Desenvolvimento de método para determinação de resíduos de antiparasitários em leite bovino empregando LLE-LTP E LC-MS/MS

Detalhes bibliográficos
Ano de defesa: 2016
Autor(a) principal: Ribeiro, Lucila Cendon lattes
Orientador(a): Zanella, Renato lattes
Banca de defesa: Richards, Neila Silvia Pereira dos Santos lattes, Peixoto, Sandra Cadore lattes
Tipo de documento: Dissertação
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:
Leite bovino
Antiparasitários
LLE-LTP
LC-MS/MS
Palavras-chave em Inglês:
Bovine milk
Antiparasitic
Área do conhecimento CNPq:
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA
Link de acesso: http://repositorio.ufsm.br/handle/1/11957
Resumo: Milk is one of the most consumed fresh food, considered a nutritionally complete product. Veterinary drugs are used in order to increase productivity. However, improper use of these products may result in the presence of residues in milk. This study aims to develop a method for determination of antiparasitic residues in bovine milk using fast liquid-liquid low temperature partitioning (LLE-LTP) method and liquid chromatographic coupled to tandem mass spectrometry (LC-MS/MS). Different classes were studied for antiparasitic, such as macrocyclic lactones, pyrethroids, benzimidazoles, organophosphates, carbamates, among others. The spikes were held comprising the Maximum Residue Limits (MRLs) of each compound at levels 1- 200 ug L-1. For validation step was adopted the following parameters: selectivity, linear range, matrix effect, limits of detection (LOD) and quantitation (LOQ), decision limit (CCα) and detection capability (CCβ), precision, accuracy. The method was considered valid to 55 antiparasitic and presented LOD from 0.03 to 6.0 μg L-1 and LOQ from 1 to 20 ug L-1. Recoveries were between 70 and 120% with RSD ≤ 20%, that were considered acceptable. The proposed method was applied to 15 real samples where all samples presented residues of at least one antiparasitic. Of these, two samples contained cyhalothrin and nicarbazin residues above the MRL. However, the method was efficient in determining antiparasitic residues in bovine milk using LLE-LTP and LCMS/ MS, showing good sensitivity and selectivity.
id UFSM_ee9fc3e8c1fb279591bff30326ca74b4
oai_identifier_str oai:repositorio.ufsm.br:1/11957
network_acronym_str UFSM
network_name_str Biblioteca Digital de Teses e Dissertações do UFSM
repository_id_str
spelling 2017-11-01T14:55:45Z2017-11-01T14:55:45Z2016-08-26http://repositorio.ufsm.br/handle/1/11957Milk is one of the most consumed fresh food, considered a nutritionally complete product. Veterinary drugs are used in order to increase productivity. However, improper use of these products may result in the presence of residues in milk. This study aims to develop a method for determination of antiparasitic residues in bovine milk using fast liquid-liquid low temperature partitioning (LLE-LTP) method and liquid chromatographic coupled to tandem mass spectrometry (LC-MS/MS). Different classes were studied for antiparasitic, such as macrocyclic lactones, pyrethroids, benzimidazoles, organophosphates, carbamates, among others. The spikes were held comprising the Maximum Residue Limits (MRLs) of each compound at levels 1- 200 ug L-1. For validation step was adopted the following parameters: selectivity, linear range, matrix effect, limits of detection (LOD) and quantitation (LOQ), decision limit (CCα) and detection capability (CCβ), precision, accuracy. The method was considered valid to 55 antiparasitic and presented LOD from 0.03 to 6.0 μg L-1 and LOQ from 1 to 20 ug L-1. Recoveries were between 70 and 120% with RSD ≤ 20%, that were considered acceptable. The proposed method was applied to 15 real samples where all samples presented residues of at least one antiparasitic. Of these, two samples contained cyhalothrin and nicarbazin residues above the MRL. However, the method was efficient in determining antiparasitic residues in bovine milk using LLE-LTP and LCMS/ MS, showing good sensitivity and selectivity.O leite é um dos alimentos in natura mais consumidos, por ser considerado um produto completo nutricionalmente. A fim de tratar e assegurar a sanidade do rebanho, faz-se uso de medicamentos veterinários. No entanto, a utilização inadequada destes produtos pode acarretar na presença de resíduos destes no leite. Este estudo tem como objetivo desenvolver um método para determinação de resíduos de antiparasitários em leite bovino, empregando método extração líquido-líquido com rápida partição a baixa temperatura (LLELTP) e cromatografia líquida acoplada à espectrometria de massas em série (LC–MS/MS). Avaliou-se diferentes classes de antiparasitários, como lactonas macrocíclicas, piretróides, benzimidazóis, organofosforados, carbamatos, entre outros. As fortificações foram realizadas abrangendo os Limites Máximos de Resíduos (LMRs) de cada composto, em níveis de 1 a 200 μg L-1. Para a etapa de validação do método avaliou-se os seguintes parâmetros: seletividade, faixa linear, efeito matriz, limites de detecção (LOD) e quantificação (LOQ), limite de decisão (CCα), capacidade de detecção (CCβ), precisão e exatidão. O método foi considerado validado para 55 antiparasitários e apresentou valores de LOD de 0,03 a 6,0 μg L-1 e de LOQ de 1 a 20 μg L-1. As recuperações ficaram entre 70 e 120%, e RSD ≤ 20%, sendo considerados aceitáveis. O método proposto foi aplicado em 14 amostras reais, onde todas apresentaram resíduos de pelo menos um antiparasitário. Destas, duas amostras continham resíduos de cialotrina e nicarbazin acima do LMR. O método mostrou-se eficiente na determinação de resíduos de antiparasitários em leite bovino empregando LLELTP e LC–MS/MS, demonstrando boa sensibilidade e seletividade.porUniversidade 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/openAccessLeite bovinoAntiparasitáriosLLE-LTPLC-MS/MSBovine milkAntiparasiticCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICADesenvolvimento de método para determinação de resíduos de antiparasitários em leite bovino empregando LLE-LTP E LC-MS/MSMethod development for determination of antiparasitic residue in employing of cattle milk LLE-LTP AND LC-MS / MSinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisZanella, Renatohttp://lattes.cnpq.br/0618653776990780Richards, Neila Silvia Pereira dos Santoshttp://lattes.cnpq.br/0618653776990780Peixoto, Sandra Cadorehttp://lattes.cnpq.br/0051729840313401http://lattes.cnpq.br/6569237867743027Ribeiro, Lucila Cendon1006000000006000aa2baab-94e8-4d3d-bbb2-85495ba77db5f874da2d-28fc-4ca8-9045-f4902d3c8ff101bafd56-2288-4c6f-8124-5c76db119beea756e725-e092-4a00-a474-12d73191eb38reponame:Biblioteca Digital de Teses e Dissertações do UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMORIGINALTES_PPGQUÍMICA_2016_VARGAS_JOSIMAR.pdfTES_PPGQUÍMICA_2016_VARGAS_JOSIMAR.pdfDissertação de