Quantificação de cocaína, benzoilecgonina e anidroecgonina em efluente hospitalar e remoção por fotocatálise e eletrocoagulação
Autor(a) principal: | |
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Data de Publicação: | 2016 |
Tipo de documento: | Dissertação |
Idioma: | por |
Título da fonte: | Repositório Institucional Manancial UFSM |
Texto Completo: | http://repositorio.ufsm.br/handle/1/17654 |
Resumo: | In this work we studied an analytical method for identification and quantification of cocaine (COC), benzoylecgonine (BEG) and anidroecgonina (AEG) in effluent samples from the University Hospital of the Federal University of Santa Maria (HUSM). Solid phase extraction (SPE) and dispersive liquid-liquid microextraction (DLLME) were used for extraction and determination of cocaine and its metabolites in the analyzed samples. For SPE we used Chromabond C18® ec 6 ml/500 mg cartridge, yielding recoveries ranging from 73.5% ± 6.3% to 85.0% ± 8.7% in aqueous solution; for the effluent samples, recoveries exceeding 78.0% were obtained when spiked for COC at 15.8 μg L-1 and 195.0 μg L-1; for BEG, at 18.8 μg L-1 and 198.0 μg L-1, and, for AEG, at 30.9 μg L-1 and 210.0 μg L-1. For DLLME we tested different combinations and volumes of solvent extractor/disperser, pH, interaction and extraction times. The best combination of the extraction solvents was of methanol and chloroform at pH 9, adding 0.3 mol L-1 NaCl, 150/350 μL-1 solvent extractor/disperser, resulting in recoveries for COC, in aqueous solution and hospital effluent, ranging from 73.5% to 102.0% (RSD 6.0% and 16.5%). The concentrations found in the HUSM effluent were 2.01 μg L-1 (RSD17.8%) for COC and 1.89 μg L-1 (RSD18.5%) for BEG, which suggests the use of narcotics by patients and/or hospital goers. In order to remove the analytes we applied heterogeneous photocatalysis, using stirred tank reactor fitted with a thermostatic jacket and TiO2 catalyst supported by polydimethylsiloxane (PDMS) bars.Ultraviolet irradiation was carried out with medium pressure mercury vapor lamp (125 W and 401 W m-2). COC and BEG degradation of 97.0% and 93.0% occurred at pH 7 and 40 °C, respectively, after 60 min of irradiation; for the degradation of AEG, the best degradation rate (32,5%) was obtained at pH 5 and 25 °C in aqueous solution; for hospital effluent, the best conditions for the degradation of COC, BEG and AEG were at pH 7 and 30 ° C with degradation rates of 61.0%, 60.0% and 75.0%, respectively. For electrochemical removal of the analytes we used a glass reactor equipped with two pairs of aluminum electrodes with adjustable distance between electrodes, voltage supply reducer, digital multimeter, rheostat and constant stirring. We observed removals of 86.0% and 91.0% for COC and BEG, respectively, for the aqueous solution at pH 3 with the addition of 0.2 mol L-1 NaCl and distance of 6 cm between electrodes. For the hospital effluent best conditions were at pH 7.0, addition of 0.2 mol L-1 NaCl and distance of 10 cm between electrodes, resulting in removals of 72.0% and 88.0% for COC and BEG, respectively. The average concentration of COC and BEG found in the effluent presented low potential environmental impact. |
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2019-07-31T19:25:14Z2019-07-31T19:25:14Z2016-02-29http://repositorio.ufsm.br/handle/1/17654In this work we studied an analytical method for identification and quantification of cocaine (COC), benzoylecgonine (BEG) and anidroecgonina (AEG) in effluent samples from the University Hospital of the Federal University of Santa Maria (HUSM). Solid phase extraction (SPE) and dispersive liquid-liquid microextraction (DLLME) were used for extraction and determination of cocaine and its metabolites in the analyzed samples. For SPE we used Chromabond C18® ec 6 ml/500 mg cartridge, yielding recoveries ranging from 73.5% ± 6.3% to 85.0% ± 8.7% in aqueous solution; for the effluent samples, recoveries exceeding 78.0% were obtained when spiked for COC at 15.8 μg L-1 and 195.0 μg L-1; for BEG, at 18.8 μg L-1 and 198.0 μg L-1, and, for AEG, at 30.9 μg L-1 and 210.0 μg L-1. For DLLME we tested different combinations and volumes of solvent extractor/disperser, pH, interaction and extraction times. The best combination of the extraction solvents was of methanol and chloroform at pH 9, adding 0.3 mol L-1 NaCl, 150/350 μL-1 solvent