Desenvolvimento e validação de método multirresíduo por QuEChERS e HPLC-DAD para análise de pesticidas em abelhas (Apis mellifera)
| Ano de defesa: | 2023 |
|---|---|
| Autor(a) principal: | |
| Orientador(a): | |
| Banca de defesa: | |
| Tipo de documento: | Dissertação |
| Tipo de acesso: | Acesso aberto |
| Idioma: | por |
| Instituição de defesa: |
Universidade Federal do Pampa
|
| Programa de Pós-Graduação: |
Mestrado Acadêmico em Bioquímica
|
| Departamento: |
Campus Uruguaiana
|
| País: |
Brasil
|
| Palavras-chave em Português: | |
| Área do conhecimento CNPq: | |
| Link de acesso: | https://repositorio.unipampa.edu.br/handle/123456789/11295 |
Resumo: | Apis mellifera, known as the honey bee, is a species of bee native to Europe and distributed worldwide. These bees play a crucial role as pollinators, collecting nectar and pollen from flowers for their food, which is essential for the pollination of many crops. During the collection of resources, such as water and food, bees travel large areas daily, exposing themselves to adverse factors, such as pesticides, which represent risks both for individuals and for the hives. The inappropriate use of pesticides in agriculture can result in the drift of these compounds to unwanted areas, affecting non-target organisms and causing toxicity. Due to the possibility of exposure of bees to low concentrations of contaminants, reliable and sensitive analytical methods are essential. In this sense, the objective of this study was to develop and validate sample preparation and quantification methodologies for the analysis of pesticides and their metabolites in honey bees (Apis mellifera). The selected pesticides were Imazethapyr, Propanil, Sulfentrazone, Chlorpyrifos and 2,4-D and the metabolites 2,4-DCP and 3,4-DCA. The QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method was used to extract pesticides from bee samples. For the separation, identification and quantification of compounds, High Performance Liquid Chromatography (HPLC) coupled to a Diode Array Detector (DAD) was used. The chromatographic method developed was validated through parameters such as linearity, intermediate precision, repeatability, limit of detection, limit of quantification, matrix effect and recovery (for extraction tests), according to the recommendations of Brazilian regulatory agencies and demonstrated high sensitivity in the detection of compounds in low concentrations. The QuEChERS method used in the extraction of bee samples proved to be efficient, allowing the recovery of sulfentrazone, 2,4-DCP, 3,4-DCA and propanyl in the range of 0.5-6 mg/L, and the pesticides imazethapyr, 2,4-D and chlorpyrifos in the range of 2-6 mg/L. In addition, this method is fast, easy and economical, allowing its wide application. The results obtained demonstrate the sensitivity and efficiency of these methods, which are essential for assessing the risks of contamination and health of bees. |
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Roehrs, Rafaelhttp://lattes.cnpq.br/2145471376587567http://lattes.cnpq.br/2015343647810677Paz, Maria Elizabeth Gomes2026-09-22T17:54:55Z20262023PAZ, Maria Elizabeth Gomes. Desenvolvimento e validação de método multirresíduo por QuEChERS e HPLC-DAD para análise de pesticidas em abelhas (Apis mellifera). 2023. 76 p. Dissertação (Mestrado em Bioquímica) – Universidade Federal do Pampa, Uruguaiana, 2023.https://repositorio.unipampa.edu.br/handle/123456789/11295Apis mellifera, known as the honey bee, is a species of bee native to Europe and distributed worldwide. These bees play a crucial role as pollinators, collecting nectar and pollen from flowers for their food, which is essential for the pollination of many crops. During the collection of resources, such as water and food, bees travel large areas daily, exposing themselves to adverse factors, such as pesticides, which represent risks both for individuals and for the hives. The inappropriate use of pesticides in agriculture can result