Antimicrobiais sulfametoxazol e trimetoprima em efluente hospitalar: determinação, degradação através de eletrocoagulação e identificação de subprodutos e metabólitos

Detalhes bibliográficos
Ano de defesa: 2009
Autor(a) principal: Brenner, Carla Geane Brandenburg lattes
Orientador(a): Martins, Ayrton Figueiredo lattes
Banca de defesa: Zanella, Renato lattes, Vasconcelos, Tibiriçá Gonçalves lattes
Tipo de documento: Dissertação
Tipo de acesso: Acesso aberto
Idioma: por
Instituição de defesa: Universidade Federal de Santa Maria
Programa de Pós-Graduação: Programa de Pós-Graduação em Química
Departamento: Química
País: BR
Palavras-chave em Português:
Área do conhecimento CNPq:
Link de acesso: http://repositorio.ufsm.br/handle/1/10446
Resumo: In this study, it was developed a methodology using liquid chromatography coupled to tandem mass spectrometry for the determination of antimicrobials sulphamethoxazole and trimethoprim in hospital effluent and for monitoring the electrocoagulation process applied to synthetic solutions, as well as, to the hospital effluent fortified with the antimicrobials, both at the same concentration of 1 mg L-1. The achieved limits of detection and quantification were 0.25 and 0.5 μg L-1, respectively. The linear range of the method was 0.5 to 100 μg L-1, with a correlation coefficient always greater than <0.9995 for both antimicrobials. The average concentration of sulphamethoxazole and trimethoprim found for the hospital effluent was 27.8 and 6.6 μg L-1, respectively. In order to study the best conditions for conducting the electrocoagulation, factorial design with surface response methodology was used. It was set as variables the distance of the electrodes, the concentration of electrolyte (NaCl) and the applied current (mA). As evaluation parameter it was used the chemical oxygen demand (COD) reduction of the hospital effluent. The best result for the COD reduction (57.9%) was achieved using 500 mg of NaCl, electrode distance of 30 mm and current of 800 mA. By means of the application of the electrocoagulation process to synthetic solutions of the antimicrobials and Soxhlet extraction, it was confirmed the true degradation or the reduction of the antimicrobial concentration by possible adsorption on the generated process sludge. From the average reduction of 84.7% of the initial sulphamethoxazole concentration, 6.0% of which were adsorbed by the sludge, resulting an average reduction 79.3%, at pH 5 and 7. The antimicrobial trimethoprim, at pH 5 and 7, showed an average reduction of 28.7% of the initial concentration by sludge adsorption, and no degradation occurred. The identification of the metabolites in hospital effluent and the degradation products generated by the electrocoagulation of the synthetic solution was performed using liquid chromatography quadrupole linear ion trap mass spectrometry. The metabolites identified were N4-acetylsulphamethoxazole and dihydroxitrimethoprim, and their paths of fragmentation were proposed. The degradation products of sulfamethoxazole identified were dihydroxyl sulphamethoxazole (identified only after 60 minutes treatment) and dehydrogenate sulphamethoxazole. For the electrocoagulation of the hospital effluent fortified with standard solutions of both antimicrobials, it was observed no degradation. Therefore, the degradation products in real effluent samples could not be studied. The electrocoagulation process applied to the hospital effluent was efficient by reducing COD under the conditions evaluated; but, it was not efficient by the degradation of the fortified antimicrobials in the effluent. The developed methodology used as analytical tool, LC-MS/MS_QTrap operating in lineal way, for the determination of the investigated antimicrobials in hospital wastewater, as well as for the efficiency evaluation of the electrocoagulation process by the concentration reduction or the degradation in synthetic solution and hospital wastewater, proved to be fast, sensitive, selective, sparing laborious manipulation of the sample.
