Desenvolvimento e validação de método para determinação multiresíduo de agrotóxicos em urina empregando método QuEChERS e LC-MS/MS
Ano de defesa: | 2022 |
---|---|
Autor(a) principal: | |
Orientador(a): | |
Banca de defesa: | , , , |
Tipo de documento: | Tese |
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/1/27607 |
Resumo: | Pesticides have been widely used in food crops to control pests, weeds, fungi, etc. The indiscriminate use of these organic compounds has contributed to the increase in cases of intoxication in humans, which can lead to more serious health problems, becoming a case of public health. Biological samples, such as urine, are more common and easy to collect, in addition to providing recent information on exposure to pesticides. In this sense, the use of methods that are capable of determining different classes and the largest number of compounds in a single procedure are of paramount importance to guarantee a more comprehensive result. Within this perspective, this work developed and validated a method for multiresidue determination of pesticides in urine using the unbuffered QuEChERS method and analysis by liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS). The parameters that influence the extraction efficiency were studied and after finding the best extraction conditions, the method was validated. The proposed procedure consisted of extracting 10 mL of urine (pH 5) with 2 mL of acetonitrile and the saltiong-out effect was achieved by adding 4 g of MgSO4 and 1 g of NaCl. Afterwards, a clean-up step was carried out using dispersive solid phase extraction, an aliquot the supernatant was transferred to a tube containing 150 mg of MgSO4, 25 mg of PSA and 25 mg of C18. Subsequently, the extract was diluted (1:4, v/v) in water, filtered (PTFE 0.22 µm) and injected into the chromatographic system. The unbuffered QuEChERS method was validated for 193 pesticides from different classes, proving to be selective and robust. Linearity was evaluated using matrix-fortified calibration from 0.5 to 20 µg L-¹ and showed r² > 0.99 for all evaluated compounds. LOQ ranged from 0.5 to 5 µg L-¹ (0.5 µg L-¹ for 177 compounds) and the LOD from 0.15 to 1.5 µg L-¹ with adequate accuracy (70 to 120%) and precision (RSD ≤20%). In the analysis of 50 urine samples collected from agricultural workers, residues of three neonicotinoids pesticides were detected with concentrations ranging from <LOQ to 4.43 µg L-¹ . Considering the results obtained, the use of the unbuffered QuEChERS method combined with LC-MS/MS detection allowed the determination of a wide range of analytes with high selectivity and sensitivity, proving to be efficient for multiresidue determination of pesticides in urine. |
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2023-01-17T12:42:08Z2023-01-17T12:42:08Z2022-09-16http://repositorio.ufsm.br/handle/1/27607Pesticides have been widely used in food crops to control pests, weeds, fungi, etc. The indiscriminate use of these organic compounds has contributed to the increase in cases of intoxication in humans, which can lead to more serious health problems, becoming a case of public health. Biological samples, such as urine, are more common and easy to collect, in addition to providing recent information on exposure to pesticides. In this sense, the use of methods that are capable of determining different classes and the largest number of compounds in a single procedure are of paramount importance to guarantee a more comprehensive result. Within this perspective, this work developed and validated a method for multiresidue determination of pesticides in urine using the unbuffered QuEChERS method and analysis by liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS). The parameters that influence the extraction efficiency were studied and after finding the best extraction conditions, the method was validated. The proposed procedure consisted of extracting 10 mL of urine (pH 5) with 2 mL of acetonitrile