Desenvolvimento de sensor eletroquímico baseado em carbon dots suportados em óxido de grafeno reduzido para determinação de hidroxicloroquina
Autor(a) principal: | |
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Data de Publicação: | 2022 |
Tipo de documento: | Dissertação |
Idioma: | por |
Título da fonte: | Repositório Institucional da UFS |
Texto Completo: | https://ri.ufs.br/jspui/handle/riufs/15692 |
Resumo: | The use of modifiers in carbon paste electrodes (CPE) has been growing every year due to the possibility of improving the performance of the electrode in relation to the selective determination of several analytes. The objective of this work is the development of modified electrodes with a hybrid material based on carbon dots and reduced graphene oxide (CD-rGO), which has a low cost of preparation, high sensitivity, and fast response for the determination of hydroxychloroquine. Graphene oxide (GO) was synthesized by the modified Hummer’s method under mild conditions and reduced with L-ascorbic acid to obtain reduced graphene oxide (rGO), then the carbon dots were synthesized in situ, on rGO matrix, using urea and glucose as precursors, by a hydrothermal route at 180 °C for 5 hours. The hybrid material obtained was characterized using scanning electron microscopy (SEM), fluorescence emission spectroscopy (PL), molecular absorption in the ultravioletvisible region (UV-Vis), Raman and vibrational spectroscopy in the Fourier-transform infrared spectroscopy (FTIR), and x-ray diffractometry (XRD). After the characterizations of CD-rGO, the modified carbon paste electrode (ECO) was applied to the voltammetric determination of commercial hydroxychloroquine tablets and synthetic urine. Parameters such as electrolyte medium, ECO composition, and parameters of differential pulse voltammetry technique were optimized and the electrochemical characterization showed that the ECO electrode has higher sensitivity in the hydroxychloroquine determination than CPE. The optimizations of the parameters of the electrolyte medium and the VPD technique resulted in a significant current gain for the analytical signal of HCQ. With the development of the analytical curve, the limits of detection (LOD) and quantification (LOQ) of 2.40 pmol∙L-1 and 7.99 pmol∙L-1 , respectively, were obtained in a linear response range of 19.90 to 138 pmol∙L-1 and the precision of the developed method showed satisfactory results of repeatability and reproducibility, presenting recoveries between 101.55 and 106.83 %, enabling the use of the ECO as an electrochemical sensor for hydroxychloroquine determination. |
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Santos Junior, José Carlos dosSussuchi, Eliana MidoriRodrigues, Marcelo Oliveira2022-05-12T21:13:03Z2022-05-12T21:13:03Z2022-01-28SANTOS JUNIOR, José Carlos dos. Desenvolvimento de sensor eletroquímico baseado em carbon dots suportados em óxido de grafeno reduzido para determinação de hidroxicloroquina. 2022. 