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spelling 2017-05-112017-05-112009-03-03BRENNER, Carla Geane Brandenburg. Sulphamethoxazole and trimethoprim antimicrobials in hospital wastewater: determination, degradation through electrocoagulation and identification of bybproducts and metabolites. 2009. 93 f. Dissertação (Mestrado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2009.http://repositorio.ufsm.br/handle/1/10446In this study, it was developed a methodology using liquid chromatography coupled to tandem mass spectrometry for the determination of antimicrobials sulphamethoxazole and trimethoprim in hospital effluent and for monitoring the electrocoagulation process applied to synthetic solutions, as well as, to the hospital effluent fortified with the antimicrobials, both at the same concentration of 1 mg L-1. The achieved limits of detection and quantification were 0.25 and 0.5 μg L-1, respectively. The linear range of the method was 0.5 to 100 μg L-1, with a correlation coefficient always greater than <0.9995 for both antimicrobials. The average concentration of sulphamethoxazole and trimethoprim found for the hospital effluent was 27.8 and 6.6 μg L-1, respectively. In order to study the best conditions for conducting the electrocoagulation, factorial design with surface response methodology was used. It was set as variables the distance of the electrodes, the concentration of electrolyte (NaCl) and the applied current (mA). As evaluation parameter it was used the chemical oxygen demand (COD) reduction of the hospital effluent. The best result for the COD reduction (57.9%) was achieved using 500 mg of NaCl, electrode distance of 30 mm and current of 800 mA. By means of the application of the electrocoagulation process to synthetic solutions of the antimicrobials and Soxhlet extraction, it was confirmed the true degradation or the reduction of the antimicrobial concentration by possible adsorption on the generated process sludge. From the average reduction of 84.7% of the initial sulphamethoxazole concentration, 6.0% of which were adsorbed by the sludge, resulting an average reduction 79.3%, at pH 5 and 7. The antimicrobial trimethoprim, at pH 5 and 7, showed an average reduction of 28.7% of the initial concentration by sludge adsorption, and no degradation occurred. The identification of the metabolites in hospital effluent and the degradation products generated by the electrocoagulation of the synthetic solution was performed using liquid chromatography quadrupole linear ion trap mass spectrometry. The metabolites identified were N4-acetylsulphamethoxazole and dihydroxitrimethoprim, and their paths of fragmentation were proposed. The degradation products of sulfamethoxazole identified were dihydroxyl sulphamethoxazole (identified only after 60 minutes treatment) and dehydrogenate sulphamethoxazole. For the electrocoagulation of the hospital effluent fortified with standard solutions of both antimicrobials, it was observed no degradation. Therefore, the degradation products in real effluent samples could not be studied. The electrocoagulation process applied to the hospital effluent was efficient by reducing COD under the conditions evaluated; but, it was not efficient by the degradation of the fortified antimicrobials in the effluent. The developed methodology used as analytical tool, LC-MS/MS_QTrap operating in lineal way, for the determination of the investigated antimicrobials in hospital wastewater, as well as for the efficiency evaluation of the electrocoagulation process by the concentration reduction or the degradation in synthetic solution and hospital wastewater, proved to be fast, sensitive, selective, sparing laborious manipulation of the sample.Neste estudo, desenvolveu-se método utilizando cromatografia líquida acoplada à espectrometria de massas seqüencial para determinação dos antimicrobiais sulfametoxazol e trimetoprima em efluente hospitalar, bem como para avaliar o processo de eletrocoagulação aplicado à solução sintética dos antimicrobiais e ao efluente hospitalar fortificado com os fármacos, ambos na concentração de 1 mg L-1. Os limites de detecção e quantificação alcançados para ambos