Antibióticos macrolídeos: determinação e identificação de metabólitos e subprodutos de degradação em efluente hospitalar
Autor(a) principal: | |
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Data de Publicação: | 2013 |
Tipo de documento: | Tese |
Idioma: | por |
Título da fonte: | Manancial - Repositório Digital da UFSM |
dARK ID: | ark:/26339/001300000q952 |
Texto Completo: | http://repositorio.ufsm.br/handle/1/4262 |
Resumo: | Macrolide antibiotics are an important group of prescription drugs; as a consequence of the large and continuous use, they are commonly found in the environment. In the present study, it was developed and optimized a chromatographic method to assess the occurrence of macrolide antibiotics Azithromycin, Clarithromycin, Erythromycin and Roxithromycin in the effluent of the University Hospital of Santa Maria, in two sampling points, by applying high performance liquid chromatography coupled to mass detection with quadrupole ion trap (HPLC-MS/MS_QTrap) and clean-up/pre-concentration by solid phase extraction with the aid of Surface Methodology Response. The concentrations measured during a week in the hospital effluent were 1.32±0.13 and 0.22±0.06 μg L-1 for Azithromycin and Clarithromycin; in the receptor water sream was 1.12±0.20, 0.20±0.05 and 0.01±0.004 μg L-1 for Azithromycin, Clarithromycin and Erythromycin. Roxithromycin was not detected in all effluent samples. After this, it was done the evaluation of the risk quotient of the macrolide antibiotics. The value of the risk quotient for the hospital effluent for Azithromycin and Clarithromycin was 11 (high risk), and for the receptor water stream the risk quotient was 9.3 and 10.0 for Azithromycin and Clarithromycin; for Erythromycin, a quocient risk value of 0.5 (medium risk). For degradation of the antibiotics in aqueous solution, it was used UV-photolysis, by which the influence of pH (3-11) was evaluated. Azithromycin showed low degradation by acid pH; for other pH, as well, for all the other antibiotics, the degradation was above 70% after 60 min of treatment. It was conducted a kinetic study of the degradation process of macrolide antibiotics in different pHs, by which Azithromycin revealed a recalcitrant profile, and Roxithromycin, as the more easily degradable one. For identification of the products formed during the photolysis experiments it was used independent information acquisition and as precursor ions of fragments m/z 116 and 158, characteristic of the macrolide compounds, at three collision energies (30, 45, and 60 V). It was proposed fragmentation routes of the degradation products: 8 products for Azithromycin, 7 for Clarithromycin, 6 of Erythromycin and 8 Roxithromycin. Through the same experiments with independent information acquisition, it was investigated the presence of eventual metabolites in hospital effluent, and three metabolites were found. By applying photolysis to the hospital effluent fortified, at pH 7, it was observed that the degradation occurs above 80% for all compounds after 60 min of irradiation. It was observed the formation of degradation products previously determined by experiments in aqueous solution. It was also found three degradation products for Azithromycin, 2 for Clarithromycin, 1 for Erythromycin and 3 for Roxithromycin. |
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Antibióticos macrolídeos: determinação e identificação de metabólitos e subprodutos de degradação em efluente hospitalarMacrolides antibiotics: determination and identification of metabolites and degradation subproducts in hospital effluentAntibióticos macrolídeosEfluente hospitalarFotodegradaçãoProdutos de degradaçãoMetabólitosMacrolide antibioticsEffluent hospitalPhotodegradationDegradation productsMetabolitesCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICAMacrolide antibiotics are an important group of prescription drugs; as a consequence of the large and continuous use, they are commonly found in the environment. In the present study, it was developed and optimized a chromatographic method to assess the occurrence of macrolide antibiotics Azithromycin, Clarithromycin, Erythromycin and Roxithromycin in the effluent of the University Hospital of Santa Maria, in two sampling points, by applying high performance liquid chromatography coupled to mass detection with quadrupole ion trap (HPLC-MS/MS_QTrap) and clean-up/pre-concentration by solid phase extraction with the aid of Surface Methodology Response. The concentrations measured during a week in the hospital effluent were 1.32±0.13 and 0.22±0.06 