Mestradoapplication/pdf8204719http://repositorio.ufsm.br/bitstream/1/11957/1/TES_PPGQU%c3%8dMICA_2016_VARGAS_JOSIMAR.pdf7eba519c0ed2ae98cde3b803d758c625MD51CC-LICENSElicense_rdflicense_rdfapplication/rdf+xml; charset=utf-8804http://repositorio.ufsm.br/bitstream/1/11957/2/license_rdfc1efe8e24d7281448e873be30ea326ffMD52LICENSElicense.txtlicense.txttext/plain; charset=utf-81956http://repositorio.ufsm.br/bitstream/1/11957/3/license.txt2f0571ecee68693bd5cd3f17c1e075dfMD53TEXTTES_PPGQUÍMICA_2016_VARGAS_JOSIMAR.pdf.txtTES_PPGQUÍMICA_2016_VARGAS_JOSIMAR.pdf.txtExtracted texttext/plain130362http://repositorio.ufsm.br/bitstream/1/11957/4/TES_PPGQU%c3%8dMICA_2016_VARGAS_JOSIMAR.pdf.txtd9a008bce20e198e60655d77c8020dddMD54THUMBNAILTES_PPGQUÍMICA_2016_VARGAS_JOSIMAR.pdf.jpgTES_PPGQUÍMICA_2016_VARGAS_JOSIMAR.pdf.jpgIM Thumbnailimage/jpeg4702http://repositorio.ufsm.br/bitstream/1/11957/5/TES_PPGQU%c3%8dMICA_2016_VARGAS_JOSIMAR.pdf.jpgb55234464c1e298da0fa2f931c88805fMD551/119572022-06-23 08:21:36.122oai: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:2022-06-23T11:21:36Biblioteca Digital de Teses e Dissertações do UFSM - Universidade Federal de Santa Maria (UFSM)false
dc.title.por.fl_str_mv Desenvolvimento de método para determinação de resíduos de antiparasitários em leite bovino empregando LLE-LTP E LC-MS/MS
dc.title.alternative.eng.fl_str_mv Method development for determination of antiparasitic residue in employing of cattle milk LLE-LTP AND LC-MS / MS
title Desenvolvimento de método para determinação de resíduos de antiparasitários em leite bovino empregando LLE-LTP E LC-MS/MS
spellingShingle Desenvolvimento de método para determinação de resíduos de antiparasitários em leite bovino empregando LLE-LTP E LC-MS/MS
Ribeiro, Lucila Cendon
Leite bovino
Antiparasitários
LLE-LTP
LC-MS/MS
Bovine milk
Antiparasitic
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA
title_short Desenvolvimento de método para determinação de resíduos de antiparasitários em leite bovino empregando LLE-LTP E LC-MS/MS
title_full Desenvolvimento de método para determinação de resíduos de antiparasitários em leite bovino empregando LLE-LTP E LC-MS/MS
title_fullStr Desenvolvimento de método para determinação de resíduos de antiparasitários em leite bovino empregando LLE-LTP E LC-MS/MS
title_full_unstemmed Desenvolvimento de método para determinação de resíduos de antiparasitários em leite bovino empregando LLE-LTP E LC-MS/MS
title_sort Desenvolvimento de método para determinação de resíduos de antiparasitários em leite bovino empregando LLE-LTP E LC-MS/MS
author Ribeiro, Lucila Cendon
author_facet Ribeiro, Lucila Cendon
author_role author
dc.contributor.advisor1.fl_str_mv Zanella, Renato
dc.contributor.advisor1Lattes.fl_str_mv http://lattes.cnpq.br/0618653776990780
dc.contributor.referee1.fl_str_mv Richards, Neila Silvia Pereira dos Santos
dc.contributor.referee1Lattes.fl_str_mv http://lattes.cnpq.br/0618653776990780
dc.contributor.referee2.fl_str_mv Peixoto, Sandra Cadore
dc.contributor.referee2Lattes.fl_str_mv http://lattes.cnpq.br/0051729840313401
dc.contributor.authorLattes.fl_str_mv http://lattes.cnpq.br/6569237867743027
dc.contributor.author.fl_str_mv Ribeiro, Lucila Cendon
contributor_str_mv Zanella, Renato
Richards, Neila Silvia Pereira dos Santos
Peixoto, Sandra Cadore
dc.subject.por.fl_str_mv Leite bovino
Antiparasitários
LLE-LTP
LC-MS/MS
topic Leite bovino
Antiparasitários
LLE-LTP
LC-MS/MS
Bovine milk
Antiparasitic
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA
dc.subject.eng.fl_str_mv Bovine milk
Antiparasitic
dc.subject.cnpq.fl_str_mv CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA
description Milk is one of the most consumed fresh food, considered a nutritionally complete product. Veterinary drugs are used in order to increase productivity. However, improper use of these products may result in the presence of residues in milk. This study aims to develop a method for determination of antiparasitic residues in bovine milk using fast liquid-liquid low temperature partitioning (LLE-LTP) method and liquid chromatographic coupled to tandem mass spectrometry (LC-MS/MS). Different classes were studied for antiparasitic, such as macrocyclic lactones, pyrethroids, benzimidazoles, organophosphates, carbamates, among others. The spikes were held comprising the Maximum Residue Limits (MRLs) of each compound at levels 1- 200 ug L-1. For validation step was adopted the following parameters: selectivity, linear range, matrix effect, limits of detection (LOD) and quantitation (LOQ), decision limit (CCα) and detection capability (CCβ), precision, accuracy. The method was considered valid to 55 antiparasitic and presented LOD from 0.03 to 6.0 μg L-1 and LOQ from 1 to 20 ug L-1. Recoveries were between 70 and 120% with RSD ≤ 20%, that were considered acceptable. The proposed method was applied to 15 real samples where all samples presented residues of at least one antiparasitic. Of these, two samples contained cyhalothrin and nicarbazin residues above the MRL. However, the method was efficient in determining antiparasitic residues in bovine milk using LLE-LTP and LCMS/ MS, showing good sensitivity and selectivity.
publishDate 2016
dc.date.issued.fl_str_mv 2016-08-26
dc.date.accessioned.fl_str_mv 2017-11-01T14:55:45Z
dc.date.available.fl_str_mv 2017-11-01T14:55:45Z
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 http://repositorio.ufsm.br/handle/1/11957
url http://repositorio.ufsm.br/handle/1/11957
dc.language.iso.fl_str_mv por
language por
dc.relation.cnpq.fl_str_mv 100600000000
dc.relation.confidence.fl_str_mv 600
dc.relation.authority.fl_str_mv 0aa2baab-94e8-4d3d-bbb2-85495ba77db5
f874da2d-28fc-4ca8-9045-f4902d3c8ff1
01bafd56-2288-4c6f-8124-5c76db119bee
a756e725-e092-4a00-a474-12d73191eb38
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 reponame:Biblioteca Digital de Teses e Dissertações do 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 Biblioteca Digital de Teses e Dissertações do UFSM
collection Biblioteca Digital de Teses e Dissertações do UFSM
bitstream.url.fl_str_mv http://repositorio.ufsm.br/bitstream/1/11957/1/TES_PPGQU%c3%8dMICA_2016_VARGAS_JOSIMAR.pdf
http://repositorio.ufsm.br/bitstream/1/11957/2/license_rdf
http://repositorio.ufsm.br/bitstream/1/11957/3/license.txt
http://repositorio.ufsm.br/bitstream/1/11957/4/TES_PPGQU%c3%8dMICA_2016_VARGAS_JOSIMAR.pdf.txt
http://repositorio.ufsm.br/bitstream/1/11957/5/TES_PPGQU%c3%8dMICA_2016_VARGAS_JOSIMAR.pdf.jpg
bitstream.checksum.fl_str_mv 7eba519c0ed2ae98cde3b803d758c625
c1efe8e24d7281448e873be30ea326ff
2f0571ecee68693bd5cd3f17c1e075df
d9a008bce20e198e60655d77c8020ddd
b55234464c1e298da0fa2f931c88805f
bitstream.checksumAlgorithm.fl_str_mv MD5
MD5
MD5
MD5
MD5
repository.name.fl_str_mv Biblioteca Digital de Teses e Dissertações do UFSM - Universidade Federal de Santa Maria (UFSM)
repository.mail.fl_str_mv atendimento.sib@ufsm.br||tedebc@gmail.com
_version_ 1793240025180143616

Registros relacionados