In-house validation for multi-residue analysis of tetracycline in cow milk by HPLC with UV detection

Detalhes bibliográficos
Autor(a) principal: Prado, Carolina Kato
Data de Publicação: 2017
Outros Autores: Ferreira, Flavio Dias, Bando, Erika, Machinski Junior, Miguel
Tipo de documento: Artigo
Idioma: eng
Título da fonte: Semina. Ciências Agrárias (Online)
Texto Completo: https://ojs.uel.br/revistas/uel/index.php/semagrarias/article/view/26373
Resumo: The indiscriminate use of antibiotics in dairy cattle without complying with the waiting period results in residual contamination, whose effective control in produced milk requires validated methods toensure analytical results. The aim of this study was to optimize and validate the HPLC-UV/VIS method at 365 nm for analyzingthe tetracycline in pasteurized cow milk in accordance with the European Community (2002/657/EC). Spiked milk with analytes (oxytetracycline, tetracycline, doxycycline, and chlortetracycline) was submitted to deproteinization and cleaning by a C18 solid-phase column and analyzed by HPLC using a gradient system with 0.01 mol L?1 oxalic acid-acetonitrile-triethylamine (90:9.9:0.1) and acetonitrile on a reverse phase (C18) column. Accuracy and precision were assessed by adding analytes to levels of 0.5, 1, and 1.5 times the permissible maximum limit allowed in Brazil. The method presented selectivity with a decision limit (CC?) and detection capability (CC?) ranging from 114.2 to 143.7 and from 129.3 to 188.7 µg kg?1, respectively. The recovery of tetracyclines was higher than 82.5% with a precision of 7.1%, demonstrating theefficiency in determining tetracycline residues in cow milk.
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spelling In-house validation for multi-residue analysis of tetracycline in cow milk by HPLC with UV detectionValidação intralaboratorial para análise múltipla dos resíduos de tetraciclina em leite bovino por cromatografia líquida de alta eficiência com detecção UVIn-house validationTetracycline residuesHigh-performance liquid chromatographyCow milkToxicology analysis.Validação intralaboratorialResíduos de tetraciclinaCromatografia líquida de alta eficiênciaLeite bovinoAnálise toxicológica.The indiscriminate use of antibiotics in dairy cattle without complying with the waiting period results in residual contamination, whose effective control in produced milk requires validated methods toensure analytical results. The aim of this study was to optimize and validate the HPLC-UV/VIS method at 365 nm for analyzingthe tetracycline in pasteurized cow milk in accordance with the European Community (2002/657/EC). Spiked milk with analytes (oxytetracycline, tetracycline, doxycycline, and chlortetracycline) was submitted to deproteinization and cleaning by a C18 solid-phase column and analyzed by HPLC using a gradient system with 0.01 mol L?1 oxalic acid-acetonitrile-triethylamine (90:9.9:0.1) and acetonitrile on a reverse phase (C18) column. Accuracy and precision were assessed by adding analytes to levels of 0.5, 1, and 1.5 times the permissible maximum limit allowed in Brazil. The method presented selectivity with a decision limit (CC?) and detection capability (CC?) ranging from 114.2 to 143.7 and from 129.3 to 188.7 µg kg?1, respectively. The recovery of tetracyclines was higher than 82.5% with a precision of 7.1%, demonstrating theefficiency in determining tetracycline residues in cow milk.O uso indiscriminado de antibiótico em gado leiteiro, sem cumprimento do período de carência, resulta em contaminação residual, cujo controle efetivo no leite produzido requer métodos validados que garantam os resultados analíticos. O estudo visou otimizar e validar o método de CLAE-UV/VIS a 365 nm para análise de tetraciclina em leite