extractor/disperser, resulting in recoveries for COC, in aqueous solution and hospital effluent, ranging from 73.5% to 102.0% (RSD 6.0% and 16.5%). The concentrations found in the HUSM effluent were 2.01 μg L-1 (RSD17.8%) for COC and 1.89 μg L-1 (RSD18.5%) for BEG, which suggests the use of narcotics by patients and/or hospital goers. In order to remove the analytes we applied heterogeneous photocatalysis, using stirred tank reactor fitted with a thermostatic jacket and TiO2 catalyst supported by polydimethylsiloxane (PDMS) bars.Ultraviolet irradiation was carried out with medium pressure mercury vapor lamp (125 W and 401 W m-2). COC and BEG degradation of 97.0% and 93.0% occurred at pH 7 and 40 °C, respectively, after 60 min of irradiation; for the degradation of AEG, the best degradation rate (32,5%) was obtained at pH 5 and 25 °C in aqueous solution; for hospital effluent, the best conditions for the degradation of COC, BEG and AEG were at pH 7 and 30 ° C with degradation rates of 61.0%, 60.0% and 75.0%, respectively. For electrochemical removal of the analytes we used a glass reactor equipped with two pairs of aluminum electrodes with adjustable distance between electrodes, voltage supply reducer, digital multimeter, rheostat and constant stirring. We observed removals of 86.0% and 91.0% for COC and BEG, respectively, for the aqueous solution at pH 3 with the addition of 0.2 mol L-1 NaCl and distance of 6 cm between electrodes. For the hospital effluent best conditions were at pH 7.0, addition of 0.2 mol L-1 NaCl and distance of 10 cm between electrodes, resulting in removals of 72.0% and 88.0% for COC and BEG, respectively. The average concentration of COC and BEG found in the effluent presented low potential environmental impact.Neste trabalho foi estudado método analítico para identificação e quantificação de cocaína (COC), benzoilecgonina (BEG) e anidroecgonina (AEG) em amostras de efluente do Hospital Universitário de Santa Maria (HUSM). Utilizou-se Cromatografia Líquida de Alta Eficiência com detecção por Fluorescência (HPLC-FLD) e Arranjo de Diodos (HPLC-DAD). Extração em Fase Sólida (SPE) e Microextração Líquido-Líquido Dispersiva (DLLME) foram empregadas para a extração e a determinação de cocaína e seus metabólitos nas amostras investigadas. Para a SPE foi utilizado cartucho Chromabond® C18 ec 6 ml/500 mg, obtendo-se recuperações variando entre 73,5% ± 6,3% e 85,0% ± 8,7%, em solução aquosa; para amostra de efluente se obteve recuperações superiores a 78,0% quando fortificada para COC em 15, 8 μg L-1 e 195,0 μg L-1, para BEG em 18,8 μg L-1 e 198,0 μg L-1 e, para a AEG, 30, 9 μg L-1 e 210,0 μg L-1. Para a DLLME foram testadas diferentes combinações e volumes de solvente extrator/dispersor, pH, tempos de interação e extração. A melhor combinação foi dos solventes metanol e clorofórmio, pH 9, adição de 0,3 mol L-1 de NaCl, 150/350 μL-1 de solventes extrator/dispersor, obtendo-se recuperações para COC, em solução aquosa e em efluente hospitalar, na faixa de 73-102% (DPR 6,0% e 16,5%). As concentrações de COC encontradas no efluente do HUSM foram de 2,01 μg L-1 (DPR 17,8%) e, de BEG, 1,89 μg L-1 (DPR 18,5%), o que sugere uso de entorpecente por frequentadores do HUSM. Como processo para a remoção dos analitos foi aplicada a fotocatálise heterogênea usando-se reator tanque agitado, provido de jaqueta termostática, e catalisador TiO2 suportado em barras de polidimetilsiloxano (PDMS). A irradiação ultravioleta (UV) foi feita com lâmpada de vapor de mercúrio de pressão média (125 W e 401 W m-2). Em pH 7 e a 40 °C obteve-se degradação de COC e BEG, de 97,0% e 93,0%, respectivamente, após 60 min de irradiação; e, para a degradação da AEG, a melhor taxa de degradação (32,5%) foi obtida com pH 5 e a 25 °C, em solução aquosa; em efluente hospitalar, as melhores condições para a degradação de COC, BEG e AEG foram pH 7 e 30 °C, com taxas de degradação de 61,0%, 60,0% e 75,0%, respectivamente. Para a remoção eletroquímica dos analitos foi utilizado reator de vidro provido de dois pares de eletrodos de alumínio com distância intereletrodo ajustável, fonte redutora de tensão, multímetro digital, reostato e agitação constante. Para solução aquosa em pH 3, com adição de 0,2 mol L-1de NaCl e distância intereletrodos de 6 cm foram obtidas remoções de 86,0% e 91,0% para COC e BEG, respectivamente. Para o efluente hospitalar foram empregadas como melhores condições pH 7,0, adição de 0,2 mol L-1de NaCl e distância intereletrodos de 10 cm, obtendo-se remoção de 72,0% e 88,0% para COC e BEG, respectivamente. A concentração média de COC e BEG encontradas no efluente apresentam baixo potencial de impacto ambiental.