μg L-1 for Azithromycin and Clarithromycin; in the receptor water sream was 1.12±0.20, 0.20±0.05 and 0.01±0.004 μg L-1 for Azithromycin, Clarithromycin and Erythromycin. Roxithromycin was not detected in all effluent samples. After this, it was done the evaluation of the risk quotient of the macrolide antibiotics. The value of the risk quotient for the hospital effluent for Azithromycin and Clarithromycin was 11 (high risk), and for the receptor water stream the risk quotient was 9.3 and 10.0 for Azithromycin and Clarithromycin; for Erythromycin, a quocient risk value of 0.5 (medium risk). For degradation of the antibiotics in aqueous solution, it was used UV-photolysis, by which the influence of pH (3-11) was evaluated. Azithromycin showed low degradation by acid pH; for other pH, as well, for all the other antibiotics, the degradation was above 70% after 60 min of treatment. It was conducted a kinetic study of the degradation process of macrolide antibiotics in different pHs, by which Azithromycin revealed a recalcitrant profile, and Roxithromycin, as the more easily degradable one. For identification of the products formed during the photolysis experiments it was used independent information acquisition and as precursor ions of fragments m/z 116 and 158, characteristic of the macrolide compounds, at three collision energies (30, 45, and 60 V). It was proposed fragmentation routes of the degradation products: 8 products for Azithromycin, 7 for Clarithromycin, 6 of Erythromycin and 8 Roxithromycin. Through the same experiments with independent information acquisition, it was investigated the presence of eventual metabolites in hospital effluent, and three metabolites were found. By applying photolysis to the hospital effluent fortified, at pH 7, it was observed that the degradation occurs above 80% for all compounds after 60 min of irradiation. It was observed the formation of degradation products previously determined by experiments in aqueous solution. It was also found three degradation products for Azithromycin, 2 for Clarithromycin, 1 for Erythromycin and 3 for Roxithromycin.Conselho Nacional de Desenvolvimento Científico e TecnológicoOs antibióticos macrolídeos são uma importante classe de fármacos preescritos no tratamento das mais variadas infecções, e como consequência se seu grande e continuo uso são comumente encontradas no ambiente. No presente estudo foi desenvolvido e otimizado método de cromatografia líquida de alta eficiência acoplada à detector de massas quadrupolo íon trap (HPLC-MS/MS_QTrap) e de clean-up/pré-concentração por extração em fase sólida com auxílio de Metodologia de Superfície de Resposta para avaliar a ocorrência dos antibióticos macrolídeos Azitromicina, Claritromicina, Eritromicina e Roxitromicina no efluente hospitalar do Hospital Universitário de Santa Maria em dois ponto de amostragem. As concentrações médias durante o ciclo de uma semana de amostragem no efluente do pronto atendimento foram de 1,32±0,13 e 0,22±0,06 g L-1 para Azitromicina e Claritromicina; no corpo recpetor foram de 1,12±0,20; 0,20±0,05 e 0,01±0,004 g L-1 para Azitromicina, Claritromicina e Eritromicina, respectivamente. Roxitromicina não foi detectada. Após foi feita a avaliação do quociente de risco dos antibióticos macrolídeos. O quociente de risco no efluente do pronto atendimento para Azitromicina e Claritromicina foi de 11, risco alto, o qual também foi evidenciado no corpo receptor com quociente de risco de 9,3 e 10 para Azitromicina e Claritromicna, e risco médio para Eritromicina de 0,5. Para degradação dos antibióticos foi utilizado fotólise artificial em solução aquosa, sendo avaliado a influência do pH de 3-11 na degradação destes compostos. Azitromicina apresentou baixa degradação em pH ácido, para os outros pH e demais compostos a degradação foi acima de 70% após 60 min de tratamento. Foi feito um estudo cinético do processo de degradação dos antibióticos macrolídeos em diferentes pH, observando-se que a Azitromicina apresentou um perfil recalcitrante para o processo, e Roxitromicina foi degradada com maior facilidade. Para a identificação dos produtos formados durante os experimentos de fotodegradação foram montados experimentos de informação independente de aquisição utilizando como íons precursores os íons de m/z 116 e 158 característicos dos compostos macrolídeos em três energias de colisão (30, 45 e 60 V). Foram identificadas e propostas rotas de fragmentação para 8 produtos de degradação de Azitromicina, 7 para Claritromicina, 6 para Eritromicina e 8 produtos de degradação de