Determinação voltamétrica de fibratos em formulações farmacêuticas utilizando eletrodos de carbono vítreo modificados com nanotubos de carbono
Autor(a) principal: | |
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Data de Publicação: | 2012 |
Tipo de documento: | Dissertação |
Idioma: | por |
Título da fonte: | Repositório Institucional da UFSCAR |
Texto Completo: | https://repositorio.ufscar.br/handle/ufscar/6538 |
Resumo: | In this work voltammetric methods were developed from gemfibrozil (GEM) and bezafibrate (BZF) determination in pharmaceutical formulations for using modified glassy carbon electrode with dihexadecyl hydrogen phosphate containing carbon nanotubes treated chemically. Firstly was studied the voltammetric behavior of GEM in 0.1 mol L 1 (pH 2.0) phosphate buffer solution, was observed an irreversible oxidation peak in 1.31 V. Square-wave adsorptive stripping voltammetry was selected for GEM quantification in pharmaceuticals formulations, with the following parameters: adsorption time of 300 s, frequency of 40 Hz, a pulse amplitude of 45 mV and scan increment of 4 mV. The analytical curve was linear over the concentration range of 7.5 × 10−8 a 1.0 × 10−6 mol L−1 of GEM, represented by following ΔI (μA) = 0,086 + 1,05 × 107 [GEM] (mol L 1), correlation coefficient of 0.997 and detection limit of 5.3 × 10−8 mol L−1. The procedure developed was successfully applied to determine GEM in commercial pharmaceutical samples and the results were compared with the reference method, described in British pharmacopoeia. There was no significant difference (5 %) between the results obtained at a confidence level of 95%. The BZF determination was carried in 0.1 mol L 1 (pH 2.0) phosphate buffer solution and an irreversible peak in 1.09 V was observed. Square-wave adsorptive stripping voltammetry technique was selected for BZF determination with the following parameters: adsorption time of 180 s, frequency of 20 Hz, pulse amplitude of 40 mV and scan increment of 7 mV. The proposed method presented a linear interval between 5.0 × 10−8 a 9.1 × 10−7 mol L−1 and detection limited of 1.6 × 10−8 mol L−1. The BZF was quantified in commercials samples and the results were compared with de spectrophotometric method, with errors between 2.9 e 0.5 %. Finally for each analyte were calculated the number of electrons involved in the oxidation reaction and was proposed a possible mechanism for the oxidation reaction of these drugs, because there are no reports in the literature. |
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Quintero, Jorge Armando ArdilaFatibello Filho, OrlandoÚltima atualização do currículo em 14/03/2011http://lattes.cnpq.br/2093399167811012f481a9d0-f5e0-4b1d-8741-5d855cb8fce82016-06-02T20:36:41Z2012-11-012016-06-02T20:36:41Z2012-07-27QUINTERO, Jorge Armando Ardila. Voltammetric determination of fibrates in pharmaceutical formulations using glassy carbon electrode modified with carbon nanotubes. 2012. 89 f. Dissertação (Mestrado em Ciências Exatas e da Terra) - Universidade Federal de São Carlos, São Carlos, 2012.https://repositorio.ufscar.br/handle/ufscar/6538In this work voltammetric methods were developed from gemfibrozil (GEM) and bezafibrate (BZF) determination in pharmaceutical formulations for using modified glassy carbon electrode with dihexadecyl hydrogen phosphate containing carbon nanotubes treated chemically. Firstly was studied the voltammetric behavior of GEM in 0.1 mol L 1 (pH 2.0) phosphate buffer solution, was observed an irreversible oxidation peak in 1.31 V. Square-wave adsorptive stripping voltammetry was selected for GEM quantification in pharmaceuticals formulations, with the following parameters: adsorption time of 300 s, frequency of 40 Hz, a pulse amplitude of 45 mV and