and the saltiong-out effect was achieved by adding 4 g of MgSO4 and 1 g of NaCl. Afterwards, a clean-up step was carried out using dispersive solid phase extraction, an aliquot the supernatant was transferred to a tube containing 150 mg of MgSO4, 25 mg of PSA and 25 mg of C18. Subsequently, the extract was diluted (1:4, v/v) in water, filtered (PTFE 0.22 µm) and injected into the chromatographic system. The unbuffered QuEChERS method was validated for 193 pesticides from different classes, proving to be selective and robust. Linearity was evaluated using matrix-fortified calibration from 0.5 to 20 µg L-¹ and showed r² > 0.99 for all evaluated compounds. LOQ ranged from 0.5 to 5 µg L-¹ (0.5 µg L-¹ for 177 compounds) and the LOD from 0.15 to 1.5 µg L-¹ with adequate accuracy (70 to 120%) and precision (RSD ≤20%). In the analysis of 50 urine samples collected from agricultural workers, residues of three neonicotinoids pesticides were detected with concentrations ranging from <LOQ to 4.43 µg L-¹ . Considering the results obtained, the use of the unbuffered QuEChERS method combined with LC-MS/MS detection allowed the determination of a wide range of analytes with high selectivity and sensitivity, proving to be efficient for multiresidue determination of pesticides in urine.O uso de agrotóxicos tem sido amplamente empregados no cultivo de alimentos para o controle de pragas, ervas dadinhas, fungos, etc. O uso indiscriminado destes compostos orgânicos tem contribuído para o aumento de casos de intoxicação em humanos podendo levar a problemas de saúde mais graves, se tornando caso de saúde pública. Amostras biológicas, como urina, são mais usuais e de fácil coleta, além de fornecer informações recentes à exposição aos agrotóxicos. Nesse sentido, o emprego de métodos que sejam capazes de determinar diferentes classes e mais quantidades de compostos em um único procedimento são de suma importância para garantir um resultado mais abrangente. Com base nisso, neste estudo desenvolveuse e validou-se um método para determinação multiresíduo de agrotóxicos em urina empregando o método QuEChERS original modificado e análise por cromatografia líquida acoplada à espectrometria de massas em série (LC-MS/MS, do inglês liquid chromatography coupled to tandem mass spectrometry). Os parâmetros que influenciam na eficiência de extração foram estudados e após encontrar-se as melhores condições de extração, o método foi validado. O procedimento proposto consistiu na extração de 10 mL de urina (pH 5) com 2 mL de acetonitrila e a etapa de partição foi realizada com 4 g de MgSO4 e 1 g de NaCl. Após, realizou-se uma etapa de limpeza do extrato empregando extração em fase sólida dispersiva, em que 1 mL do sobrenadante foi misturado com 150 mg de MgSO4, 25 mg de PSA e 25 mg de C18. Posteriormente o extrato foi diluído (1:4, v/v) em água, filtrado (PTFE 0,22 um) e injetado no sistema LC-MS/MS. O método QuEChERS original modificado foi validado para 193 compostos, realizado através de curva de trabalho extraída na matriz branco, demonstrando ser um método seletivo e robusto. Todos os compostos apresentaram linearidade nas faixas de trabalho avaliada de 0,5 a 20 µg L-¹ com coeficientes de determinação superiores a 0,99. As recuperações obtidas variaram de 70 a 120% com desvio padrão relativo ≤ 20%, sendo que o limite de quantificação do método (LOQ) variou de 0,5 a 5 µg L-¹ , (0,5 µg L-¹ para 177 compostos) e o LOD variou de 0,15 a 1,5 µg L-¹ . Foram analisadas 50 amostras de urina doadas de agricultores e três inseticidas neonicotinóides foram detectados com concentrações variando de <LOQ a 4,43 µg L-¹ . Considerando os resultados obtidos, a utilização do método QuEChERS original modificado juntamente com o uso de LC-MS/MS permitiu a determinação dos analitos com alta seletividade e sensibilidade, demonstrando ser eficiente para determinação multirresíduo de agrotóxicos em urina.Coordenação de Aperfeiçoamento de Pessoal de Nível Superior - CAPESporUniversidade 