bovino pasteurizado em conformidade com a Comunidade Europeia (2002/657/EC). O leite fortificado com analitos (oxitetraciclina, tetraciclina, doxiciclina e clortetraciclina) foi submetido à extração por desproteinização e limpeza por coluna de fase sólida C18 e submetido à análise por CLAE empregando sistema gradiente com 0,01 mol L-1 de ácido oxálico-acetonitrila-trietilamina (90:9,9:0,1) e acetonitrila, em coluna de fase reversa (C18). A exatidão e precisão foram avaliadas adicionando o analitos em níveis de 0,5, 1 e 1,5 vezes o limite máximo permitido no Brasil. O método apresentou seletividade com limite de decisão (CC?) e capacidade de detecção (CC?) variando de 114,2 a 143,7 e 129,3 a 188,7 µg kg-1, respectivamente. A recuperação de tetraciclinas foi superior a 82,5% e a precisão de 7,1%, demonstrando eficiência para a determinação de resíduos de tetraciclina em leite bovino.UEL2017-11-23info:eu-repo/semantics/articleinfo:eu-repo/semantics/publishedVersionInvestigação científicaapplication/pdfhttps://ojs.uel.br/revistas/uel/index.php/semagrarias/article/view/2637310.5433/1679-0359.2017v38n6p3539Semina: Ciências Agrárias; Vol. 38 No. 6 (2017); 3539-3548Semina: Ciências Agrárias; v. 38 n. 6 (2017); 3539-35481679-03591676-546Xreponame:Semina. Ciências Agrárias (Online)instname:Universidade Estadual de Londrina (UEL)instacron:UELenghttps://ojs.uel.br/revistas/uel/index.php/semagrarias/article/view/26373/22261Copyright (c) 2017 Semina: Ciências Agráriashttp://creativecommons.org/licenses/by-nc/4.0info:eu-repo/semantics/openAccessPrado, Carolina KatoFerreira, Flavio DiasBando, ErikaMachinski Junior, Miguel2022-10-21T12:49:17Zoai:ojs.pkp.sfu.ca:article/26373Revistahttp://www.uel.br/revistas/uel/index.php/semagrariasPUBhttps://ojs.uel.br/revistas/uel/index.php/semagrarias/oaisemina.agrarias@uel.br1679-03591676-546Xopendoar:2022-10-21T12:49:17Semina. Ciências Agrárias (Online) - Universidade Estadual de Londrina (UEL)false
dc.title.none.fl_str_mv In-house validation for multi-residue analysis of tetracycline in cow milk by HPLC with UV detection
Validação intralaboratorial para análise múltipla dos resíduos de tetraciclina em leite bovino por cromatografia líquida de alta eficiência com detecção UV
title In-house validation for multi-residue analysis of tetracycline in cow milk by HPLC with UV detection
spellingShingle In-house validation for multi-residue analysis of tetracycline in cow milk by HPLC with UV detection
Prado, Carolina Kato
In-house validation
Tetracycline residues
High-performance liquid chromatography
Cow milk
Toxicology analysis.
Validação intralaboratorial
Resíduos de tetraciclina
Cromatografia líquida de alta eficiência
Leite bovino
Análise toxicológica.
title_short In-house validation for multi-residue analysis of tetracycline in cow milk by HPLC with UV detection
title_full In-house validation for multi-residue analysis of tetracycline in cow milk by HPLC with UV detection
title_fullStr In-house validation for multi-residue analysis of tetracycline in cow milk by HPLC with UV detection
title_full_unstemmed In-house validation for multi-residue analysis of tetracycline in cow milk by HPLC with UV detection
title_sort In-house validation for multi-residue analysis of tetracycline in cow milk by HPLC with UV detection
author Prado, Carolina Kato
author_facet Prado, Carolina Kato
Ferreira, Flavio Dias
Bando, Erika
Machinski Junior, Miguel
author_role author
author2 Ferreira, Flavio Dias
Bando, Erika
Machinski Junior, Miguel
author2_role author
author
author
dc.contributor.author.fl_str_mv Prado, Carolina Kato
Ferreira, Flavio Dias
Bando, Erika
Machinski Junior, Miguel
dc.subject.por.fl_str_mv In-house validation
Tetracycline residues
High-performance liquid chromatography
Cow milk
Toxicology analysis.
