Sulfonamides in milk by high performance liquid chromatography with pre-column derivatization and fluorescence detection

Detalhes bibliográficos
Autor(a) principal: Alaburda, Janete
Data de Publicação: 2007
Outros Autores: Ruvieri, Valter, Shundo, Luzia, Almeida, Adriana Palma de, Tiglea, Paulo, Sabino, Myrna
Tipo de documento: Artigo
Idioma: por
Título da fonte: Pesquisa Agropecuária Brasileira (Online)
Texto Completo: https://seer.sct.embrapa.br/index.php/pab/article/view/7736
Resumo: The objective of this work was to evaluate and validate a method for analysis of sulfathiazole (STZ), sulfamethazine (SMZ) and sulfadimethoxine (SDM) residues in milk. Extraction was carried out with diclhoromethane followed by silica solid phase extraction. The extracts were derivatizated with fluorescamine and quantified by reversed-phase high performance liquid chromatography with fluorescence detection. The detection limit for the three sulfonamides was 0.3 µg L-1 and the quantification limit was 1 µg L-1 for STZ and SMZ and 2.5 µg L-1 for SDM, with coefficient of variation ranging from 4.4 to 6.6%. The recoveries for STZ, SMZ and SDM were 63.2, 91.2 and 63.2%, respectively. Considering that Brazilian regulation sets maximum residue limit in milk of 100 µg kg-1 for total sulfonamide concentrations (STZ, SMZ and SDM), the present method is adequate to quantify the residues of three sulfonamides simultaneously in UHT milk.
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spelling Sulfonamides in milk by high performance liquid chromatography with pre-column derivatization and fluorescence detectionSulfonamidas em leite por cromatografia líquida de alta eficiência com derivação pré-coluna e detecção por fluorescênciafluorescamine; sulphonamides; sulfamethazine; sulfadimethoxinefluorescamina; sulfonamida; sulfametazina; sulfadimetoxinaThe objective of this work was to evaluate and validate a method for analysis of sulfathiazole (STZ), sulfamethazine (SMZ) and sulfadimethoxine (SDM) residues in milk. Extraction was carried out with diclhoromethane followed by silica solid phase extraction. The extracts were derivatizated with fluorescamine and quantified by reversed-phase high performance liquid chromatography with fluorescence detection. The detection limit for the three sulfonamides was 0.3 µg L-1 and the quantification limit was 1 µg L-1 for STZ and SMZ and 2.5 µg L-1 for SDM, with coefficient of variation ranging from 4.4 to 6.6%. The recoveries for STZ, SMZ and SDM were 63.2, 91.2 and 63.2%, respectively. Considering that Brazilian regulation sets maximum residue limit in milk of 100 µg kg-1 for total sulfonamide concentrations (STZ, SMZ and SDM), the present method is adequate to quantify the residues of three sulfonamides simultaneously in UHT milk.O objetivo deste trabalho foi avaliar e validar um método para deteminação de resíduos de sulfatiazol (STZ), sulfametazina (SMZ) e sulfadimetoxina (SDM) em leite UHT integral. A extração foi realizada com diclorometano e coluna de extração em fase sólida de sílica. Os resíduos, após derivação com fluorescamina, foram quantificados por cromatografia líquida de alta eficiência com detector de fluorescência. O limite de detecção das três sulfas em amostra de leite integral foi 0,3 µg L-1 e o limite de quantificação foi 1 µg L-1 para STZ e SMZ e 2,5 µg L-1 para SDM, com coeficientes de variação entre 4,4 e 6,6%. Os valores de recuperação para STZ, SMZ e SDM foram 63,2, 91,2 e 63,2%, respectivamente. Considerando o limite máximo de resíduo estabelecido pela legislação brasileira de 100 µg kg-1 para a soma das concentrações totais de STZ, SMZ e SDM, o método descrito permite a determinação simultânea dos três analitos em amostras de leite UTH integral.Pesquisa Agropecuaria BrasileiraPesquisa Agropecuária BrasileiraAlaburda, JaneteRuvieri, ValterShundo, LuziaAlmeida, Adriana Palma deTiglea, PauloSabino, Myrna2007-11-01info:eu-repo/semantics/articleinfo:eu-repo/semantics/publishedVersionapplication/pdfhttps://seer.sct.embrapa.br/index.php/pab/article/view/7736Pesquisa Agropecuaria Brasileira; v.42, n.11, nov. 2007; 1587-1592Pesquisa Agropecuária Brasileira; v.42, n.11, nov. 2007; 1587-15921678-39210100-104xreponame:Pesquisa Agropecuária Brasileira (Online)instname:Empresa Brasileira de Pesquisa Agropecuária (Embrapa)instacron:EMBRAPAporhttps://seer.sct.embrapa.br/index.php/pab/article/view/7736/4655info:eu-repo/semantics/openAccess2010-10-04T14:48:46Zoai:ojs.seer.sct.embrapa.br:article/7736Revistahttp://seer.sct.embrapa.br/index.php/pabPRIhttps://old.scielo.br/oai/scielo-oai.phppab@sct.embrapa.br || sct.pab@embrapa.br1678-39210100-204Xopendoar:2010-10-04T14:48:46Pesquisa Agropecuária Brasileira (Online) - Empresa Brasileira de Pesquisa Agropecuária (Embrapa)false