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/openAccessAgrotóxicosMulticlasseUrinaQuEChERSLC-MS/MSPesticidesMulticlassUrineCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICADesenvolvimento e validação de método para determinação multiresíduo de agrotóxicos em urina empregando método QuEChERS e LC-MS/MSDevelopment and validation of a method for multiresidue determination of pesticides in urine using QuEChERS method and LC-MS/MSinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/doctoralThesisPrestes, Osmar Damianhttp://lattes.cnpq.br/9632234955509028Zanella, RenatoMüller, Aline Lima HermesLoro, Vania LuciaFrancesquett, Janice ZulmaViera, Mariela de Souzahttp://lattes.cnpq.br/4207717961248387Demarco, Marisa100600000000600600600600600600600600f79cc0c9-c923-4244-9c1f-c80d74674410ab4279f7-c65d-41d7-8427-afa08cc9cfc0afca1482-db26-48dd-b760-a9d0165dc5793a5b86e4-a4fc-4124-b40b-b860a9eed50b301a3550-6b95-45aa-be7f-19ffad13abc4b037a137-b45b-4319-91b8-847c1c875be39697695f-a869-4500-a917-8937d2067f6areponame:Biblioteca Digital de Teses e Dissertações do UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMORIGINALTES_PPGQUÍMICA_2022_DEMARCO_MARISA.pdfTES_PPGQUÍMICA_2022_DEMARCO_MARISA.pdfTese de Doutoradoapplication/pdf2850206http://repositorio.ufsm.br/bitstream/1/27607/1/TES_PPGQU%c3%8dMICA_2022_DEMARCO_MARISA.pdfa16b3890cd44f81072558d22ebe05556MD51CC-LICENSElicense_rdflicense_rdfapplication/rdf+xml; charset=utf-8805http://repositorio.ufsm.br/bitstream/1/27607/2/license_rdf4460e5956bc1d1639be9ae6146a50347MD52LICENSElicense.txtlicense.txttext/plain; charset=utf-81956http://repositorio.ufsm.br/bitstream/1/27607/3/license.txt2f0571ecee68693bd5cd3f17c1e075dfMD531/276072023-01-17 09:42:08.993oai:repositorio.ufsm.br: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 Digital de Teses e Dissertaçõeshttps://repositorio.ufsm.br/ONGhttps://repositorio.ufsm.br/oai/requestatendimento.sib@ufsm.br||tedebc@gmail.comopendoar:2023-01-17T12:42:08Biblioteca Digital de Teses e Dissertações do UFSM - Universidade Federal de Santa Maria (UFSM)false |
dc.title.por.fl_str_mv |
Desenvolvimento e validação de método para determinação multiresíduo de agrotóxicos em urina empregando método QuEChERS e LC-MS/MS |
dc.title.alternative.eng.fl_str_mv |
Development and validation of a method for multiresidue determination of pesticides in urine using QuEChERS method and LC-MS/MS |
title |
Desenvolvimento e validação de método para determinação multiresíduo de agrotóxicos em urina empregando método QuEChERS e LC-MS/MS |
spellingShingle |
Desenvolvimento e validação de método para determinação multiresíduo de agrotóxicos em urina empregando método QuEChERS e LC-MS/MS Demarco, Marisa Agrotóxicos Multiclasse Urina QuEChERS LC-MS/MS Pesticides Multiclass Urine CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Desenvolvimento e validação de método para determinação multiresíduo de agrotóxicos em urina empregando método QuEChERS e LC-MS/MS |
title_full |
Desenvolvimento e validação de método para determinação multiresíduo de agrotóxicos em urina empregando método QuEChERS e LC-MS/MS |
title_fullStr |
Desenvolvimento e validação de método para determinação multiresíduo de agrotóxicos em urina empregando método QuEChERS e LC-MS/MS |
title_full_unstemmed |
Desenvolvimento e validação de método para determinação multiresíduo de agrotóxicos em urina empregando método QuEChERS e LC-MS/MS |
title_sort |
Desenvolvimento e validação de método para determinação multiresíduo de agrotóxicos em urina empregando método QuEChERS e LC-MS/MS |
author |
Demarco, Marisa |
author_facet |
Demarco, Marisa |
author_role |
author |
dc.contributor.advisor1.fl_str_mv |
Prestes, Osmar Damian |
dc.contributor.advisor1Lattes.fl_str_mv |
http://lattes.cnpq.br/9632234955509028 |
dc.contributor.advisor-co1.fl_str_mv |
Zanella, Renato |
dc.contributor.referee1.fl_str_mv |
Müller, Aline Lima Hermes |
dc.contributor.referee2.fl_str_mv |
Loro, Vania Lucia |
dc.contributor.referee3.fl_str_mv |