Validação intralaboratorial
Resíduos de tetraciclina
Cromatografia líquida de alta eficiência
Leite bovino
Análise toxicológica.
topic In-house validation
Tetracycline residues
High-performance liquid chromatography
Cow milk
Toxicology analysis.
Validação intralaboratorial
Resíduos de tetraciclina
Cromatografia líquida de alta eficiência
Leite bovino
Análise toxicológica.
description The indiscriminate use of antibiotics in dairy cattle without complying with the waiting period results in residual contamination, whose effective control in produced milk requires validated methods toensure analytical results. The aim of this study was to optimize and validate the HPLC-UV/VIS method at 365 nm for analyzingthe tetracycline in pasteurized cow milk in accordance with the European Community (2002/657/EC). Spiked milk with analytes (oxytetracycline, tetracycline, doxycycline, and chlortetracycline) was submitted to deproteinization and cleaning by a C18 solid-phase column and analyzed by HPLC using a gradient system with 0.01 mol L?1 oxalic acid-acetonitrile-triethylamine (90:9.9:0.1) and acetonitrile on a reverse phase (C18) column. Accuracy and precision were assessed by adding analytes to levels of 0.5, 1, and 1.5 times the permissible maximum limit allowed in Brazil. The method presented selectivity with a decision limit (CC?) and detection capability (CC?) ranging from 114.2 to 143.7 and from 129.3 to 188.7 µg kg?1, respectively. The recovery of tetracyclines was higher than 82.5% with a precision of 7.1%, demonstrating theefficiency in determining tetracycline residues in cow milk.
publishDate 2017
dc.date.none.fl_str_mv 2017-11-23
dc.type.driver.fl_str_mv info:eu-repo/semantics/article
info:eu-repo/semantics/publishedVersion
Investigação científica
format article
status_str publishedVersion
dc.identifier.uri.fl_str_mv https://ojs.uel.br/revistas/uel/index.php/semagrarias/article/view/26373
10.5433/1679-0359.2017v38n6p3539
url https://ojs.uel.br/revistas/uel/index.php/semagrarias/article/view/26373
identifier_str_mv 10.5433/1679-0359.2017v38n6p3539
dc.language.iso.fl_str_mv eng
language eng
dc.relation.none.fl_str_mv https://ojs.uel.br/revistas/uel/index.php/semagrarias/article/view/26373/22261
dc.rights.driver.fl_str_mv Copyright (c) 2017 Semina: Ciências Agrárias
http://creativecommons.org/licenses/by-nc/4.0
info:eu-repo/semantics/openAccess
rights_invalid_str_mv Copyright (c) 2017 Semina: Ciências Agrárias
http://creativecommons.org/licenses/by-nc/4.0
eu_rights_str_mv openAccess
dc.format.none.fl_str_mv application/pdf
dc.publisher.none.fl_str_mv UEL
publisher.none.fl_str_mv UEL
dc.source.none.fl_str_mv Semina: Ciências Agrárias; Vol. 38 No. 6 (2017); 3539-3548
Semina: Ciências Agrárias; v. 38 n. 6 (2017); 3539-3548
1679-0359
1676-546X
reponame:Semina. Ciências Agrárias (Online)
instname:Universidade Estadual de Londrina (UEL)
instacron:UEL
instname_str Universidade Estadual de Londrina (UEL)
instacron_str UEL
institution UEL
reponame_str Semina. Ciências Agrárias (Online)
collection Semina. Ciências Agrárias (Online)
repository.name.fl_str_mv Semina. Ciências Agrárias (Online) - Universidade Estadual de Londrina (UEL)
repository.mail.fl_str_mv semina.agrarias@uel.br
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