Roxiromicina. Através dos mesmos experimentos de informação independente de aquisição, foi investigada a presença de possíveis metabólitos no efluente hospitalar sendo encontrados 3 metabólitos. Com a aplicação de fotólise ao efluente hospitalar fortificado, em pH 7, observou-se que ocorre degradação acima de 80% para todos os compostos após 60 min de tratamneto. Foi observada a formação de produtos de degradação, que tinham sido previamente determinados em solução aquosa. Foram encontrados 3 produtos de degradação de Azitromicina, 2 para Claritromicina, 1 para Eritromicina e 3 produtos para Roxitromicina.Universidade Federal de Santa MariaBRQuímicaUFSMPrograma de Pós-Graduação em QuímicaMartins, Ayrton Figueiredohttp://lattes.cnpq.br/2113532494494821Arsand, Daniel Ricardohttp://lattes.cnpq.br/2243464346389170Primel, Ednei Gilbertohttp://lattes.cnpq.br/3259602390948297Vasconcelos, Tibiriçá Gonçalveshttp://lattes.cnpq.br/6407925163803842Martins, Manoel Leonardohttp://lattes.cnpq.br/4404290090180984Minetto, Luciane2017-05-182017-05-182013-08-09info:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/doctoralThesisapplication/pdfapplication/pdfMINETTO, Luciane. Macrolides antibiotics: determination and identification of metabolites and degradation subproducts in hospital effluent. 2013. 146 f. Tese (Doutorado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2013.http://repositorio.ufsm.br/handle/1/4262ark:/26339/001300000q952porinfo:eu-repo/semantics/openAccessreponame:Manancial - Repositório Digital da UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSM2022-06-03T12:54:28Zoai:repositorio.ufsm.br:1/4262Biblioteca Digital de Teses e Dissertaçõeshttps://repositorio.ufsm.br/ONGhttps://repositorio.ufsm.br/oai/requestatendimento.sib@ufsm.br||tedebc@gmail.comopendoar:2022-06-03T12:54:28Manancial - Repositório Digital da UFSM - Universidade Federal de Santa Maria (UFSM)false |
dc.title.none.fl_str_mv |
Antibióticos macrolídeos: determinação e identificação de metabólitos e subprodutos de degradação em efluente hospitalar Macrolides antibiotics: determination and identification of metabolites and degradation subproducts in hospital effluent |
title |
Antibióticos macrolídeos: determinação e identificação de metabólitos e subprodutos de degradação em efluente hospitalar |
spellingShingle |
Antibióticos macrolídeos: determinação e identificação de metabólitos e subprodutos de degradação em efluente hospitalar Minetto, Luciane Antibióticos macrolídeos Efluente hospitalar Fotodegradação Produtos de degradação Metabólitos Macrolide antibiotics Effluent hospital Photodegradation Degradation products Metabolites CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Antibióticos macrolídeos: determinação e identificação de metabólitos e subprodutos de degradação em efluente hospitalar |
title_full |
Antibióticos macrolídeos: determinação e identificação de metabólitos e subprodutos de degradação em efluente hospitalar |
title_fullStr |
Antibióticos macrolídeos: determinação e identificação de metabólitos e subprodutos de degradação em efluente hospitalar |
title_full_unstemmed |
Antibióticos macrolídeos: determinação e identificação de metabólitos e subprodutos de degradação em efluente hospitalar |
title_sort |
Antibióticos macrolídeos: determinação e identificação de metabólitos e subprodutos de degradação em efluente hospitalar |
author |
Minetto, Luciane |
author_facet |
Minetto, Luciane |
author_role |
author |
dc.contributor.none.fl_str_mv |
Martins, Ayrton Figueiredo http://lattes.cnpq.br/2113532494494821 Arsand, Daniel Ricardo http://lattes.cnpq.br/2243464346389170 Primel, Ednei Gilberto http://lattes.cnpq.br/3259602390948297 Vasconcelos, Tibiriçá Gonçalves http://lattes.cnpq.br/6407925163803842 Martins, Manoel Leonardo http://lattes.cnpq.br/4404290090180984 |
dc.contributor.author.fl_str_mv |
Minetto, Luciane |
dc.subject.por.fl_str_mv |
Antibióticos macrolídeos Efluente hospitalar Fotodegradação Produtos de degradação Metabólitos Macrolide antibiotics Effluent hospital Photodegradation Degradation products Metabolites CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
topic |
Antibióticos macrolídeos Efluente hospitalar Fotodegradação Produtos de degradação Metabólitos Macrolide antibiotics Effluent hospital Photodegradation Degradation products Metabolites CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