Francesquett, Janice Zulma |
dc.contributor.referee4.fl_str_mv |
Viera, Mariela de Souza |
dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/4207717961248387 |
dc.contributor.author.fl_str_mv |
Demarco, Marisa |
contributor_str_mv |
Prestes, Osmar Damian Zanella, Renato Müller, Aline Lima Hermes Loro, Vania Lucia Francesquett, Janice Zulma Viera, Mariela de Souza |
dc.subject.por.fl_str_mv |
Agrotóxicos Multiclasse Urina QuEChERS LC-MS/MS |
topic |
Agrotóxicos Multiclasse Urina QuEChERS LC-MS/MS Pesticides Multiclass Urine CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.eng.fl_str_mv |
Pesticides Multiclass Urine |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
Pesticides have been widely used in food crops to control pests, weeds, fungi, etc. The indiscriminate use of these organic compounds has contributed to the increase in cases of intoxication in humans, which can lead to more serious health problems, becoming a case of public health. Biological samples, such as urine, are more common and easy to collect, in addition to providing recent information on exposure to pesticides. In this sense, the use of methods that are capable of determining different classes and the largest number of compounds in a single procedure are of paramount importance to guarantee a more comprehensive result. Within this perspective, this work developed and validated a method for multiresidue determination of pesticides in urine using the unbuffered QuEChERS method and analysis by liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS). The parameters that influence the extraction efficiency were studied and after finding the best extraction conditions, the method was validated. The proposed procedure consisted of extracting 10 mL of urine (pH 5) with 2 mL of acetonitrile and the saltiong-out effect was achieved by adding 4 g of MgSO4 and 1 g of NaCl. Afterwards, a clean-up step was carried out using dispersive solid phase extraction, an aliquot the supernatant was transferred to a tube containing 150 mg of MgSO4, 25 mg of PSA and 25 mg of C18. Subsequently, the extract was diluted (1:4, v/v) in water, filtered (PTFE 0.22 µm) and injected into the chromatographic system. The unbuffered QuEChERS method was validated for 193 pesticides from different classes, proving to be selective and robust. Linearity was evaluated using matrix-fortified calibration from 0.5 to 20 µg L-¹ and showed r² > 0.99 for all evaluated compounds. LOQ ranged from 0.5 to 5 µg L-¹ (0.5 µg L-¹ for 177 compounds) and the LOD from 0.15 to 1.5 µg L-¹ with adequate accuracy (70 to 120%) and precision (RSD ≤20%). In the analysis of 50 urine samples collected from agricultural workers, residues of three neonicotinoids pesticides were detected with concentrations ranging from <LOQ to 4.43 µg L-¹ . Considering the results obtained, the use of the unbuffered QuEChERS method combined with LC-MS/MS detection allowed the determination of a wide range of analytes with high selectivity and sensitivity, proving to be efficient for multiresidue determination of pesticides in urine. |
publishDate |
2022 |
dc.date.issued.fl_str_mv |
2022-09-16 |
dc.date.accessioned.fl_str_mv |
2023-01-17T12:42:08Z |
dc.date.available.fl_str_mv |
2023-01-17T12:42:08Z |
dc.type.status.fl_str_mv |
info:eu-repo/semantics/publishedVersion |
dc.type.driver.fl_str_mv |
info:eu-repo/semantics/doctoralThesis |
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doctoralThesis |
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publishedVersion |
dc.identifier.uri.fl_str_mv |
http://repositorio.ufsm.br/handle/1/27607 |
url |
http://repositorio.ufsm.br/handle/1/27607 |
dc.language.iso.fl_str_mv |
por |
language |
por |
dc.relation.cnpq.fl_str_mv |
100600000000 |
dc.relation.confidence.fl_str_mv |
600 600 600 600 600 600 600 600 |
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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 |
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