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/openAccessCocaínaDroga de abusoEfluente hospitalarFotocatálise heterogêneaEletrocoagulaçãoMicroextração dispersiva líquido-líquidoHeterogeneous photocatalysisCocaineDrug abuseHospital effluentElectrocoagulationDispersive liquid-liquid microextractionCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICAQuantificação de cocaína, benzoilecgonina e anidroecgonina em efluente hospitalar e remoção por fotocatálise e eletrocoagulaçãoQuantification of cocaine, benzoylecgonine and anidroecgonina in effluent hospital and removal by photocatalysis and electrocoagulationinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisMartins, Ayrton Figueiredohttp://lattes.cnpq.br/2113532494494821Silveira, Djalma Dias dahttp://lattes.cnpq.br/1988016337388120Martins, Manoel Leonardohttp://lattes.cnpq.br/4404290090180984http://lattes.cnpq.br/5810284131463109Santos, Jeremias Bastos dos100600000000600ade6000d-a348-4d49-a531-6500a65a153aa8b093f1-d31f-48a2-ad9e-f645c59c56f85391f7fd-6a7e-4287-8d99-962b76326f4772f05bf0-a74b-4221-b1e1-573a89d1841ereponame:Repositório Institucional Manancial UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMORIGINALDIS_PPGQUIMICA_2016_SANTOS_JEREMIAS.pdfDIS_PPGQUIMICA_2016_SANTOS_JEREMIAS.pdfDissertação de Mestradoapplication/pdf2083200http://repositorio.ufsm.br/bitstream/1/17654/1/DIS_PPGQUIMICA_2016_SANTOS_JEREMIAS.pdff682d79508c41083b7ebe5ed7f6f5ad4MD51CC-LICENSElicense_rdflicense_rdfapplication/rdf+xml; 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dc.title.por.fl_str_mv |
Quantificação de cocaína, benzoilecgonina e anidroecgonina em efluente hospitalar e remoção por fotocatálise e eletrocoagulação |
dc.title.alternative.eng.fl_str_mv |
Quantification of cocaine, benzoylecgonine and anidroecgonina in effluent hospital and removal by photocatalysis and electrocoagulation |
title |
Quantificação de cocaína, benzoilecgonina e anidroecgonina em efluente hospitalar e remoção por fotocatálise e eletrocoagulação |
spellingShingle |
Quantificação de cocaína, benzoilecgonina e anidroecgonina em efluente hospitalar e remoção por fotocatálise e eletrocoagulação Santos, Jeremias Bastos dos Cocaína Droga de abuso Efluente hospitalar Fotocatálise heterogênea Eletrocoagulação Microextração dispersiva líquido-líquido Heterogeneous photocatalysis Cocaine Drug abuse Hospital effluent Electrocoagulation Dispersive liquid-liquid microextraction CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Quantificação de cocaína, benzoilecgonina e anidroecgonina em efluente hospitalar e remoção por fotocatálise e eletrocoagulação |
title_full |
Quantificação de cocaína, benzoilecgonina e anidroecgonina em efluente hospitalar e remoção por fotocatálise e eletrocoagulação |
title_fullStr |
Quantificação de cocaína, benzoilecgonina e anidroecgonina em efluente hospitalar e remoção por fotocatálise e eletrocoagulação |
title_full_unstemmed |
Quantificação de cocaína, benzoilecgonina e anidroecgonina em efluente hospitalar e remoção por fotocatálise e eletrocoagulação |
title_sort |
Quantificação de cocaína, benzoilecgonina e anidroecgonina em efluente hospitalar e remoção por fotocatálise e eletrocoagulação |
author |
Santos, Jeremias Bastos dos |
author_facet |
Santos, Jeremias Bastos dos |
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 |
Silveira, Djalma Dias da |
dc.contributor.referee1Lattes.fl_str_mv |
http://lattes.cnpq.br/1988016337388120 |
dc.contributor.referee2.fl_str_mv |
Martins, Manoel Leonardo |
dc.contributor.referee2Lattes.fl_str_mv |
http://lattes.cnpq.br/4404290090180984 |
dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/5810284131463109 |
dc.contributor.author.fl_str_mv |
Santos, Jeremias Bastos dos |
contributor_str_mv |
Martins, Ayrton Figueiredo Silveira, Djalma Dias da Martins, Manoel Leonardo |
dc.subject.por.fl_str_mv |
Cocaína Droga de abuso Efluente hospitalar Fotocatálise heterogênea Eletrocoagulação Microextração dispersiva líquido-líquido Heterogeneous photocatalysis |
topic |