in the drift of these compounds to unwanted areas, affecting non-target organisms and causing toxicity. Due to the possibility of exposure of bees to low concentrations of contaminants, reliable and sensitive analytical methods are essential. In this sense, the objective of this study was to develop and validate sample preparation and quantification methodologies for the analysis of pesticides and their metabolites in honey bees (Apis mellifera). The selected pesticides were Imazethapyr, Propanil, Sulfentrazone, Chlorpyrifos and 2,4-D and the metabolites 2,4-DCP and 3,4-DCA. The QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method was used to extract pesticides from bee samples. For the separation, identification and quantification of compounds, High Performance Liquid Chromatography (HPLC) coupled to a Diode Array Detector (DAD) was used. The chromatographic method developed was validated through parameters such as linearity, intermediate precision, repeatability, limit of detection, limit of quantification, matrix effect and recovery (for extraction tests), according to the recommendations of Brazilian regulatory agencies and demonstrated high sensitivity in the detection of compounds in low concentrations. The QuEChERS method used in the extraction of bee samples proved to be efficient, allowing the recovery of sulfentrazone, 2,4-DCP, 3,4-DCA and propanyl in the range of 0.5-6 mg/L, and the pesticides imazethapyr, 2,4-D and chlorpyrifos in the range of 2-6 mg/L. In addition, this method is fast, easy and economical, allowing its wide application. The results obtained demonstrate the sensitivity and efficiency of these methods, which are essential for assessing the risks of contamination and health of bees.A Apis mellifera, conhecida como abelha do mel, é uma espécie de abelha nativa da Europa e distribuída mundialmente. Essas abelhas desempenham um papel crucial como polinizadoras, coletando néctar e pólen de flores para sua alimentação, o que é essencial para a polinização de várias culturas. Durante a coleta de recursos, como água e alimento, as abelhas percorrem extensas áreas diariamente, expondo-se a fatores adversos, como pesticidas, que representam riscos tanto para os indivíduos quanto para as colmeias. A utilização inadequada de pesticidas na agricultura pode resultar na deriva desses compostos para áreas não desejadas, afetando organismos não alvo e causando toxicidade. Devido à possibilidade de exposição das abelhas a baixas concentrações de contaminantes, métodos analíticos confiáveis e sensíveis são essenciais. Nesse sentido, o objetivo deste estudo foi desenvolver e validar metodologia de preparo de amostra e quantificação para a análise de pesticidas e seus metabólitos em abelhas do mel (Apis mellifera). Os pesticidas selecionados foram Imazetapir, Propanil, Sulfentrazone, Clorpirifós e 2,4-D e os metabólitos 2,4-DCP e 3,4-DCA. O método QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe), foi utilizado para a extração dos pesticidas das amostras de abelhas. Para a separação, identificação e quantificação dos compostos, utilizou-se a Cromatografia Líquida de Alta Eficiência (CLAE) acoplada ao Detector de Arranjo de Diodos (DAD). O método cromatográfico desenvolvido foi validado através de parâmetros como linearidade, precisão intermediária, repetibilidade, limite de detecção, limite de quantificação, efeito da matriz e recuperação (para os testes de extração), de acordo com as recomendações das agências regulatórias brasileiras e demonstrou alta sensibilidade na detecção dos compostos em baixas concentrações. O método QuEChERS utilizado na extração das amostras de abelhas mostrou-se eficiente, permitindo a recuperação dos compostos sulfentrazone, 2,4-DCP, 3,4-DCA e propanil na faixa de 0,5-6 mg/L, e dos pesticidas imazetapir, 2,4-D e clorpirifós na faixa de 2-6 mg/L Além disso, esse método é rápido, fácil e econômico, possibilitando sua ampla aplicação. Os resultados obtidos demonstraram a sensibilidade