antimicrobiais foram de 0,25 e 0,5 μg L-1, respectivamente. A faixa linear do método foi de 0,5 a 100 μg L-1, com um coeficiente de correlação sempre superior à 0,9995, para ambos os antimicrobiais. As concentrações de sulfametoxazol e de trimetoprima encontradas no efluente hospitalar ficaram na faixa de 12,5 à 37,3 e 3,65 à 11,30 μg L-1, respectivamente. Para determinação das melhores condições de aplicação do processo de eletrocoagulação ao efluente hospitalar utilizou-se planejamento fatorial com superfície de resposta. Como variáveis foram usadas a distância dos eletrodos, a concentração de eletrólito (NaCl) e a corrente aplicada (mA). Como parâmetro de avaliação usou-se a redução da demanda química de oxigênio (DQO). Os melhores resultados obtidos na redução da DQO (57,9%) foram alcançados utilizando-se 500 mg de NaCl, distância dos eletrodos de 30 mm e corrente de 800 mA. Através da aplicação do processo de eletrocoagulação à solução sintética de ambos os antimicrobiais e por meio da extração Soxhlet pôde-se confirmar a real degradação ou a diminuição da concentração dos antimicrobiais em solução pela possível adsorção destes, no lodo gerado no processo. O sulfametoxazol apresentou uma diminuição média da concentração inicial de 84,7%, sendo que, destes, 6,0% ficaram adsorvidos ao lodo, alcançando, assim, uma degradação média de 79,2%, em pH 5 e 7. A trimetoprima, em pH 5 e 7, apresentou uma redução média da concentração inicial de 28,7% sendo que ocorreu total adsorção ao lodo, não havendo degradação. A identificação dos metabólitos no efluente hospitalar e de produtos de degradação gerados na aplicação de eletrocoagulação à solução sintética foi feita através de cromatografia líquida acoplada à espectrometria de massas quadrupolo linear e trapeamento iônico (LC-MS/MS_QTrap). Os metabólitos identificados foram o N4-acetilsulfametoxazol e o dihidroxitrimetoprima. Caminhos de fragmentação foram propostos: os produtos da degradação do sulfametoxazol, identificados, foram o sulfametoxazol dihidroxilado (identificado apenas após 60 minutos de tratamento) e o sulfametoxazol dihidrogenado. Na aplicação da eletrocoagulação ao efluente hospitalar, fortificado com solução padrão de ambos os antimicrobiais, observou-se que não ocorre degradação destes. Assim sendo, não foi possível estudar-se os produtos da degradação em amostras reais de efluente. O processo de eletrocoagulação aplicado ao efluente hospitalar é eficiente na redução da DQO nas condições avaliadas; mas, não é eficiente na degradação dos antimicrobiais no efluente fortificado. O método desenvolvido, utilizando-se como ferramenta analítica LCMS/ MS_QTrap operando em modo linear, para a determinação dos fármacos investigados, em efluente hospitalar, como também, para a avaliação da eficiência do processo de eletrocoagulação na redução da concentração ou na degradação dos antimicrobiais em solução sintética e, em efluente hospitalar, provou ser rápido, sensível, seletivo, dispensando laboriosa manipulação da amostra.Coordenação de Aperfeiçoamento de Pessoal de Nível Superiorapplication/pdfporUniversidade Federal de Santa MariaPrograma de Pós-Graduação em QuímicaUFSMBRQuímicaQuímicaQuímica analíticaEfluentes hospitalaresMedicamentos antimicrobianosSulfametoxazolTrimetoprimaCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICAAntimicrobiais sulfametoxazol e trimetoprima em efluente hospitalar: determinação, degradação através de eletrocoagulação e identificação de subprodutos e metabólitosSulphamethoxazole and trimethoprim antimicrobials in hospital wastewater: determination, degradation through electrocoagulation and identification of bybproducts and metabolitesinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisMartins, Ayrton Figueiredohttp://lattes.cnpq.br/2113532494494821Zanella, Renatohttp://lattes.cnpq.br/2541865299438479Vasconcelos, Tibiriçá Gonçalveshttp://lattes.cnpq.br/6407925163803842http://lattes.cnpq.br/5204109280070297Brenner, Carla Geane Brandenburg100600000000400500500300300ade6000d-a348-4d49-a531-6500a65a153a8ddfdeac-1966-472a-9110-fbb2275bfbfca5080cbf-61ea-435f-870d-c05ac5884a8af36ad0ab-009d-4071-a573-195334263a37info:eu-repo/semantics/openAccessreponame:Biblioteca