Cocaína Droga de abuso Efluente hospitalar Fotocatálise heterogênea Eletrocoagulação Microextração dispersiva líquido-líquido Heterogeneous photocatalysis Cocaine Drug abuse Hospital effluent Electrocoagulation Dispersive liquid-liquid microextraction CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.eng.fl_str_mv |
Cocaine Drug abuse Hospital effluent Electrocoagulation Dispersive liquid-liquid microextraction |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
In this work we studied an analytical method for identification and quantification of cocaine (COC), benzoylecgonine (BEG) and anidroecgonina (AEG) in effluent samples from the University Hospital of the Federal University of Santa Maria (HUSM). Solid phase extraction (SPE) and dispersive liquid-liquid microextraction (DLLME) were used for extraction and determination of cocaine and its metabolites in the analyzed samples. For SPE we used Chromabond C18® ec 6 ml/500 mg cartridge, yielding recoveries ranging from 73.5% ± 6.3% to 85.0% ± 8.7% in aqueous solution; for the effluent samples, recoveries exceeding 78.0% were obtained when spiked for COC at 15.8 μg L-1 and 195.0 μg L-1; for BEG, at 18.8 μg L-1 and 198.0 μg L-1, and, for AEG, at 30.9 μg L-1 and 210.0 μg L-1. For DLLME we tested different combinations and volumes of solvent extractor/disperser, pH, interaction and extraction times. The best combination of the extraction solvents was of methanol and chloroform at pH 9, adding 0.3 mol L-1 NaCl, 150/350 μL-1 solvent extractor/disperser, resulting in recoveries for COC, in aqueous solution and hospital effluent, ranging from 73.5% to 102.0% (RSD 6.0% and 16.5%). The concentrations found in the HUSM effluent were 2.01 μg L-1 (RSD17.8%) for COC and 1.89 μg L-1 (RSD18.5%) for BEG, which suggests the use of narcotics by patients and/or hospital goers. In order to remove the analytes we applied heterogeneous photocatalysis, using stirred tank reactor fitted with a thermostatic jacket and TiO2 catalyst supported by polydimethylsiloxane (PDMS) bars.Ultraviolet irradiation was carried out with medium pressure mercury vapor lamp (125 W and 401 W m-2). COC and BEG degradation of 97.0% and 93.0% occurred at pH 7 and 40 °C, respectively, after 60 min of irradiation; for the degradation of AEG, the best degradation rate (32,5%) was obtained at pH 5 and 25 °C in aqueous solution; for hospital effluent, the best conditions for the degradation of COC, BEG and AEG were at pH 7 and 30 ° C with degradation rates of 61.0%, 60.0% and 75.0%, respectively. For electrochemical removal of the analytes we used a glass reactor equipped with two pairs of aluminum electrodes with adjustable distance between electrodes, voltage supply reducer, digital multimeter, rheostat and constant stirring. We observed removals of 86.0% and 91.0% for COC and BEG, respectively, for the aqueous solution at pH 3 with the addition of 0.2 mol L-1 NaCl and distance of 6 cm between electrodes. For the hospital effluent best conditions were at pH 7.0, addition of 0.2 mol L-1 NaCl and distance of 10 cm between electrodes, resulting in removals of 72.0% and 88.0% for COC and BEG, respectively. The average concentration of COC and BEG found in the effluent presented low potential environmental impact. |
publishDate |
2016 |
dc.date.issued.fl_str_mv |
2016-02-29 |
dc.date.accessioned.fl_str_mv |
2019-07-31T19:25:14Z |
dc.date.available.fl_str_mv |
2019-07-31T19:25:14Z |
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/1/17654 |
url |
http://repositorio.ufsm.br/handle/1/17654 |
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 |
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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:Repositório Institucional Manancial UFSM instname:Universidade Federal de Santa Maria (UFSM) instacron:UFSM |
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Universidade Federal de Santa Maria (UFSM) |
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UFSM |
institution |
UFSM |
reponame_str |
Repositório Institucional Manancial UFSM |
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Repositório Institucional Manancial UFSM |
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MD5 MD5 MD5 MD5 MD5 |
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Repositório Institucional Manancial UFSM - Universidade Federal de Santa Maria (UFSM) |
repository.mail.fl_str_mv |
ouvidoria@ufsm.br |
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