93 f. Dissertação (Mestrado em Química) - Universidade Federal de Sergipe, São Cristóvão, 2022.https://ri.ufs.br/jspui/handle/riufs/15692The use of modifiers in carbon paste electrodes (CPE) has been growing every year due to the possibility of improving the performance of the electrode in relation to the selective determination of several analytes. The objective of this work is the development of modified electrodes with a hybrid material based on carbon dots and reduced graphene oxide (CD-rGO), which has a low cost of preparation, high sensitivity, and fast response for the determination of hydroxychloroquine. Graphene oxide (GO) was synthesized by the modified Hummer’s method under mild conditions and reduced with L-ascorbic acid to obtain reduced graphene oxide (rGO), then the carbon dots were synthesized in situ, on rGO matrix, using urea and glucose as precursors, by a hydrothermal route at 180 °C for 5 hours. The hybrid material obtained was characterized using scanning electron microscopy (SEM), fluorescence emission spectroscopy (PL), molecular absorption in the ultravioletvisible region (UV-Vis), Raman and vibrational spectroscopy in the Fourier-transform infrared spectroscopy (FTIR), and x-ray diffractometry (XRD). After the characterizations of CD-rGO, the modified carbon paste electrode (ECO) was applied to the voltammetric determination of commercial hydroxychloroquine tablets and synthetic urine. Parameters such as electrolyte medium, ECO composition, and parameters of differential pulse voltammetry technique were optimized and the electrochemical characterization showed that the ECO electrode has higher sensitivity in the hydroxychloroquine determination than CPE. The optimizations of the parameters of the electrolyte medium and the VPD technique resulted in a significant current gain for the analytical signal of HCQ. With the development of the analytical curve, the limits of detection (LOD) and quantification (LOQ) of 2.40 pmol∙L-1 and 7.99 pmol∙L-1 , respectively, were obtained in a linear response range of 19.90 to 138 pmol∙L-1 and the precision of the developed method showed satisfactory results of repeatability and reproducibility, presenting recoveries between 101.55 and 106.83 %, enabling the use of the ECO as an electrochemical sensor for hydroxychloroquine determination.O uso de modificadores em eletrodos de pasta de carbono (EPC) vem crescendo a cada ano, devido à possibilidade de melhorar o desempenho do eletrodo em relação a determinação seletiva de diversos analitos. O objetivo deste trabalho é o desenvolvimento de eletrodos modificados com um material híbrido baseado em carbon dots e óxido de grafeno reduzido (CD-OGr), que possua um baixo custo de preparação, alta sensibilidade e rápida resposta para detecção de hidroxicloroquina. O óxido de grafeno (OG) foi sintetizado pelo método de Hummers modificado, em condições brandas, e reduzido com ácido L-ascórbico para obtenção do óxido de grafeno reduzido (OGr), em seguida os carbon dots foram sintetizados in situ, em matriz de OGr, utilizando como precursores ureia e glicose, por rota hidrotermal a 180 °C por 5 horas. O material híbrido obtido foi caracterizado usando microscopia eletrônica de varredura (MEV), espectroscopia de emissão fluorescente (PL), de absorção molecular na região do ultravioleta-visível (UV-Vis), espetroscopia Raman e vibracional na região do infravermelho por transformada de Fourier (FTIR) além de difratometria de raios x (DRX). Após as caracterizações do CD-OGr o eletrodo de pasta de carbono modificado (ECO) foi aplicado na determinação voltamétrica de hidroxicloroquina em comprimidos comerciais e urina sintética. Os parâmetros como meio eletrolítico, composição do ECO e parâmetros da técnica de voltametria de pulso diferencial, foram otimizados e a caracterização eletroquímica mostrou que o eletrodo ECO apresentou maior sensibilidade na determinação de hidroxicloroquina