dc.title.none.fl_str_mv Sulfonamides in milk by high performance liquid chromatography with pre-column derivatization and fluorescence detection
Sulfonamidas em leite por cromatografia líquida de alta eficiência com derivação pré-coluna e detecção por fluorescência
title Sulfonamides in milk by high performance liquid chromatography with pre-column derivatization and fluorescence detection
spellingShingle Sulfonamides in milk by high performance liquid chromatography with pre-column derivatization and fluorescence detection
Alaburda, Janete
fluorescamine; sulphonamides; sulfamethazine; sulfadimethoxine
fluorescamina; sulfonamida; sulfametazina; sulfadimetoxina
title_short Sulfonamides in milk by high performance liquid chromatography with pre-column derivatization and fluorescence detection
title_full Sulfonamides in milk by high performance liquid chromatography with pre-column derivatization and fluorescence detection
title_fullStr Sulfonamides in milk by high performance liquid chromatography with pre-column derivatization and fluorescence detection
title_full_unstemmed Sulfonamides in milk by high performance liquid chromatography with pre-column derivatization and fluorescence detection
title_sort Sulfonamides in milk by high performance liquid chromatography with pre-column derivatization and fluorescence detection
author Alaburda, Janete
author_facet Alaburda, Janete
Ruvieri, Valter
Shundo, Luzia
Almeida, Adriana Palma de
Tiglea, Paulo
Sabino, Myrna
author_role author
author2 Ruvieri, Valter
Shundo, Luzia
Almeida, Adriana Palma de
Tiglea, Paulo
Sabino, Myrna
author2_role author
author
author
author
author
dc.contributor.none.fl_str_mv

dc.contributor.author.fl_str_mv Alaburda, Janete
Ruvieri, Valter
Shundo, Luzia
Almeida, Adriana Palma de
Tiglea, Paulo
Sabino, Myrna
dc.subject.por.fl_str_mv fluorescamine; sulphonamides; sulfamethazine; sulfadimethoxine
fluorescamina; sulfonamida; sulfametazina; sulfadimetoxina
topic fluorescamine; sulphonamides; sulfamethazine; sulfadimethoxine
fluorescamina; sulfonamida; sulfametazina; sulfadimetoxina
description The objective of this work was to evaluate and validate a method for analysis of sulfathiazole (STZ), sulfamethazine (SMZ) and sulfadimethoxine (SDM) residues in milk. Extraction was carried out with diclhoromethane followed by silica solid phase extraction. The extracts were derivatizated with fluorescamine and quantified by reversed-phase high performance liquid chromatography with fluorescence detection. The detection limit for the three sulfonamides was 0.3 µg L-1 and the quantification limit was 1 µg L-1 for STZ and SMZ and 2.5 µg L-1 for SDM, with coefficient of variation ranging from 4.4 to 6.6%. The recoveries for STZ, SMZ and SDM were 63.2, 91.2 and 63.2%, respectively. Considering that Brazilian regulation sets maximum residue limit in milk of 100 µg kg-1 for total sulfonamide concentrations (STZ, SMZ and SDM), the present method is adequate to quantify the residues of three sulfonamides simultaneously in UHT milk.
publishDate 2007
dc.date.none.fl_str_mv 2007-11-01
dc.type.none.fl_str_mv
dc.type.driver.fl_str_mv info:eu-repo/semantics/article
info:eu-repo/semantics/publishedVersion
format article
status_str publishedVersion
dc.identifier.uri.fl_str_mv https://seer.sct.embrapa.br/index.php/pab/article/view/7736
url https://seer.sct.embrapa.br/index.php/pab/article/view/7736
dc.language.iso.fl_str_mv por
language por
dc.relation.none.fl_str_mv https://seer.sct.embrapa.br/index.php/pab/article/view/7736/4655
dc.rights.driver.fl_str_mv info:eu-repo/semantics/openAccess
eu_rights_str_mv openAccess
dc.format.none.fl_str_mv application/pdf
dc.publisher.none.fl_str_mv Pesquisa Agropecuaria Brasileira
Pesquisa Agropecuária Brasileira
publisher.none.fl_str_mv Pesquisa Agropecuaria Brasileira
Pesquisa Agropecuária Brasileira
dc.source.none.fl_str_mv Pesquisa Agropecuaria Brasileira; v.42, n.11, nov. 2007; 1587-1592
Pesquisa Agropecuária Brasileira; v.42, n.11, nov. 2007; 1587-1592
1678-3921
0100-104x
reponame:Pesquisa Agropecuária Brasileira (Online)
instname:Empresa Brasileira de Pesquisa Agropecuária (Embrapa)
instacron:EMBRAPA
instname_str Empresa Brasileira de Pesquisa Agropecuária (Embrapa)
instacron_str EMBRAPA
institution EMBRAPA
reponame_str Pesquisa Agropecuária Brasileira (Online)
collection Pesquisa Agropecuária Brasileira (Online)
repository.name.fl_str_mv Pesquisa Agropecuária Brasileira (Online) - Empresa Brasileira de Pesquisa Agropecuária (Embrapa)
repository.mail.fl_str_mv pab@sct.embrapa.br || sct.pab@embrapa.br
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