scan increment of 4 mV. The analytical curve was linear over the concentration range of 7.5 × 10−8 a 1.0 × 10−6 mol L−1 of GEM, represented by following ΔI (μA) = 0,086 + 1,05 × 107 [GEM] (mol L 1), correlation coefficient of 0.997 and detection limit of 5.3 × 10−8 mol L−1. The procedure developed was successfully applied to determine GEM in commercial pharmaceutical samples and the results were compared with the reference method, described in British pharmacopoeia. There was no significant difference (5 %) between the results obtained at a confidence level of 95%. The BZF determination was carried in 0.1 mol L 1 (pH 2.0) phosphate buffer solution and an irreversible peak in 1.09 V was observed. Square-wave adsorptive stripping voltammetry technique was selected for BZF determination with the following parameters: adsorption time of 180 s, frequency of 20 Hz, pulse amplitude of 40 mV and scan increment of 7 mV. The proposed method presented a linear interval between 5.0 × 10−8 a 9.1 × 10−7 mol L−1 and detection limited of 1.6 × 10−8 mol L−1. The BZF was quantified in commercials samples and the results were compared with de spectrophotometric method, with errors between 2.9 e 0.5 %. Finally for each analyte were calculated the number of electrons involved in the oxidation reaction and was proposed a possible mechanism for the oxidation reaction of these drugs, because there are no reports in the literature.Neste trabalho foram desenvolvidos métodos voltamétricos para a determinação de genfibrozila (GEN) e bezafibrato (BZF) em formulações farmacêuticas, empregando eletrodos de carbono vítreo modificados com filme de dihexadecil hidrogênio fosfato contendo nanotubos de carbono de paredes múltiplas tratados quimicamente. Inicialmente estudou-se o comportamento voltamétrico de GEN em tampão fosfato 0,1 mol L−1 (pH 2,0), observando-se um pico irreversível de oxidação em 1,31 V. A técnica de voltametria de redissolução anódica de onda quadrada foi selecionada para a quantificação do GEN em formulações farmacêuticas, com os seguintes parâmetros avaliados: tempo de pré-concentração de 300 s, frequência de 40 Hz, amplitude de pulso de 45 mV e incremento de varredura de 4 mV. A curva analítica foi linear no intervalo de concentração de GEN de 7,5 × 10−8 a 1,0 × 10−6 mol L−1, representada pela equação ΔI (μA) = 0,086 + 1,05 × 107 [GEN] (mol L 1), com um coeficiente de correlação linear de 0,997 e um limite de detecção de 5,3 × 10−8 mol L−1. O procedimento desenvolvido foi empregado com sucesso na determinação de GEN em amostras farmacêuticas comerciais e os resultados obtidos foram comparados com o método de referencia, descrito na farmacopeia britânica. Não houve diferença significativa (5,0 %) entre os resultados obtidos a um nível de confiança de 95%. A determinação do BZF foi realizada em tampão fosfato 0,1 mol L−1 (pH 2,0) sendo observado um pico de oxidação irreversível em 1,09 V. A técnica de voltametria de redissolução anódica de onda quadrada foi selecionada para a determinação de BZF com os seguintes parâmetros otimizados: tempo de pré-concentração de 180 s, frequência de 20 Hz, amplitude de pulso de 40 mV e incremento de varredura de 7 mV. O método proposto apresentou uma curva analítica para BZF variando entre 5,0 × 10−8 e 9,1 × 10−7 mol L−1 e um limite de detecção de 1,6 × 10−8 mol L−1. O BZF foi quantificado em amostras comerciais e os resultados comparados com o método espectrofotométrico, os erros obtidos variaram entre 2,9 e 0,5 %. Finalmente, para cada analito foram calculados o número de elétrons envolvidos na reação de oxidação e foi proposto um possível mecanismo para reação de eletrooxidação destes fármacos, uma vez que, não relatos na literatura.Universidade Federal de Sao Carlosapplication/pdfporUniversidade