e eficiência desses métodos, que são essenciais para a avaliação dos riscos de contaminação e saúde das abelhas.porUniversidade Federal do PampaMestrado Acadêmico em BioquímicaUNIPAMPABrasilCampus UruguaianaCIENCIAS DA SAUDEBiomonitoramentoCLAE-DADBiomonitoringContaminantsPesticidesExtração; PesticidasContaminantesHPLC-DADExtractionDesenvolvimento e validação de método multirresíduo por QuEChERS e HPLC-DAD para análise de pesticidas em abelhas (Apis mellifera)Development and validation of a multiresidue method by QuEChERS and HPLC-DAD for the analysis of pesticides in bees (Apis mellifera)info:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisinfo:eu-repo/semantics/openAccessreponame:Repositório Institucional da UNIPAMPAinstname:Universidade Federal do Pampa (UNIPAMPA)instacron:UNIPAMPAORIGINALMaria Elizabeth Gomes Paz ate DEZ 2024.pdfMaria Elizabeth Gomes Paz ate DEZ 2024.pdfapplication/pdf1092049https://repositorio.unipampa.edu.br/bitstreams/3ac3ef7e-f46d-4bab-87a9-45a43729bf2c/download1251782b8e4a3c3046dfe3a4a99e69f0MD51trueAnonymousREADLICENSElicense.txtWritten by org.dspace.content.LicenseUtilstext/plain; charset=utf-81670https://repositorio.unipampa.edu.br/bitstreams/5d6c4061-eb73-46be-94d9-e8aa39a9964d/download0d1676a7f543432696ddf2f1676dffe0MD52falseAnonymousREAD123456789/112952026-09-22 14:54:55.738open.accessoai:repositorio.unipampa.edu.br:123456789/11295https://repositorio.unipampa.edu.brRepositório InstitucionalPUBhttp://dspace.unipampa.edu.br:8080/oai/requestsisbi@unipampa.edu.bropendoar:2026-09-22T17:54:55Repositório Institucional da UNIPAMPA - Universidade Federal do Pampa (UNIPAMPA)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 |
| dc.title.none.fl_str_mv |
Desenvolvimento e validação de método multirresíduo por QuEChERS e HPLC-DAD para análise de pesticidas em abelhas (Apis mellifera) |
| dc.title.alternative.none.fl_str_mv |
Development and validation of a multiresidue method by QuEChERS and HPLC-DAD for the analysis of pesticides in bees (Apis mellifera) |
| title |
Desenvolvimento e validação de método multirresíduo por QuEChERS e HPLC-DAD para análise de pesticidas em abelhas (Apis mellifera) |
| spellingShingle |
Desenvolvimento e validação de método multirresíduo por QuEChERS e HPLC-DAD para análise de pesticidas em abelhas (Apis mellifera) Paz, Maria Elizabeth Gomes CIENCIAS DA SAUDE Biomonitoramento CLAE-DAD Biomonitoring Contaminants Pesticides Extração; Pesticidas Contaminantes HPLC-DAD Extraction |
| title_short |
Desenvolvimento e validação de método multirresíduo por QuEChERS e HPLC-DAD para análise de pesticidas em abelhas (Apis mellifera) |
| title_full |
Desenvolvimento e validação de método multirresíduo por QuEChERS e HPLC-DAD para análise de pesticidas em abelhas (Apis mellifera) |
| title_fullStr |
Desenvolvimento e validação de método multirresíduo por QuEChERS e HPLC-DAD para análise de pesticidas em abelhas (Apis mellifera) |
| title_full_unstemmed |
Desenvolvimento e validação de método multirresíduo por QuEChERS e HPLC-DAD para análise de pesticidas em abelhas (Apis mellifera) |
| title_sort |
Desenvolvimento e validação de método multirresíduo por QuEChERS e HPLC-DAD para análise de pesticidas em abelhas (Apis mellifera) |
| author |
Paz, Maria Elizabeth Gomes |
| author_facet |
Paz, Maria Elizabeth Gomes |
| author_role |
author |
| dc.contributor.advisor1.fl_str_mv |
Roehrs, Rafael |
| dc.contributor.advisor1Lattes.fl_str_mv |
http://lattes.cnpq.br/2145471376587567 |
| dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/2015343647810677 |
| dc.contributor.author.fl_str_mv |
Paz, Maria Elizabeth Gomes |
| contributor_str_mv |
Roehrs, Rafael |
| dc.subject.cnpq.fl_str_mv |
CIENCIAS DA SAUDE |
| topic |
CIENCIAS DA SAUDE Biomonitoramento CLAE-DAD Biomonitoring Contaminants Pesticides Extração; Pesticidas Contaminantes HPLC-DAD Extraction |
| dc.subject.por.fl_str_mv |
Biomonitoramento CLAE-DAD Biomonitoring Contaminants Pesticides Extração; Pesticidas Contaminantes HPLC-DAD Extraction |
