Desenvolvimento de procedimentos eletroanalíticos para a determinação de fármacos em formulações farmacêuticas e fluidos biológicos empregando sensores à base de carbon black
Autor(a) principal: | |
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Data de Publicação: | 2019 |
Tipo de documento: | Dissertação |
Idioma: | por |
Título da fonte: | Repositório Institucional da UFSCAR |
Texto Completo: | https://repositorio.ufscar.br/handle/ufscar/11278 |
Resumo: | In this work, voltammetric methods for determination of losartan potassium and ketoconazole using an electrode modified with carbon black were developed. Originally, a sensor was constructed with carbon black, chitosan and epichlorohydrin. Than, it was used for the determination of losartan. The electrochemical behavior of the losartan was studied with cyclic voltammetry in 0.2 mol L−1 phosphate buffer solution (pH 3.0), which presented an irreversible oxidation peak at a potential of 1.28 V. The square wave voltammetry technique was selected for the quantification of losartan in commercial pharmaceutical formulations and synthetic biological samples. The following parameters were evaluated: frequency, pulse amplitude and step potential. A linear response was observed in the concentration range from 4.97 × 10−6 to 4.76 × 10−5 mol L−1 represented by the linear regression equation: Ip (μA) = − 6.04 × 10−8 + 0.122 [LOS] (μmol L−1); r = 0.990 and with a limit of detection of 4.79 × 10−7 mol L−1. The method developed was successfully applied for the determination of losartan in pharmaceutical formulations and the comparison of these results to UV-visible spectrophotometry determination, do not presented significant difference at confidence level of 95% using a t-test student. In addition, the determination of losartan was performed in samples of synthetic biological fluids, with satisfactory results. The electrochemical behavior of the ketoconazole was performed through cyclic voltammetry using a glassy carbon electrode modified with carbon black, chitosan and gold nanoparticles in 0.2 mol L−1 phosphate buffer (pH 10). An irreversible oxidation peak was observed at 0.65 V. The ketoconazole determination was developed using square wave voltammetry under optimized conditions. The obtained analytical curve was linear in the concentrations range of ketoconazole, from 1.00 × 10−7 to 2.90 × 10−6 mol L−1, according to the linear regression equation: Ip (μA) = −1, 8 × 10−8 + 3.6 [CTO] (μmol L−1); r = 0.999, with a limit of detection of 4.43 × 10−9 mol L−1. In addition, the voltammetric procedures were successfully applied in the ketoconazole determination in pharmaceutical formulations and synthetic biological samples with satisfactory results. |
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Silva, Laís PereiraFatibello Filho, Orlandohttp://lattes.cnpq.br/9859737944357808http://lattes.cnpq.br/376158692266925904d541e8-9fbe-4d54-9cad-bb02e9025b8e2019-04-18T19:57:49Z2019-04-18T19:57:49Z2019-02-28SILVA, Laís Pereira. Desenvolvimento de procedimentos eletroanalíticos para a determinação de fármacos em formulações farmacêuticas e fluidos biológicos empregando sensores à base de carbon black. 2019. Dissertação (Mestrado em Química) – Universidade Federal de São Carlos, São Carlos, 2019. Disponível em: https://repositorio.ufscar.br/handle/ufscar/11278.https://repositorio.ufscar.br/handle/ufscar/11278In this work, voltammetric methods for determination of losartan potassium and ketoconazole using an electrode modified with carbon black were developed. Originally, a sensor was constructed with carbon black, chitosan and epichlorohydrin. Than, it was used for the determination of losartan. The electrochemical behavior of the losartan was studied with cyclic voltammetry in 0.2 mol L−1 phosphate buffer solution (pH 3.0), which presented an irreversible oxidation peak at a potential of 1.28 V. The square wave voltammetry technique was selected for the quantification of losartan in commercial pharmaceutical formulations and synthetic biological samples. The following parameters were evaluated: frequency, pulse amplitude and step potential. A linear response was observed in the concentration range from 4.97 × 10−6 to 4.76 × 10−5 mol L−1 represented by the linear regression equation: Ip (μA) = − 6.04 × 10−8 + 0.122 [LOS] (μmol L−1); r = 0.990 and with a limit of detection of 4.79 × 10−7 mol L−1. The method developed was successfully applied for the determination of losartan in pharmaceutical formulations and the comparison of these results to UV-visible spectrophotometry determination, do not presented significant difference at confidence level of 95% using a t-test student. In addition, the determination of losartan was performed in samples of synthetic biological fluids, with satisfactory results. The electrochemical behavior of the ketoconazole was performed through cyclic voltammetry using a glassy carbon electrode modified with carbon black, chitosan and gold nanoparticles in 0.2 mol L−1 phosphate buffer (pH 10). An irreversible oxidation peak was observed at 0.65 V. The ketoconazole determination was developed using square wave voltammetry under optimized conditions. The obtained analytical curve was linear in the concentrations range of ketoconazole, from 1.00 × 10−7 to 2.90 × 10−6 mol L−1, according to the linear regression equation: Ip (μA) = −1, 8 × 10−8 + 3.6 [CTO] (μmol L−1); r = 0.999, with a limit of detection of 4.43 × 10−9 mol L−1. In addition, the voltammetric procedures were successfully applied in the ketoconazole determination in pharmaceutical formulations and synthetic biological samples with satisfactory results.Neste trabalho, foram desenvolvidos métodos voltamétricos para a determinação de losartana potássica e cetoconazol empregando-se um eletrodo de carbono vítreo modificado com carbon black. Inicialmente foi proposto um sensor utilizando carbon black, quitosana e epicloridrina e este foi empregado para a determinação do fármaco losartana potássica. Avaliou-se o comportamento deste fármaco utilizando a voltametria cíclica em tampão fosfato 0,2 mol L−1 (pH 3,0), observando-se um pico de oxidação irreversível em 1,28 V. A voltametria de onda quadrada foi selecionada para a quantificação da losartana potássica em formulações farmacêuticas e fluidos biológicos sintéticos, com os seguintes parâmetros avaliados: frequência, amplitude de pulso de potencial e incremento de varredura. Foi observada uma resposta linear no intervalo de concentrações de losartana potássica de 4,97 × 10−6 a 4,76 × 10−5 mol L−1 representada pela equação de regressão linear: Ip (μA) = −6,04 × 10−8 + 0,122 [LOS] (μmol L−1); com coeficiente de correlação linear, r = 0,990 e limite de detecção de 4,79 μmol L−1. O procedimento desenvolvido foi empregado com sucesso para a determinação de losartana potássica em amostras farmacêutica comerciais e os resultados obtidos foram comparados com o método de espectrofotometria UV-visível, sendo que não houve diferença estatística significativa entre os resultados, a um nível de confiança de 95%, segundo o teste-t pareado. Além disso, a determinação deste fármaco também foi realizada em amostras de fluidos biológicos sintéticos, obtendo-se valores satisfatórios. A determinação de cetoconazol foi realizada utilizando-se um sensor com filme do compósito de carbon black, quitosana e nanopartículas de ouro. Utilizando-se a voltametria cíclica foi observado um pico de oxidação para a molécula de cetoconazol em 0,65 V em tampão fosfato 0,2 mol L−1 (pH 10). A determinação deste fármaco foi realizada empregando-se a voltametria de onda quadrada, sendo os paramêtros da técnica previamente otimizados. A curva obtida foi linear no intervalo de concentração de cetoconazol de 1,00 × 10−7 a 2,90 × 10−6 mol L−1, e obedeceu a seguinte equação de regressão linear: Ip (μA) = − 1,8 × 10−8 + 3,6 [CTO] (μmol L−1); r = 0,999, sendo o LOD igual a 4,43 nmol L−1. Finalmente, o método proposto foi aplicado nas análises de amostras farmacêuticas e biológicas sintéticas, sendo os valores obtidos comparados com àquele obtidos empregando-se o método espectrofotométrico.Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)CNPq: 132843/2017-0porUniversidade Federal de São CarlosCâmpus São CarlosPrograma de Pós-Graduação em Química - PPGQUFSCarDeterminação voltamétricaFármacosSensoresEletroanalíticaNegro de fumoQuímica analíticaVoltammetric determinationCarbon blackAnalytical chemistryCIENCIAS EXATAS E DA TERRA::QUIMICA::QUIMICA ANALITICA::ELETROANALITICADesenvolvimento de procedimentos eletroanalíticos para a determinação de fármacos em formulações farmacêuticas e fluidos biológicos empregando sensores à base de carbon blackDevelopment of eletroanalytic procedures for determination of drugs in pharmaceutical formulations and biological fluids using sensors based on carbon blackinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisOnline6007a1dec22-4b2d-4dba-8971-ab07f55c7d54info:eu-repo/semantics/openAccessreponame:Repositório Institucional da UFSCARinstname:Universidade Federal de São Carlos (UFSCAR)instacron:UFSCARORIGINALLaís Pereira Silva.pdfLaís Pereira Silva.pdfdissertaçãoapplication/pdf2459485https://repositorio.ufscar.br/bitstream/ufscar/11278/1/La%c3%ads%20Pereira%20Silva.pdff05f154edc9a21dd2a1e0e9b33c29513MD51LICENSElicense.txtlicense.txttext/plain; charset=utf-81957https://repositorio.ufscar.br/bitstream/ufscar/11278/3/license.txtae0398b6f8b235e40ad82cba6c50031dMD53TEXTLaís Pereira Silva.pdf.txtLaís Pereira Silva.pdf.txtExtracted texttext/plain152411https://repositorio.ufscar.br/bitstream/ufscar/11278/4/La%c3%ads%20Pereira%20Silva.pdf.txtf704d56a031774bf4af7bdb8d75f469eMD54THUMBNAILLaís Pereira Silva.pdf.jpgLaís Pereira Silva.pdf.jpgIM Thumbnailimage/jpeg10161https://repositorio.ufscar.br/bitstream/ufscar/11278/5/La%c3%ads%20Pereira%20Silva.pdf.jpg36e0ca8c03a91934d79b90f0916f060bMD55ufscar/112782023-09-18 18:31:21.806oai:repositorio.ufscar.br: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Repositório InstitucionalPUBhttps://repositorio.ufscar.br/oai/requestopendoar:43222023-09-18T18:31:21Repositório Institucional da UFSCAR - Universidade Federal de São Carlos (UFSCAR)false |
dc.title.por.fl_str_mv |
Desenvolvimento de procedimentos eletroanalíticos para a determinação de fármacos em formulações farmacêuticas e fluidos biológicos empregando sensores à base de carbon black |
dc.title.alternative.eng.fl_str_mv |
Development of eletroanalytic procedures for determination of drugs in pharmaceutical formulations and biological fluids using sensors based on carbon black |
title |
Desenvolvimento de procedimentos eletroanalíticos para a determinação de fármacos em formulações farmacêuticas e fluidos biológicos empregando sensores à base de carbon black |
spellingShingle |
Desenvolvimento de procedimentos eletroanalíticos para a determinação de fármacos em formulações farmacêuticas e fluidos biológicos empregando sensores à base de carbon black Silva, Laís Pereira Determinação voltamétrica Fármacos Sensores Eletroanalítica Negro de fumo Química analítica Voltammetric determination Carbon black Analytical chemistry CIENCIAS EXATAS E DA TERRA::QUIMICA::QUIMICA ANALITICA::ELETROANALITICA |
title_short |
Desenvolvimento de procedimentos eletroanalíticos para a determinação de fármacos em formulações farmacêuticas e fluidos biológicos empregando sensores à base de carbon black |
title_full |
Desenvolvimento de procedimentos eletroanalíticos para a determinação de fármacos em formulações farmacêuticas e fluidos biológicos empregando sensores à base de carbon black |
title_fullStr |
Desenvolvimento de procedimentos eletroanalíticos para a determinação de fármacos em formulações farmacêuticas e fluidos biológicos empregando sensores à base de carbon black |
title_full_unstemmed |
Desenvolvimento de procedimentos eletroanalíticos para a determinação de fármacos em formulações farmacêuticas e fluidos biológicos empregando sensores à base de carbon black |
title_sort |
Desenvolvimento de procedimentos eletroanalíticos para a determinação de fármacos em formulações farmacêuticas e fluidos biológicos empregando sensores à base de carbon black |
author |
Silva, Laís Pereira |
author_facet |
Silva, Laís Pereira |
author_role |
author |
dc.contributor.authorlattes.por.fl_str_mv |
http://lattes.cnpq.br/3761586922669259 |
dc.contributor.author.fl_str_mv |
Silva, Laís Pereira |
dc.contributor.advisor1.fl_str_mv |
Fatibello Filho, Orlando |
dc.contributor.advisor1Lattes.fl_str_mv |
http://lattes.cnpq.br/9859737944357808 |
dc.contributor.authorID.fl_str_mv |
04d541e8-9fbe-4d54-9cad-bb02e9025b8e |
contributor_str_mv |
Fatibello Filho, Orlando |
dc.subject.por.fl_str_mv |
Determinação voltamétrica Fármacos Sensores Eletroanalítica Negro de fumo Química analítica |
topic |
Determinação voltamétrica Fármacos Sensores Eletroanalítica Negro de fumo Química analítica Voltammetric determination Carbon black Analytical chemistry CIENCIAS EXATAS E DA TERRA::QUIMICA::QUIMICA ANALITICA::ELETROANALITICA |
dc.subject.eng.fl_str_mv |
Voltammetric determination Carbon black Analytical chemistry |
dc.subject.cnpq.fl_str_mv |
CIENCIAS EXATAS E DA TERRA::QUIMICA::QUIMICA ANALITICA::ELETROANALITICA |
description |
In this work, voltammetric methods for determination of losartan potassium and ketoconazole using an electrode modified with carbon black were developed. Originally, a sensor was constructed with carbon black, chitosan and epichlorohydrin. Than, it was used for the determination of losartan. The electrochemical behavior of the losartan was studied with cyclic voltammetry in 0.2 mol L−1 phosphate buffer solution (pH 3.0), which presented an irreversible oxidation peak at a potential of 1.28 V. The square wave voltammetry technique was selected for the quantification of losartan in commercial pharmaceutical formulations and synthetic biological samples. The following parameters were evaluated: frequency, pulse amplitude and step potential. A linear response was observed in the concentration range from 4.97 × 10−6 to 4.76 × 10−5 mol L−1 represented by the linear regression equation: Ip (μA) = − 6.04 × 10−8 + 0.122 [LOS] (μmol L−1); r = 0.990 and with a limit of detection of 4.79 × 10−7 mol L−1. The method developed was successfully applied for the determination of losartan in pharmaceutical formulations and the comparison of these results to UV-visible spectrophotometry determination, do not presented significant difference at confidence level of 95% using a t-test student. In addition, the determination of losartan was performed in samples of synthetic biological fluids, with satisfactory results. The electrochemical behavior of the ketoconazole was performed through cyclic voltammetry using a glassy carbon electrode modified with carbon black, chitosan and gold nanoparticles in 0.2 mol L−1 phosphate buffer (pH 10). An irreversible oxidation peak was observed at 0.65 V. The ketoconazole determination was developed using square wave voltammetry under optimized conditions. The obtained analytical curve was linear in the concentrations range of ketoconazole, from 1.00 × 10−7 to 2.90 × 10−6 mol L−1, according to the linear regression equation: Ip (μA) = −1, 8 × 10−8 + 3.6 [CTO] (μmol L−1); r = 0.999, with a limit of detection of 4.43 × 10−9 mol L−1. In addition, the voltammetric procedures were successfully applied in the ketoconazole determination in pharmaceutical formulations and synthetic biological samples with satisfactory results. |
publishDate |
2019 |
dc.date.accessioned.fl_str_mv |
2019-04-18T19:57:49Z |
dc.date.available.fl_str_mv |
2019-04-18T19:57:49Z |
dc.date.issued.fl_str_mv |
2019-02-28 |
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 |
SILVA, Laís Pereira. Desenvolvimento de procedimentos eletroanalíticos para a determinação de fármacos em formulações farmacêuticas e fluidos biológicos empregando sensores à base de carbon black. 2019. Dissertação (Mestrado em Química) – Universidade Federal de São Carlos, São Carlos, 2019. Disponível em: https://repositorio.ufscar.br/handle/ufscar/11278. |
dc.identifier.uri.fl_str_mv |
https://repositorio.ufscar.br/handle/ufscar/11278 |
identifier_str_mv |
SILVA, Laís Pereira. Desenvolvimento de procedimentos eletroanalíticos para a determinação de fármacos em formulações farmacêuticas e fluidos biológicos empregando sensores à base de carbon black. 2019. Dissertação (Mestrado em Química) – Universidade Federal de São Carlos, São Carlos, 2019. Disponível em: https://repositorio.ufscar.br/handle/ufscar/11278. |
url |
https://repositorio.ufscar.br/handle/ufscar/11278 |
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por |
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por |
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info:eu-repo/semantics/openAccess |
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openAccess |
dc.publisher.none.fl_str_mv |
Universidade Federal de São Carlos Câmpus São Carlos |
dc.publisher.program.fl_str_mv |
Programa de Pós-Graduação em Química - PPGQ |
dc.publisher.initials.fl_str_mv |
UFSCar |
publisher.none.fl_str_mv |
Universidade Federal de São Carlos Câmpus São Carlos |
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Repositório Institucional da UFSCAR |
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