Digital de Teses e Dissertações do UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMORIGINALBRENNER, CARLA GEANE BRANDENBURG.pdfapplication/pdf2643924http://repositorio.ufsm.br/bitstream/1/10446/1/BRENNER%2c%20CARLA%20GEANE%20BRANDENBURG.pdf9548f4960faca3d44e49412f6a077286MD51TEXTBRENNER, CARLA GEANE BRANDENBURG.pdf.txtBRENNER, CARLA GEANE BRANDENBURG.pdf.txtExtracted texttext/plain133455http://repositorio.ufsm.br/bitstream/1/10446/2/BRENNER%2c%20CARLA%20GEANE%20BRANDENBURG.pdf.txte9fac8762f0240a527ac65648e846de4MD52THUMBNAILBRENNER, CARLA GEANE BRANDENBURG.pdf.jpgBRENNER, CARLA GEANE BRANDENBURG.pdf.jpgIM Thumbnailimage/jpeg7293http://repositorio.ufsm.br/bitstream/1/10446/3/BRENNER%2c%20CARLA%20GEANE%20BRANDENBURG.pdf.jpg654c953e09e4e4c3794fff74d4508e89MD531/104462023-04-11 16:22:24.056oai:repositorio.ufsm.br:1/10446Biblioteca Digital de Teses e Dissertaçõeshttps://repositorio.ufsm.br/ONGhttps://repositorio.ufsm.br/oai/requestatendimento.sib@ufsm.br||tedebc@gmail.comopendoar:2023-04-11T19:22:24Biblioteca Digital de Teses e Dissertações do UFSM - Universidade Federal de Santa Maria (UFSM)false
dc.title.por.fl_str_mv Antimicrobiais sulfametoxazol e trimetoprima em efluente hospitalar: determinação, degradação através de eletrocoagulação e identificação de subprodutos e metabólitos
dc.title.alternative.eng.fl_str_mv Sulphamethoxazole and trimethoprim antimicrobials in hospital wastewater: determination, degradation through electrocoagulation and identification of bybproducts and metabolites
title Antimicrobiais sulfametoxazol e trimetoprima em efluente hospitalar: determinação, degradação através de eletrocoagulação e identificação de subprodutos e metabólitos
spellingShingle Antimicrobiais sulfametoxazol e trimetoprima em efluente hospitalar: determinação, degradação através de eletrocoagulação e identificação de subprodutos e metabólitos
Brenner, Carla Geane Brandenburg
Química
Química analítica
Efluentes hospitalares
Medicamentos antimicrobianos
Sulfametoxazol
Trimetoprima
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA
title_short Antimicrobiais sulfametoxazol e trimetoprima em efluente hospitalar: determinação, degradação através de eletrocoagulação e identificação de subprodutos e metabólitos
title_full Antimicrobiais sulfametoxazol e trimetoprima em efluente hospitalar: determinação, degradação através de eletrocoagulação e identificação de subprodutos e metabólitos
title_fullStr Antimicrobiais sulfametoxazol e trimetoprima em efluente hospitalar: determinação, degradação através de eletrocoagulação e identificação de subprodutos e metabólitos
title_full_unstemmed Antimicrobiais sulfametoxazol e trimetoprima em efluente hospitalar: determinação, degradação através de eletrocoagulação e identificação de subprodutos e metabólitos
title_sort Antimicrobiais sulfametoxazol e trimetoprima em efluente hospitalar: determinação, degradação através de eletrocoagulação e identificação de subprodutos e metabólitos
author Brenner, Carla Geane Brandenburg
author_facet Brenner, Carla Geane Brandenburg
author_role author
dc.contributor.advisor1.fl_str_mv Martins, Ayrton Figueiredo
dc.contributor.advisor1Lattes.fl_str_mv http://lattes.cnpq.br/2113532494494821
dc.contributor.referee1.fl_str_mv Zanella, Renato
dc.contributor.referee1Lattes.fl_str_mv http://lattes.cnpq.br/2541865299438479
dc.contributor.referee2.fl_str_mv Vasconcelos, Tibiriçá Gonçalves
dc.contributor.referee2Lattes.fl_str_mv http://lattes.cnpq.br/6407925163803842
dc.contributor.authorLattes.fl_str_mv http://lattes.cnpq.br/5204109280070297
dc.contributor.author.fl_str_mv Brenner, Carla Geane Brandenburg
contributor_str_mv Martins, Ayrton Figueiredo
Zanella, Renato
Vasconcelos, Tibiriçá Gonçalves
dc.subject.por.fl_str_mv Química
Química analítica
Efluentes hospitalares
Medicamentos antimicrobianos
Sulfametoxazol
Trimetoprima
topic Química
Química analítica
Efluentes hospitalares
Medicamentos antimicrobianos
Sulfametoxazol
Trimetoprima
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA
dc.subject.cnpq.fl_str_mv CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA
description In this study, it was developed a methodology using liquid chromatography coupled to tandem mass spectrometry for the determination of antimicrobials sulphamethoxazole and trimethoprim in hospital effluent and for monitoring the electrocoagulation process applied to synthetic solutions, as well as, to the hospital effluent fortified with the antimicrobials, both at the same concentration of 1 mg L-1. The achieved limits of detection and quantification were 0.25 and 0.5 μg L-1, respectively. The linear range of the method was 0.5 to 100 μg L-1, with a correlation coefficient always greater than <0.9995 for both antimicrobials. The average concentration of sulphamethoxazole and trimethoprim found for the hospital effluent was 27.8 and 6.6 μg L-1, respectively. In order to study the best conditions for conducting the electrocoagulation, factorial design with surface response methodology was used. It was set as variables the distance of the electrodes, the concentration of electrolyte (NaCl) and the applied current (mA). As evaluation parameter it was used the chemical oxygen demand (COD) reduction of the hospital effluent. The best result for the COD reduction (57.9%) was achieved using 500 mg of NaCl, electrode distance of 30 mm and current of 800 mA. By means of the application of the electrocoagulation process to synthetic solutions of the antimicrobials and Soxhlet extraction, it was confirmed the true degradation or the reduction of the antimicrobial concentration by possible adsorption on the generated process sludge. From the average reduction of 84.7% of the initial sulphamethoxazole concentration, 6.0% of which were adsorbed by the sludge, resulting an average reduction 79.3%, at pH 5 and 7. The antimicrobial trimethoprim, at pH 5 and 7, showed an average reduction of 28.7% of the initial concentration by sludge adsorption, and no degradation occurred. The identification of the metabolites in hospital effluent and the degradation products generated by the electrocoagulation of the synthetic solution was performed using liquid chromatography quadrupole linear ion trap mass spectrometry. The metabolites identified were N4-acetylsulphamethoxazole and dihydroxitrimethoprim, and their paths of fragmentation were proposed. The degradation products of sulfamethoxazole identified were dihydroxyl sulphamethoxazole (identified only after 60 minutes treatment) and dehydrogenate sulphamethoxazole. For the electrocoagulation of the hospital effluent fortified with standard solutions of both antimicrobials, it was observed no degradation. Therefore, the degradation products in real effluent samples could not be studied. The electrocoagulation process applied to the hospital effluent was efficient by reducing COD under the conditions evaluated; but, it was not efficient by the degradation of the fortified antimicrobials in the effluent. The developed methodology used as analytical tool, LC-MS/MS_QTrap operating in lineal way, for the determination of the investigated antimicrobials in hospital wastewater, as well as for the efficiency evaluation of the electrocoagulation process by the concentration reduction or the degradation in synthetic solution and hospital wastewater, proved to be fast, sensitive, selective, sparing laborious manipulation of the sample.
publishDate 2009
dc.date.issued.fl_str_mv 2009-03-03
dc.date.accessioned.fl_str_mv 2017-05-11
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dc.identifier.citation.fl_str_mv BRENNER, Carla Geane Brandenburg. Sulphamethoxazole and trimethoprim antimicrobials in hospital wastewater: determination, degradation through electrocoagulation and identification of bybproducts and metabolites. 2009. 93 f. Dissertação (Mestrado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2009.
dc.identifier.uri.fl_str_mv http://repositorio.ufsm.br/handle/1/10446
identifier_str_mv BRENNER, Carla Geane Brandenburg. Sulphamethoxazole and trimethoprim antimicrobials in hospital wastewater: determination, degradation through electrocoagulation and identification of bybproducts and metabolites. 2009. 93 f. Dissertação (Mestrado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2009.
url http://repositorio.ufsm.br/handle/1/10446
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