Desenvolvimento e validação de metodologia para avaliação de rupatadina por cromatografia líquida e eletroforese capilar
Autor(a) principal: | |
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Data de Publicação: | 2009 |
Tipo de documento: | Dissertação |
Idioma: | por |
Título da fonte: | Repositório Institucional Manancial UFSM |
Texto Completo: | http://repositorio.ufsm.br/handle/1/5884 |
Resumo: | Rupatadine is a second generation antihistamine H1, from the pyperidinic group, which inhibits both the histamine and platelet activating factor effects, and is clinically used for the treatment of allergic rhinitis and chronic urticaria. The methods for the evaluation of rupatadine in pharmaceutical products were developed and validated in the present work. The reversed-phase liquid chromatography (RP-LC) analysis was carried out using a Gemini C18 column (150 mm x 4.6 mm), maintained at 30 oC. The mobile phase consisted of ammonium acetate buffer 0.01 M, pH 3.0 with 0.05% of 1-heptanosulfonic acid/acetonitrile (71.5:28.5 v/v), run at a flow rate of 1.0 mL/min with detection at 242 nm. The chromatographic separation was obtained within 7 min and it was linear in the concentration range of 0.5-400 μg/mL (r2=0.9999). The capillary electrophoresis method was developed and validated, using the micellar electrokinetic chromatography (MEKC) as the separation mode, and nimesulide as internal standard (IS). The analysis were performed on a fused-silica capillary (50 μm id, effective length, 40 cm), maintained at 35ºC, using electrolyte solution consisted of 15 mM borate buffer and 25 mM anionic detergent SDS solution at pH 10, with detection by photodiode array detector set at 205 nm. The injection was performed using the hydrodynamic mode at 50 mbar for 5 s, and a constant voltage of 25 kV was applied during the analysis. The electrophoretic separation was obtained within 6 min and it was linear in the oncentration range of 0.5-150 μg/mL (r2=0.9996). The procedures were validated evaluating parameters such as the specificity, linearity, precision, accuracy, limits of detection and quantitation, robustness, and system suitability test, giving results within the acceptable range. The proposed methods were applied for the analysis of pharmaceutical products, showing significant correlation (P>0.05) of the results. Therefore, the procedures can be applied to improve the quality control of pharmaceutical products and to assure the safety and therapeutic efficacy of the drug. |
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2009-06-162009-06-162009-03-12NOGUEIRA, Daniele Rubert. Development and validation of methodology for the evaluation of rupatadine by liquid chromatography and capillary electrophoresis. 2009. 73 f. Dissertação (Mestrado em Farmacologia) - Universidade Federal de Santa Maria, Santa Maria, 2009.http://repositorio.ufsm.br/handle/1/5884Rupatadine is a second generation antihistamine H1, from the pyperidinic group, which inhibits both the histamine and platelet activating factor effects, and is clinically used for the treatment of allergic rhinitis and chronic urticaria. The methods for the evaluation of rupatadine in pharmaceutical products were developed and validated in the present work. The reversed-phase liquid chromatography (RP-LC) analysis was carried out using a Gemini C18 column (150 mm x 4.6 mm), maintained at 30 oC. The mobile phase consisted of ammonium acetate buffer 0.01 M, pH 3.0 with 0.05% of 1-heptanosulfonic acid/acetonitrile (71.5:28.5 v/v), run at a flow rate of 1.0 mL/min with detection at 242 nm. The chromatographic separation was obtained within 7 min and it was linear in the concentration range of 0.5-400 μg/mL (r2=0.9999). The capillary electrophoresis method was developed and validated, using the micellar electrokinetic chromatography (MEKC) as the separation mode, and