que o EPC. As otimizações dos parâmetros do meio eletrolítico e da técnica de VPD resultaram em um ganho de corrente expressivo para o sinal analítico da HCQ. Com o desenvolvimento da curva analítica obteve-se os limites de detecção (LD) e quantificação (LQ) de 2,40 pmol∙L-1 e 7,99 pmol∙L-1 , respectivamente, em um intervalo de resposta linear de 19,90 a 138 pmol∙L -1 e a precisão do método desenvolvido mostrou resultados satisfatórios de repetibilidade e reprodutibilidade, apresentando recuperações de 101,55 a 106,83 %, possibilitando o uso do ECO como sensor eletroquímico para a determinação de hidroxicloroquina.Coordenação de Aperfeiçoamento de Pessoal de Nível Superior - CAPESSão CristóvãoporQuímicaGrafenoCloroquinaCovid-19 (Doença)Carbon dotsHidroxicloroquinaGrapheneCarbon dotsHydroxychloroquineCIENCIAS EXATAS E DA TERRA::QUIMICADesenvolvimento de sensor eletroquímico baseado em carbon dots suportados em óxido de grafeno reduzido para determinação de hidroxicloroquinaDevelopment of electrochemical sensor based on carbon dots suported on reduced graphene oxide for hydroxychloroquine determinationinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisPós-Graduação em QuímicaUniversidade Federal de Sergipereponame:Repositório Institucional da UFSinstname:Universidade Federal de Sergipe (UFS)instacron:UFSinfo:eu-repo/semantics/openAccessLICENSElicense.txtlicense.txttext/plain; charset=utf-81475https://ri.ufs.br/jspui/bitstream/riufs/15692/1/license.txt098cbbf65c2c15e1fb2e49c5d306a44cMD51TEXTJOSE_CARLOS_SANTOS_JUNIOR.pdf.txtJOSE_CARLOS_SANTOS_JUNIOR.pdf.txtExtracted texttext/plain144396https://ri.ufs.br/jspui/bitstream/riufs/15692/3/JOSE_CARLOS_SANTOS_JUNIOR.pdf.txt82e768c7ced98ea568e9c1e1514aaebeMD53THUMBNAILJOSE_CARLOS_SANTOS_JUNIOR.pdf.jpgJOSE_CARLOS_SANTOS_JUNIOR.pdf.jpgGenerated Thumbnailimage/jpeg1476https://ri.ufs.br/jspui/bitstream/riufs/15692/4/JOSE_CARLOS_SANTOS_JUNIOR.pdf.jpgd22228c025815ea5f4aa5ab5e1154890MD54ORIGINALJOSE_CARLOS_SANTOS_JUNIOR.pdfJOSE_CARLOS_SANTOS_JUNIOR.pdfapplication/pdf2683385https://ri.ufs.br/jspui/bitstream/riufs/15692/5/JOSE_CARLOS_SANTOS_JUNIOR.pdf225cba79a44c12caa0023d7fc7b954f1MD55riufs/156922022-05-16 16:26:22.691oai:ufs.br:riufs/15692TElDRU7Dh0EgREUgRElTVFJJQlVJw4fDg08gTsODTy1FWENMVVNJVkEKCkNvbSBhIGFwcmVzZW50YcOnw6NvIGRlc3RhIGxpY2Vuw6dhLCB2b2PDqiAobyBhdXRvcihlcykgb3UgbyB0aXR1bGFyIGRvcyBkaXJlaXRvcyBkZSBhdXRvcikgY29uY2VkZSDDoCBVbml2ZXJzaWRhZGUgRmVkZXJhbCBkZSBTZXJnaXBlIG8gZGlyZWl0byBuw6NvLWV4Y2x1c2l2byBkZSByZXByb2R1emlyIHNldSB0cmFiYWxobyBubyBmb3JtYXRvIGVsZXRyw7RuaWNvLCBpbmNsdWluZG8gb3MgZm9ybWF0b3Mgw6F1ZGlvIG91IHbDrWRlby4KClZvY8OqIGNvbmNvcmRhIHF1ZSBhIFVuaXZlcnNpZGFkZSBGZWRlcmFsIGRlIFNlcmdpcGUgcG9kZSwgc2VtIGFsdGVyYXIgbyBjb250ZcO6ZG8sIHRyYW5zcG9yIHNldSB0cmFiYWxobyBwYXJhIHF1YWxxdWVyIG1laW8gb3UgZm9ybWF0byBwYXJhIGZpbnMgZGUgcHJlc2VydmHDp8Ojby4KClZvY8OqIHRhbWLDqW0gY29uY29yZGEgcXVlIGEgVW5pdmVyc2lkYWRlIEZlZGVyYWwgZGUgU2VyZ2lwZSBwb2RlIG1hbnRlciBtYWlzIGRlIHVtYSBjw7NwaWEgZGUgc2V1IHRyYWJhbGhvIHBhcmEgZmlucyBkZSBzZWd1cmFuw6dhLCBiYWNrLXVwIGUgcHJlc2VydmHDp8Ojby4KClZvY8OqIGRlY2xhcmEgcXVlIHNldSB0cmFiYWxobyDDqSBvcmlnaW5hbCBlIHF1ZSB2b2PDqiB0ZW0gbyBwb2RlciBkZSBjb25jZWRlciBvcyBkaXJlaXRvcyBjb250aWRvcyBuZXN0YSBsaWNlbsOnYS4gVm9jw6ogdGFtYsOpbSBkZWNsYXJhIHF1ZSBvIGRlcMOzc2l0bywgcXVlIHNlamEgZGUgc2V1IGNvbmhlY2ltZW50bywgbsOjbyBpbmZyaW5nZSBkaXJlaXRvcyBhdXRvcmFpcyBkZSBuaW5ndcOpbS4KCkNhc28gbyB0cmFiYWxobyBjb250ZW5oYSBtYXRlcmlhbCBxdWUgdm9jw6ogbsOjbyBwb3NzdWkgYSB0aXR1bGFyaWRhZGUgZG9zIGRpcmVpdG9zIGF1dG9yYWlzLCB2b2PDqiBkZWNsYXJhIHF1ZSBvYnRldmUgYSBwZXJtaXNzw6NvIGlycmVzdHJpdGEgZG8gZGV0ZW50b3IgZG9zIGRpcmVpdG9zIGF1dG9yYWlzIHBhcmEgY29uY2VkZXIgw6AgVW5pdmVyc2lkYWRlIEZlZGVyYWwgZGUgU2VyZ2lwZSBvcyBkaXJlaXRvcyBhcHJlc2VudGFkb3MgbmVzdGEgbGljZW7Dp2EsIGUgcXVlIGVzc2UgbWF0ZXJpYWwgZGUgcHJvcHJpZWRhZGUgZGUgdGVyY2Vpcm9zIGVzdMOhIGNsYXJhbWVudGUgaWRlbnRpZmljYWRvIGUgcmVjb25oZWNpZG8gbm8gdGV4dG8gb3Ugbm8gY29udGXDumRvLgoKQSBVbml2ZXJzaWRhZGUgRmVkZXJhbCBkZSBTZXJnaXBlIHNlIGNvbXByb21ldGUgYSBpZGVudGlmaWNhciBjbGFyYW1lbnRlIG8gc2V1IG5vbWUocykgb3UgbyhzKSBub21lKHMpIGRvKHMpIApkZXRlbnRvcihlcykgZG9zIGRpcmVpdG9zIGF1dG9yYWlzIGRvIHRyYWJhbGhvLCBlIG7Do28gZmFyw6EgcXVhbHF1ZXIgYWx0ZXJhw6fDo28sIGFsw6ltIGRhcXVlbGFzIGNvbmNlZGlkYXMgcG9yIGVzdGEgbGljZW7Dp2EuIAo=Repositório InstitucionalPUBhttps://ri.ufs.br/oai/requestrepositorio@academico.ufs.bropendoar:2022-05-16T19:26:22Repositório Institucional da UFS - Universidade Federal de Sergipe (UFS)false |
dc.title.pt_BR.fl_str_mv |
Desenvolvimento de sensor eletroquímico baseado em carbon dots suportados em óxido de grafeno reduzido para determinação de hidroxicloroquina |
dc.title.alternative.por.fl_str_mv |
Development of electrochemical sensor based on carbon dots suported on reduced graphene oxide for hydroxychloroquine determination |
title |
Desenvolvimento de sensor eletroquímico baseado em carbon dots suportados em óxido de grafeno reduzido para determinação de hidroxicloroquina |
spellingShingle |
Desenvolvimento de sensor eletroquímico baseado em carbon dots suportados em óxido de grafeno reduzido para determinação de hidroxicloroquina Santos Junior, José Carlos dos Química Grafeno Cloroquina Covid-19 (Doença) Carbon dots Hidroxicloroquina Graphene Carbon dots Hydroxychloroquine CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Desenvolvimento de sensor eletroquímico baseado em carbon dots suportados em óxido de grafeno reduzido para determinação de hidroxicloroquina |
title_full |
Desenvolvimento de sensor eletroquímico baseado em carbon dots suportados em óxido de grafeno reduzido para determinação de hidroxicloroquina |
title_fullStr |
Desenvolvimento de sensor eletroquímico baseado em carbon dots suportados em óxido de grafeno reduzido para determinação de hidroxicloroquina |
title_full_unstemmed |
Desenvolvimento de sensor eletroquímico baseado em carbon dots suportados em óxido de grafeno reduzido para determinação de hidroxicloroquina |
title_sort |
Desenvolvimento de sensor eletroquímico baseado em carbon dots suportados em óxido de grafeno reduzido para determinação de hidroxicloroquina |
author |
Santos Junior, José Carlos dos |
author_facet |
Santos Junior, José Carlos dos |
author_role |
author |
dc.contributor.author.fl_str_mv |
Santos Junior, José Carlos dos |
dc.contributor.advisor1.fl_str_mv |
Sussuchi, Eliana Midori |
dc.contributor.advisor-co1.fl_str_mv |
Rodrigues, Marcelo Oliveira |
contributor_str_mv |
Sussuchi, Eliana Midori Rodrigues, Marcelo Oliveira |
dc.subject.por.fl_str_mv |
Química Grafeno Cloroquina Covid-19 (Doença) Carbon dots Hidroxicloroquina |
topic |
Química Grafeno Cloroquina Covid-19 (Doença) Carbon dots Hidroxicloroquina Graphene Carbon dots Hydroxychloroquine CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.eng.fl_str_mv |
Graphene Carbon dots Hydroxychloroquine |
dc.subject.cnpq.fl_str_mv |
CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