Federal de São CarlosPrograma de Pós-Graduação em Química - PPGQUFSCarBRQuímica analíticaEletrodos modificadosCarbono vítreoNanotubos de carbonoVoltametria de onda quadradaCIENCIAS EXATAS E DA TERRA::QUIMICADeterminação voltamétrica de fibratos em formulações farmacêuticas utilizando eletrodos de carbono vítreo modificados com nanotubos de carbonoVoltammetric determination of fibrates in pharmaceutical formulations using glassy carbon electrode modified with carbon nanotubesinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesis-1-17a1dec22-4b2d-4dba-8971-ab07f55c7d54info:eu-repo/semantics/openAccessreponame:Repositório Institucional da UFSCARinstname:Universidade Federal de São Carlos (UFSCAR)instacron:UFSCARORIGINAL4645.pdfapplication/pdf1392525https://repositorio.ufscar.br/bitstream/ufscar/6538/1/4645.pdfff16f9dff6056896d391bac171f65279MD51TEXT4645.pdf.txt4645.pdf.txtExtracted texttext/plain0https://repositorio.ufscar.br/bitstream/ufscar/6538/4/4645.pdf.txtd41d8cd98f00b204e9800998ecf8427eMD54THUMBNAIL4645.pdf.jpg4645.pdf.jpgIM Thumbnailimage/jpeg9176https://repositorio.ufscar.br/bitstream/ufscar/6538/5/4645.pdf.jpgdd3dcc729051875b98bcbeb76040e108MD55ufscar/65382023-09-18 18:30:39.421oai:repositorio.ufscar.br:ufscar/6538Repositório InstitucionalPUBhttps://repositorio.ufscar.br/oai/requestopendoar:43222023-09-18T18:30:39Repositório Institucional da UFSCAR - Universidade Federal de São Carlos (UFSCAR)false |
dc.title.por.fl_str_mv |
Determinação voltamétrica de fibratos em formulações farmacêuticas utilizando eletrodos de carbono vítreo modificados com nanotubos de carbono |
dc.title.alternative.eng.fl_str_mv |
Voltammetric determination of fibrates in pharmaceutical formulations using glassy carbon electrode modified with carbon nanotubes |
title |
Determinação voltamétrica de fibratos em formulações farmacêuticas utilizando eletrodos de carbono vítreo modificados com nanotubos de carbono |
spellingShingle |
Determinação voltamétrica de fibratos em formulações farmacêuticas utilizando eletrodos de carbono vítreo modificados com nanotubos de carbono Quintero, Jorge Armando Ardila Química analítica Eletrodos modificados Carbono vítreo Nanotubos de carbono Voltametria de onda quadrada CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Determinação voltamétrica de fibratos em formulações farmacêuticas utilizando eletrodos de carbono vítreo modificados com nanotubos de carbono |
title_full |
Determinação voltamétrica de fibratos em formulações farmacêuticas utilizando eletrodos de carbono vítreo modificados com nanotubos de carbono |
title_fullStr |
Determinação voltamétrica de fibratos em formulações farmacêuticas utilizando eletrodos de carbono vítreo modificados com nanotubos de carbono |
title_full_unstemmed |
Determinação voltamétrica de fibratos em formulações farmacêuticas utilizando eletrodos de carbono vítreo modificados com nanotubos de carbono |
title_sort |
Determinação voltamétrica de fibratos em formulações farmacêuticas utilizando eletrodos de carbono vítreo modificados com nanotubos de carbono |
author |
Quintero, Jorge Armando Ardila |
author_facet |
Quintero, Jorge Armando Ardila |
author_role |
author |
dc.contributor.authorlattes.por.fl_str_mv |
http://lattes.cnpq.br/2093399167811012 |
dc.contributor.author.fl_str_mv |
Quintero, Jorge Armando Ardila |
dc.contributor.advisor1.fl_str_mv |
Fatibello Filho, Orlando |
dc.contributor.advisor1Lattes.fl_str_mv |
Última atualização do currículo em 14/03/2011 |
dc.contributor.authorID.fl_str_mv |
f481a9d0-f5e0-4b1d-8741-5d855cb8fce8 |
contributor_str_mv |
Fatibello Filho, Orlando |
dc.subject.por.fl_str_mv |
Química analítica Eletrodos modificados Carbono vítreo Nanotubos de carbono Voltametria de onda quadrada |
topic |