Macrolide antibiotics are an important group of prescription drugs; as a consequence of the large and continuous use, they are commonly found in the environment. In the present study, it was developed and optimized a chromatographic method to assess the occurrence of macrolide antibiotics Azithromycin, Clarithromycin, Erythromycin and Roxithromycin in the effluent of the University Hospital of Santa Maria, in two sampling points, by applying high performance liquid chromatography coupled to mass detection with quadrupole ion trap (HPLC-MS/MS_QTrap) and clean-up/pre-concentration by solid phase extraction with the aid of Surface Methodology Response. The concentrations measured during a week in the hospital effluent were 1.32±0.13 and 0.22±0.06 μg L-1 for Azithromycin and Clarithromycin; in the receptor water sream was 1.12±0.20, 0.20±0.05 and 0.01±0.004 μg L-1 for Azithromycin, Clarithromycin and Erythromycin. Roxithromycin was not detected in all effluent samples. After this, it was done the evaluation of the risk quotient of the macrolide antibiotics. The value of the risk quotient for the hospital effluent for Azithromycin and Clarithromycin was 11 (high risk), and for the receptor water stream the risk quotient was 9.3 and 10.0 for Azithromycin and Clarithromycin; for Erythromycin, a quocient risk value of 0.5 (medium risk). For degradation of the antibiotics in aqueous solution, it was used UV-photolysis, by which the influence of pH (3-11) was evaluated. Azithromycin showed low degradation by acid pH; for other pH, as well, for all the other antibiotics, the degradation was above 70% after 60 min of treatment. It was conducted a kinetic study of the degradation process of macrolide antibiotics in different pHs, by which Azithromycin revealed a recalcitrant profile, and Roxithromycin, as the more easily degradable one. For identification of the products formed during the photolysis experiments it was used independent information acquisition and as precursor ions of fragments m/z 116 and 158, characteristic of the macrolide compounds, at three collision energies (30, 45, and 60 V). It was proposed fragmentation routes of the degradation products: 8 products for Azithromycin, 7 for Clarithromycin, 6 of Erythromycin and 8 Roxithromycin. Through the same experiments with independent information acquisition, it was investigated the presence of eventual metabolites in hospital effluent, and three metabolites were found. By applying photolysis to the hospital effluent fortified, at pH 7, it was observed that the degradation occurs above 80% for all compounds after 60 min of irradiation. It was observed the formation of degradation products previously determined by experiments in aqueous solution. It was also found three degradation products for Azithromycin, 2 for Clarithromycin, 1 for Erythromycin and 3 for Roxithromycin. |
publishDate |
2013 |
dc.date.none.fl_str_mv |
2013-08-09 2017-05-18 2017-05-18 |
dc.type.status.fl_str_mv |
info:eu-repo/semantics/publishedVersion |
dc.type.driver.fl_str_mv |
info:eu-repo/semantics/doctoralThesis |
format |
doctoralThesis |
status_str |
publishedVersion |
dc.identifier.uri.fl_str_mv |
MINETTO, Luciane. Macrolides antibiotics: determination and identification of metabolites and degradation subproducts in hospital effluent. 2013. 146 f. Tese (Doutorado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2013. http://repositorio.ufsm.br/handle/1/4262 |
dc.identifier.dark.fl_str_mv |
ark:/26339/001300000q952 |
identifier_str_mv |
MINETTO, Luciane. Macrolides antibiotics: determination and identification of metabolites and degradation subproducts in hospital effluent. 2013. 146 f. Tese (Doutorado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2013. ark:/26339/001300000q952 |
url |
http://repositorio.ufsm.br/handle/1/4262 |
dc.language.iso.fl_str_mv |
por |
language |
por |
dc.rights.driver.fl_str_mv |
info:eu-repo/semantics/openAccess |
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openAccess |
dc.format.none.fl_str_mv |
application/pdf application/pdf |
dc.publisher.none.fl_str_mv |
Universidade Federal de Santa Maria BR Química UFSM Programa de Pós-Graduação em Química |
publisher.none.fl_str_mv |
Universidade Federal de Santa Maria BR Química UFSM Programa de Pós-Graduação em Química |
dc.source.none.fl_str_mv |
reponame:Manancial - Repositório Digital da 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 |
Manancial - Repositório Digital da UFSM |
collection |
Manancial - Repositório Digital da UFSM |
repository.name.fl_str_mv |
Manancial - Repositório Digital da UFSM - Universidade Federal de Santa Maria (UFSM) |
repository.mail.fl_str_mv |
atendimento.sib@ufsm.br||tedebc@gmail.com |
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1815172378217414656 |