The use of modifiers in carbon paste electrodes (CPE) has been growing every year due to the possibility of improving the performance of the electrode in relation to the selective determination of several analytes. The objective of this work is the development of modified electrodes with a hybrid material based on carbon dots and reduced graphene oxide (CD-rGO), which has a low cost of preparation, high sensitivity, and fast response for the determination of hydroxychloroquine. Graphene oxide (GO) was synthesized by the modified Hummer’s method under mild conditions and reduced with L-ascorbic acid to obtain reduced graphene oxide (rGO), then the carbon dots were synthesized in situ, on rGO matrix, using urea and glucose as precursors, by a hydrothermal route at 180 °C for 5 hours. The hybrid material obtained was characterized using scanning electron microscopy (SEM), fluorescence emission spectroscopy (PL), molecular absorption in the ultravioletvisible region (UV-Vis), Raman and vibrational spectroscopy in the Fourier-transform infrared spectroscopy (FTIR), and x-ray diffractometry (XRD). After the characterizations of CD-rGO, the modified carbon paste electrode (ECO) was applied to the voltammetric determination of commercial hydroxychloroquine tablets and synthetic urine. Parameters such as electrolyte medium, ECO composition, and parameters of differential pulse voltammetry technique were optimized and the electrochemical characterization showed that the ECO electrode has higher sensitivity in the hydroxychloroquine determination than CPE. The optimizations of the parameters of the electrolyte medium and the VPD technique resulted in a significant current gain for the analytical signal of HCQ. With the development of the analytical curve, the limits of detection (LOD) and quantification (LOQ) of 2.40 pmol∙L-1 and 7.99 pmol∙L-1 , respectively, were obtained in a linear response range of 19.90 to 138 pmol∙L-1 and the precision of the developed method showed satisfactory results of repeatability and reproducibility, presenting recoveries between 101.55 and 106.83 %, enabling the use of the ECO as an electrochemical sensor for hydroxychloroquine determination. |
publishDate |
2022 |
dc.date.accessioned.fl_str_mv |
2022-05-12T21:13:03Z |
dc.date.available.fl_str_mv |
2022-05-12T21:13:03Z |
dc.date.issued.fl_str_mv |
2022-01-28 |
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.citation.fl_str_mv |
SANTOS JUNIOR, José Carlos dos. Desenvolvimento de sensor eletroquímico baseado em carbon dots suportados em óxido de grafeno reduzido para determinação de hidroxicloroquina. 2022. 93 f. Dissertação (Mestrado em Química) - Universidade Federal de Sergipe, São Cristóvão, 2022. |
dc.identifier.uri.fl_str_mv |
https://ri.ufs.br/jspui/handle/riufs/15692 |
identifier_str_mv |
SANTOS JUNIOR, José Carlos dos. Desenvolvimento de sensor eletroquímico baseado em carbon dots suportados em óxido de grafeno reduzido para determinação de hidroxicloroquina. 2022. 93 f. Dissertação (Mestrado em Química) - Universidade Federal de Sergipe, São Cristóvão, 2022. |
url |
https://ri.ufs.br/jspui/handle/riufs/15692 |
dc.language.iso.fl_str_mv |
por |
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por |
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info:eu-repo/semantics/openAccess |
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openAccess |
dc.publisher.program.fl_str_mv |
Pós-Graduação em Química |
dc.publisher.initials.fl_str_mv |
Universidade Federal de Sergipe |
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