nimesulide as internal standard (IS). The analysis were performed on a fused-silica capillary (50 μm id, effective length, 40 cm), maintained at 35ºC, using electrolyte solution consisted of 15 mM borate buffer and 25 mM anionic detergent SDS solution at pH 10, with detection by photodiode array detector set at 205 nm. The injection was performed using the hydrodynamic mode at 50 mbar for 5 s, and a constant voltage of 25 kV was applied during the analysis. The electrophoretic separation was obtained within 6 min and it was linear in the oncentration range of 0.5-150 μg/mL (r2=0.9996). The procedures were validated evaluating parameters such as the specificity, linearity, precision, accuracy, limits of detection and quantitation, robustness, and system suitability test, giving results within the acceptable range. The proposed methods were applied for the analysis of pharmaceutical products, showing significant correlation (P>0.05) of the results. Therefore, the procedures can be applied to improve the quality control of pharmaceutical products and to assure the safety and therapeutic efficacy of the drug.A rupatadina é um anti-histamínico H1 de segunda geração pertencente ao grupo piperidínico, que inibe os efeitos da histamina e do fator ativador plaquetário, sendo utilizada clinicamente no tratamento de rinite alérgica e urticária crônica. No presente trabalho foram desenvolvidos e validados métodos para avaliação de rupatadina em produtos farmacêuticos. As análises por cromatografia líquida em fase reversa (CL-FR) foram realizadas utilizando coluna Gemini C18 (150 mm x 4,6 mm), mantida a 30 oC. A fase móvel foi composta de tampão acetato de amônio 0,01 M, pH 3,0 com 0,05% de ácido 1-heptanosulfônico/acetonitrila (71,5:28,5, v/v), eluída na vazão de 1,0 mL/min com detecção no ultravioleta a 242 nm. A separação cromatográfica foi obtida no tempo de 7 min, sendo linear na faixa de concentração de 0,5-400 μg/mL (r2=0,9999). Paralelamente, desenvolveu-se e validou-se método por eletroforese capilar, utilizando modo de separação por cromatografia eletrocinética micelar (MEKC) e nimesulida como padrão interno (PI). Executaram-se as análises em capilar de sílica fundida (50 μm id, comprimento efetivo de 40 cm), mantido a 35ºC, utilizando solução eletrolítica composta de tampão borato 15 mM e tensoativo aniônico SDS 25 mM, pH 10, com detecção no ultravioleta a 205 nm. A injeção foi realizada no modo hidrodinâmico a 50 mbar durante 5 s e voltagem constante de 25 kV foi aplicada durante as análises. A separação eletroforética foi obtida em 6 min, sendo linear na faixa de concentração de 0,5-150 μg/mL (r2=0,9996). Os procedimentos foram validados, avaliando-se os parâmetros de especificidade, linearidade, precisão, exatidão, limite de detecção e quantificação, robustez e teste de adequabilidade do sistema, cujos resultados cumpriram os requisitos preconizados. Os métodos propostos foram aplicados na análise de produtos farmacêuticos, demonstrando correlação significativa dos resultados (P>0,05). Desse modo, estabeleceram-se procedimentos que podem ser aplicados para aprimorar o controle da qualidade de medicamentos, bem como garantir a segurança e eficácia no uso terapêutico.Coordenação de Aperfeiçoamento de Pessoal de Nível Superiorapplication/pdfporUniversidade Federal de Santa MariaPrograma de Pós-Graduação em Ciências FarmacêuticasUFSMBRFarmáciaCromatografia eletrocinética micelarCromatografia líquidaProdutos farmacêuticosRupatadinaValidaçãoLiquid chromatographyMicellar electrokinetic chromatographyPharmaceutical productsRupatadineValidationCNPQ::CIENCIAS DA SAUDE::FARMACIADesenvolvimento e validação de metodologia para avaliação de rupatadina por cromatografia líquida e eletroforese capilarDevelopment and validation of methodology for the evaluation of rupatadine by liquid chromatography and capillary electrophoresisinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisDalmora, Sergio Luizhttp://lattes.cnpq.br/4505166045049607Macedo, Rui Oliveirahttp://lattes.cnpq.br/8326594695097434Aragão, Cícero Flávio Soareshttp://lattes.cnpq.br/9657118649043311http://lattes.cnpq.br/1940490517223751Nogueira, Daniele Rubert201000000000400500300300300c5c3d2e7-af0f-4f36-b006-046daf37340a0d9bba46-0fa3-403d-aa7f-f690646a75cbe07fc67c-96bd-43bd-b296-2f633f2a7b9bb3b23699-2a09-4265-b53e-c77831b002c8info:eu-repo/semantics/openAccessreponame:Repositório Institucional Manancial UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMORIGINALNOGUEIRA, DANIELE RUBERT.pdfapplication/pdf967226http://repositorio.ufsm.br/bitstream/1/5884/1/NOGUEIRA%2c%20DANIELE%20RUBERT.pdf8e971a589692e96df5e6f7ef6225d428MD51TEXTNOGUEIRA, DANIELE RUBERT.pdf.txtNOGUEIRA, DANIELE RUBERT.pdf.txtExtracted texttext/plain152963http://repositorio.ufsm.br/bitstream/1/5884/2/NOGUEIRA%2c%20DANIELE%20RUBERT.pdf.txt0349c505e1a9e2a66e7f793967072d55MD52THUMBNAILNOGUEIRA, DANIELE RUBERT.pdf.jpgNOGUEIRA, DANIELE RUBERT.pdf.jpgIM Thumbnailimage/jpeg5096http://repositorio.ufsm.br/bitstream/1/5884/3/NOGUEIRA%2c%20DANIELE%20RUBERT.pdf.jpg739dd69fbe3e4a655c6f530b3ae8c76fMD531/58842022-10-17 11:26:47.301oai:repositorio.ufsm.br:1/5884Repositório Institucionalhttp://repositorio.ufsm.br/PUBhttp://repositorio.ufsm.br/oai/requestouvidoria@ufsm.bropendoar:39132022-10-17T14:26:47Repositório Institucional Manancial UFSM - Universidade Federal de Santa Maria (UFSM)false |
dc.title.por.fl_str_mv |
Desenvolvimento e validação de metodologia para avaliação de rupatadina por cromatografia líquida e eletroforese capilar |
dc.title.alternative.eng.fl_str_mv |
Development and validation of methodology for the evaluation of rupatadine by liquid chromatography and capillary electrophoresis |
title |
Desenvolvimento e validação de metodologia para avaliação de rupatadina por cromatografia líquida e eletroforese capilar |
spellingShingle |
Desenvolvimento e validação de metodologia para avaliação de rupatadina por cromatografia líquida e eletroforese capilar Nogueira, Daniele Rubert Cromatografia eletrocinética micelar Cromatografia líquida Produtos farmacêuticos Rupatadina Validação Liquid chromatography Micellar electrokinetic chromatography Pharmaceutical products Rupatadine Validation CNPQ::CIENCIAS DA SAUDE::FARMACIA |
title_short |
Desenvolvimento e validação de metodologia para avaliação de rupatadina por cromatografia líquida e eletroforese capilar |
title_full |
Desenvolvimento e validação de metodologia para avaliação de rupatadina por cromatografia líquida e eletroforese capilar |
title_fullStr |
Desenvolvimento e validação de metodologia para avaliação de rupatadina por cromatografia líquida e eletroforese capilar |
title_full_unstemmed |
Desenvolvimento e validação de metodologia para avaliação de rupatadina por cromatografia líquida e eletroforese capilar |
title_sort |
Desenvolvimento e validação de metodologia para avaliação de rupatadina por cromatografia líquida e eletroforese capilar |
author |
Nogueira, Daniele Rubert |
author_facet |
Nogueira, Daniele Rubert |
author_role |
author |
dc.contributor.advisor1.fl_str_mv |
Dalmora, Sergio Luiz |
dc.contributor.advisor1Lattes.fl_str_mv |
http://lattes.cnpq.br/4505166045049607 |
dc.contributor.referee1.fl_str_mv |
Macedo, Rui Oliveira |
dc.contributor.referee1Lattes.fl_str_mv |
http://lattes.cnpq.br/8326594695097434 |
dc.contributor.referee2.fl_str_mv |
Aragão, Cícero Flávio Soares |
dc.contributor.referee2Lattes.fl_str_mv |
http://lattes.cnpq.br/9657118649043311 |
dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/1940490517223751 |
dc.contributor.author.fl_str_mv |
Nogueira, Daniele Rubert |
contributor_str_mv |
Dalmora, Sergio Luiz Macedo, Rui Oliveira Aragão, Cícero Flávio Soares |
dc.subject.por.fl_str_mv |
Cromatografia eletrocinética micelar Cromatografia líquida Produtos farmacêuticos Rupatadina Validação |
topic |
Cromatografia eletrocinética micelar Cromatografia líquida Produtos farmacêuticos Rupatadina Validação Liquid chromatography Micellar electrokinetic chromatography Pharmaceutical products Rupatadine Validation CNPQ::CIENCIAS DA SAUDE::FARMACIA |
dc.subject.eng.fl_str_mv |
Liquid chromatography Micellar electrokinetic chromatography Pharmaceutical products Rupatadine Validation |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS DA SAUDE::FARMACIA |
description |
Rupatadine is a second generation antihistamine H1, from the pyperidinic group, which inhibits both the histamine and platelet activating factor effects, and is clinically used for the treatment of allergic rhinitis and chronic urticaria. The methods for the evaluation of rupatadine in pharmaceutical products were developed and validated in the present work. The reversed-phase liquid chromatography (RP-LC) analysis was carried out using a Gemini C18 column (150 mm x 4.6 mm), maintained at 30 oC. The mobile phase consisted of ammonium acetate buffer 0.01 M, pH 3.0 with 0.05% of 1-heptanosulfonic acid/acetonitrile (71.5:28.5 v/v), run at a flow rate of 1.0 mL/min with detection at 242 nm. The chromatographic separation was obtained within 7 min and it was linear in the concentration range of 0.5-400 μg/mL (r2=0.9999). The capillary electrophoresis method was developed and validated, using the micellar electrokinetic chromatography (MEKC) as the separation mode, and nimesulide as internal standard (IS). The analysis were performed on a fused-silica capillary (50 μm id, effective length, 40 cm), maintained at 35ºC, using electrolyte solution consisted of 15 mM borate buffer and 25 mM anionic detergent SDS solution at pH 10, with detection by photodiode array detector set at 205 nm. The injection was performed using the hydrodynamic mode at 50 mbar for 5 s, and a constant voltage of 25 kV was applied during the analysis. The electrophoretic separation was obtained within 6 min and it was linear in the oncentration range of 0.5-150 μg/mL (r2=0.9996). The procedures were validated evaluating parameters such as the specificity, linearity, precision, accuracy, limits of detection and quantitation, robustness, and system suitability test, giving results within the acceptable range. The proposed methods were applied for the analysis of pharmaceutical products, showing significant correlation (P>0.05) of the results. Therefore, the procedures can be applied to improve the quality control of pharmaceutical products and to assure the safety and therapeutic efficacy of the drug. |
publishDate |
2009 |
dc.date.accessioned.fl_str_mv |
2009-06-16 |
dc.date.available.fl_str_mv |
2009-06-16 |
dc.date.issued.fl_str_mv |
2009-03-12 |
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info:eu-repo/semantics/publishedVersion |
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info:eu-repo/semantics/masterThesis |
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dc.identifier.citation.fl_str_mv |
NOGUEIRA, Daniele Rubert. Development and validation of methodology for the evaluation of rupatadine by liquid chromatography and capillary electrophoresis. 2009. 73 f. Dissertação (Mestrado em Farmacologia) - Universidade Federal de Santa Maria, Santa Maria, 2009. |
dc.identifier.uri.fl_str_mv |
http://repositorio.ufsm.br/handle/1/5884 |
identifier_str_mv |
NOGUEIRA, Daniele Rubert. Development and validation of methodology for the evaluation of rupatadine by liquid chromatography and capillary electrophoresis. 2009. 73 f. Dissertação (Mestrado em Farmacologia) - Universidade Federal de Santa Maria, Santa Maria, 2009. |
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http://repositorio.ufsm.br/handle/1/5884 |
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