| description |
Apis mellifera, known as the honey bee, is a species of bee native to Europe and distributed worldwide. These bees play a crucial role as pollinators, collecting nectar and pollen from flowers for their food, which is essential for the pollination of many crops. During the collection of resources, such as water and food, bees travel large areas daily, exposing themselves to adverse factors, such as pesticides, which represent risks both for individuals and for the hives. The inappropriate use of pesticides in agriculture can result in the drift of these compounds to unwanted areas, affecting non-target organisms and causing toxicity. Due to the possibility of exposure of bees to low concentrations of contaminants, reliable and sensitive analytical methods are essential. In this sense, the objective of this study was to develop and validate sample preparation and quantification methodologies for the analysis of pesticides and their metabolites in honey bees (Apis mellifera). The selected pesticides were Imazethapyr, Propanil, Sulfentrazone, Chlorpyrifos and 2,4-D and the metabolites 2,4-DCP and 3,4-DCA. The QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method was used to extract pesticides from bee samples. For the separation, identification and quantification of compounds, High Performance Liquid Chromatography (HPLC) coupled to a Diode Array Detector (DAD) was used. The chromatographic method developed was validated through parameters such as linearity, intermediate precision, repeatability, limit of detection, limit of quantification, matrix effect and recovery (for extraction tests), according to the recommendations of Brazilian regulatory agencies and demonstrated high sensitivity in the detection of compounds in low concentrations. The QuEChERS method used in the extraction of bee samples proved to be efficient, allowing the recovery of sulfentrazone, 2,4-DCP, 3,4-DCA and propanyl in the range of 0.5-6 mg/L, and the pesticides imazethapyr, 2,4-D and chlorpyrifos in the range of 2-6 mg/L. In addition, this method is fast, easy and economical, allowing its wide application. The results obtained demonstrate the sensitivity and efficiency of these methods, which are essential for assessing the risks of contamination and health of bees. |
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2023 |
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2023 |
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2026-09-22T17:54:55Z |
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2026 |
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info:eu-repo/semantics/publishedVersion |
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info:eu-repo/semantics/masterThesis |
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PAZ, Maria Elizabeth Gomes. Desenvolvimento e validação de método multirresíduo por QuEChERS e HPLC-DAD para análise de pesticidas em abelhas (Apis mellifera). 2023. 76 p. Dissertação (Mestrado em Bioquímica) – Universidade Federal do Pampa, Uruguaiana, 2023. |
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https://repositorio.unipampa.edu.br/handle/123456789/11295 |
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PAZ, Maria Elizabeth Gomes. Desenvolvimento e validação de método multirresíduo por QuEChERS e HPLC-DAD para análise de pesticidas em abelhas (Apis mellifera). 2023. 76 p. Dissertação (Mestrado em Bioquímica) – Universidade Federal do Pampa, Uruguaiana, 2023. |
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Universidade Federal do Pampa |
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Mestrado Acadêmico em Bioquímica |
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UNIPAMPA |
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Brasil |
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Campus Uruguaiana |
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Universidade Federal do Pampa |
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