Química analítica Eletrodos modificados Carbono vítreo Nanotubos de carbono Voltametria de onda quadrada CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.cnpq.fl_str_mv |
CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
In this work voltammetric methods were developed from gemfibrozil (GEM) and bezafibrate (BZF) determination in pharmaceutical formulations for using modified glassy carbon electrode with dihexadecyl hydrogen phosphate containing carbon nanotubes treated chemically. Firstly was studied the voltammetric behavior of GEM in 0.1 mol L 1 (pH 2.0) phosphate buffer solution, was observed an irreversible oxidation peak in 1.31 V. Square-wave adsorptive stripping voltammetry was selected for GEM quantification in pharmaceuticals formulations, with the following parameters: adsorption time of 300 s, frequency of 40 Hz, a pulse amplitude of 45 mV and scan increment of 4 mV. The analytical curve was linear over the concentration range of 7.5 × 10−8 a 1.0 × 10−6 mol L−1 of GEM, represented by following ΔI (μA) = 0,086 + 1,05 × 107 [GEM] (mol L 1), correlation coefficient of 0.997 and detection limit of 5.3 × 10−8 mol L−1. The procedure developed was successfully applied to determine GEM in commercial pharmaceutical samples and the results were compared with the reference method, described in British pharmacopoeia. There was no significant difference (5 %) between the results obtained at a confidence level of 95%. The BZF determination was carried in 0.1 mol L 1 (pH 2.0) phosphate buffer solution and an irreversible peak in 1.09 V was observed. Square-wave adsorptive stripping voltammetry technique was selected for BZF determination with the following parameters: adsorption time of 180 s, frequency of 20 Hz, pulse amplitude of 40 mV and scan increment of 7 mV. The proposed method presented a linear interval between 5.0 × 10−8 a 9.1 × 10−7 mol L−1 and detection limited of 1.6 × 10−8 mol L−1. The BZF was quantified in commercials samples and the results were compared with de spectrophotometric method, with errors between 2.9 e 0.5 %. Finally for each analyte were calculated the number of electrons involved in the oxidation reaction and was proposed a possible mechanism for the oxidation reaction of these drugs, because there are no reports in the literature. |
publishDate |
2012 |
dc.date.available.fl_str_mv |
2012-11-01 2016-06-02T20:36:41Z |
dc.date.issued.fl_str_mv |
2012-07-27 |
dc.date.accessioned.fl_str_mv |
2016-06-02T20:36:41Z |
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 |
QUINTERO, Jorge Armando Ardila. Voltammetric determination of fibrates in pharmaceutical formulations using glassy carbon electrode modified with carbon nanotubes. 2012. 89 f. Dissertação (Mestrado em Ciências Exatas e da Terra) - Universidade Federal de São Carlos, São Carlos, 2012. |
dc.identifier.uri.fl_str_mv |
https://repositorio.ufscar.br/handle/ufscar/6538 |
identifier_str_mv |
QUINTERO, Jorge Armando Ardila. Voltammetric determination of fibrates in pharmaceutical formulations using glassy carbon electrode modified with carbon nanotubes. 2012. 89 f. Dissertação (Mestrado em Ciências Exatas e da Terra) - Universidade Federal de São Carlos, São Carlos, 2012. |
url |
https://repositorio.ufscar.br/handle/ufscar/6538 |
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openAccess |
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Universidade Federal de São Carlos |
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Programa de Pós-Graduação em Química - PPGQ |
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UFSCar |
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BR |
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Universidade Federal de São Carlos |
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