |