Desenvolvimento de procedimentos eletroanalíticos para a determinação de fármacos em formulações farmacêuticas e fluidos biológicos empregando sensores à base de carbon black

Detalhes bibliográficos
Autor(a) principal: Silva, Laís Pereira
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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spelling 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:ufscar/11278TElDRU7Dh0EgREUgRElTVFJJQlVJw4fDg08gTsODTy1FWENMVVNJVkEKCkNvbSBhIGFwcmVzZW50YcOnw6NvIGRlc3RhIGxpY2Vuw6dhLCB2b2PDqiAobyBhdXRvciAoZXMpIG91IG8gdGl0dWxhciBkb3MgZGlyZWl0b3MgZGUgYXV0b3IpIGNvbmNlZGUgw6AgVW5pdmVyc2lkYWRlCkZlZGVyYWwgZGUgU8OjbyBDYXJsb3MgbyBkaXJlaXRvIG7Do28tZXhjbHVzaXZvIGRlIHJlcHJvZHV6aXIsICB0cmFkdXppciAoY29uZm9ybWUgZGVmaW5pZG8gYWJhaXhvKSwgZS9vdQpkaXN0cmlidWlyIGEgc3VhIHRlc2Ugb3UgZGlzc2VydGHDp8OjbyAoaW5jbHVpbmRvIG8gcmVzdW1vKSBwb3IgdG9kbyBvIG11bmRvIG5vIGZvcm1hdG8gaW1wcmVzc28gZSBlbGV0csO0bmljbyBlCmVtIHF1YWxxdWVyIG1laW8sIGluY2x1aW5kbyBvcyBmb3JtYXRvcyDDoXVkaW8gb3UgdsOtZGVvLgoKVm9jw6ogY29uY29yZGEgcXVlIGEgVUZTQ2FyIHBvZGUsIHNlbSBhbHRlcmFyIG8gY29udGXDumRvLCB0cmFuc3BvciBhIHN1YSB0ZXNlIG91IGRpc3NlcnRhw6fDo28KcGFyYSBxdWFscXVlciBtZWlvIG91IGZvcm1hdG8gcGFyYSBmaW5zIGRlIHByZXNlcnZhw6fDo28uCgpWb2PDqiB0YW1iw6ltIGNvbmNvcmRhIHF1ZSBhIFVGU0NhciBwb2RlIG1hbnRlciBtYWlzIGRlIHVtYSBjw7NwaWEgYSBzdWEgdGVzZSBvdQpkaXNzZXJ0YcOnw6NvIHBhcmEgZmlucyBkZSBzZWd1cmFuw6dhLCBiYWNrLXVwIGUgcHJlc2VydmHDp8Ojby4KClZvY8OqIGRlY2xhcmEgcXVlIGEgc3VhIHRlc2Ugb3UgZGlzc2VydGHDp8OjbyDDqSBvcmlnaW5hbCBlIHF1ZSB2b2PDqiB0ZW0gbyBwb2RlciBkZSBjb25jZWRlciBvcyBkaXJlaXRvcyBjb250aWRvcwpuZXN0YSBsaWNlbsOnYS4gVm9jw6ogdGFtYsOpbSBkZWNsYXJhIHF1ZSBvIGRlcMOzc2l0byBkYSBzdWEgdGVzZSBvdSBkaXNzZXJ0YcOnw6NvIG7Do28sIHF1ZSBzZWphIGRlIHNldQpjb25oZWNpbWVudG8sIGluZnJpbmdlIGRpcmVpdG9zIGF1dG9yYWlzIGRlIG5pbmd1w6ltLgoKQ2FzbyBhIHN1YSB0ZXNlIG91IGRpc3NlcnRhw6fDo28gY29udGVuaGEgbWF0ZXJpYWwgcXVlIHZvY8OqIG7Do28gcG9zc3VpIGEgdGl0dWxhcmlkYWRlIGRvcyBkaXJlaXRvcyBhdXRvcmFpcywgdm9jw6oKZGVjbGFyYSBxdWUgb2J0ZXZlIGEgcGVybWlzc8OjbyBpcnJlc3RyaXRhIGRvIGRldGVudG9yIGRvcyBkaXJlaXRvcyBhdXRvcmFpcyBwYXJhIGNvbmNlZGVyIMOgIFVGU0NhcgpvcyBkaXJlaXRvcyBhcHJlc2VudGFkb3MgbmVzdGEgbGljZW7Dp2EsIGUgcXVlIGVzc2UgbWF0ZXJpYWwgZGUgcHJvcHJpZWRhZGUgZGUgdGVyY2Vpcm9zIGVzdMOhIGNsYXJhbWVudGUKaWRlbnRpZmljYWRvIGUgcmVjb25oZWNpZG8gbm8gdGV4dG8gb3Ugbm8gY29udGXDumRvIGRhIHRlc2Ugb3UgZGlzc2VydGHDp8OjbyBvcmEgZGVwb3NpdGFkYS4KCkNBU08gQSBURVNFIE9VIERJU1NFUlRBw4fDg08gT1JBIERFUE9TSVRBREEgVEVOSEEgU0lETyBSRVNVTFRBRE8gREUgVU0gUEFUUk9Dw41OSU8gT1UKQVBPSU8gREUgVU1BIEFHw4pOQ0lBIERFIEZPTUVOVE8gT1UgT1VUUk8gT1JHQU5JU01PIFFVRSBOw4NPIFNFSkEgQSBVRlNDYXIsClZPQ8OKIERFQ0xBUkEgUVVFIFJFU1BFSVRPVSBUT0RPUyBFIFFVQUlTUVVFUiBESVJFSVRPUyBERSBSRVZJU8ODTyBDT01PClRBTULDiU0gQVMgREVNQUlTIE9CUklHQcOHw5VFUyBFWElHSURBUyBQT1IgQ09OVFJBVE8gT1UgQUNPUkRPLgoKQSBVRlNDYXIgc2UgY29tcHJvbWV0ZSBhIGlkZW50aWZpY2FyIGNsYXJhbWVudGUgbyBzZXUgbm9tZSAocykgb3UgbyhzKSBub21lKHMpIGRvKHMpCmRldGVudG9yKGVzKSBkb3MgZGlyZWl0b3MgYXV0b3JhaXMgZGEgdGVzZSBvdSBkaXNzZXJ0YcOnw6NvLCBlIG7Do28gZmFyw6EgcXVhbHF1ZXIgYWx0ZXJhw6fDo28sIGFsw6ltIGRhcXVlbGFzCmNvbmNlZGlkYXMgcG9yIGVzdGEgbGljZW7Dp2EuCg==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
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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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dc.relation.confidence.fl_str_mv 600
dc.relation.authority.fl_str_mv 7a1dec22-4b2d-4dba-8971-ab07f55c7d54
dc.rights.driver.fl_str_mv info:eu-repo/semantics/openAccess
eu_rights_str_mv 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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