Quantificação de cocaína, benzoilecgonina e anidroecgonina em efluente hospitalar e remoção por fotocatálise e eletrocoagulação

Detalhes bibliográficos
Ano de defesa: 2016
Autor(a) principal: Santos, Jeremias Bastos dos lattes
Orientador(a): Martins, Ayrton Figueiredo lattes
Banca de defesa: Silveira, Djalma Dias da lattes, Martins, Manoel Leonardo lattes
Tipo de documento: Dissertação
Tipo de acesso: Acesso aberto
Idioma: por
Instituição de defesa: Universidade Federal de Santa Maria
Centro de Ciências Naturais e Exatas
Programa de Pós-Graduação: Programa de Pós-Graduação em Química
Departamento: Química
País: Brasil
Palavras-chave em Português:
Palavras-chave em Inglês:
Área do conhecimento CNPq:
Link de acesso: 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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spelling 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:Biblioteca Digital de Teses e Dissertações do 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
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