Desenvolvimento e validação de metodologias para avaliação de etoricoxibe por cromatografia líquida e espectrometria de massas
Autor(a) principal: | |
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Data de Publicação: | 2006 |
Tipo de documento: | Dissertação |
Idioma: | por |
Título da fonte: | Manancial - Repositório Digital da UFSM |
Texto Completo: | http://repositorio.ufsm.br/handle/1/6000 |
Resumo: | Etoricoxib is a non-steroidal anti-inflammatory drug, from the coxibs group, that represents a second-generation of COX-2 inhibitors, used for the treatment of arthritis and pain. The methodologies for the evaluation of etoricoxib in pharmaceutical products and plasma were developed and validated in the present work. The reversed-phase liquid chromatography (RP-LC) analysis was carried out using a Synergi fusion C18 column (150 mm x 4.6 mm), maintained at a controlled-ambient temperature. The mobile phase consisted of phosphoric acid 0.01 M, pH 3.0/acetonitrile (62:38, V/V), run at a flow rate of 1.0 mL/min with detection at 234 nm. The chromatographic separation was obtained within 7.0 min and it was linear in the concentration range of 0.02-150 µg/mL. The liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated using a Luna C18 column (50 mm x 3.0 mm), maintained at 40 ºC and the mobile phase consisted of acetonitrile:water (95:5, V/V)/ 0.1% acetic acid (90:10, V/V), run at flow rate of 0.4 mL/min. The mass spectrometer, equipped with electrospray positive source, was used in multiple reaction monitoring mode (MRM), monitoring the transitions of 359.3>280.0 and 332.0>95.0, for etoricoxib and piroxicam (internal standard), respectively. The chromatographic separation was obtained within 2.0 min and it was linear in the concentration range of 1-5000 ng/mL. The procedures were validated evaluating parameters such as the specificity, linearity, precision, accuracy, robustness, limit of detection and limit of quantitation. Besides, for the bioanalytical method, the matrix effects, recovery and stability studies were also analyzed, giving results within the acceptable range. The proposed methods were applied for the analysis of pharmaceutical products, showing significant correlation (r=0.9999) of the results. Moreover, the liquid-liquid and solid phase extraction methods developed and optimized allowed high mean recoveries of etoricoxib and internal standard from the plasma samples. The procedures can be applied for the biovailability studies and for the quality control of pharmaceutical products. |
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Desenvolvimento e validação de metodologias para avaliação de etoricoxibe por cromatografia líquida e espectrometria de massasDevelopment and validation of methodologies for the evaluation of etoricoxib by liquid chromatography and mass spectrometryCromatografia líquidaEspectrometria de massasEtoricoxibeValidaçãoPlasma humanoProdutos farmacêuticosLiquid chromatographyMass spectrometryEtoricoxibValidationHuman plasmaPharmaceutical productsCNPQ::CIENCIAS DA SAUDE::FARMACIAEtoricoxib is a non-steroidal anti-inflammatory drug, from the coxibs group, that represents a second-generation of COX-2 inhibitors, used for the treatment of arthritis and pain. The methodologies for the evaluation of etoricoxib in pharmaceutical products and plasma were developed and validated in the present work. The reversed-phase liquid chromatography (RP-LC) analysis was carried out using a Synergi fusion C18 column (150 mm x 4.6 mm), maintained at a controlled-ambient temperature. The mobile phase consisted of phosphoric acid 0.01 M, pH 3.0/acetonitrile (62:38, V/V), run at a flow rate of 1.0 mL/min with detection at 234 nm. The chromatographic separation was obtained within 7.0 min and it was linear in the concentration range of 0.02-150 µg/mL. The liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated using a Luna C18 column (50 mm x 3.0 mm), maintained at 40 ºC and the mobile phase consisted of acetonitrile:water (95:5, V/V)/ 0.1% acetic acid (90:10, V/V), run at flow rate of 0.4 mL/min. The mass spectrometer, equipped with electrospray positive source, was used in multiple reaction monitoring mode (MRM), monitoring the transitions of 359.3>280.0 and 332.0>95.0, for etoricoxib and piroxicam (internal standard), respectively. The chromatographic separation was obtained within 2.0 min and it was linear in the concentration range of 1-5000 ng/mL. The procedures were validated evaluating parameters such as the specificity, linearity, precision, accuracy, robustness, limit of detection and limit of quantitation. Besides, for the bioanalytical method, the matrix effects, recovery and stability studies were also analyzed, giving results within the acceptable range. The proposed methods were applied for the analysis of pharmaceutical products, showing significant correlation (r=0.9999) of the results. Moreover, the liquid-liquid and solid phase extraction methods developed and optimized allowed high mean recoveries of etoricoxib and internal standard from the plasma samples. The procedures can be applied for the biovailability studies and for the quality control of pharmaceutical products.Etoricoxibe é um antiinflamatório não esteroidal, pertencente ao grupo dos coxibes, que representa a segunda geração dos inibidores seletivos da cicloxigenase-2. É indicado para o tratamento de artrites e dor aguda. No presente trabalho foram desenvolvidas e validadas metodologias para avaliação de etoricoxibe em produtos farmacêuticos e plasma humano. As análises por cromatografia líquida em fase reversa (CL-FR) foram realizadas utilizando coluna Synergi fusion C18 (150 mm x 4,6 mm), mantida a temperatura ambiente. A fase móvel foi composta de ácido fosfórico 0,01 M, pH 3,0/acetonitrila (62:38, V/V) na vazão de 1,0 mL/min e detecção no ultravioleta a 234 nm. A separação cromatográfica foi obtida no tempo de 7 minutos, sendo linear na faixa de concentração de 0,02-150 µg/mL. Paralelamente, desenvolveu-se e validou-se método por cromatografia líquida combinada à espectrometria de massas (CL-EM/EM). Realizaram-se as análises utilizando Luna C18 (50 mm x 4,6 mm), mantida a 40 ºC e fase móvel composta de acetonitrila:água (95:5, V/V)/ 0,1% ácido acético (90:10, V/V), na vazão de 0,4 mL/min. O espectrômetro de massas, equipado com fonte de electrospray positivo, foi empregado no modo de monitoramento de reação múltipla (MRM), monitorando as transições de 359,3>280,0 e 332,0>95,0, para o etoricoxibe e piroxicam (padrão interno), respectivamente. A separação cromatográfica foi obtida em 2 minutos, sendo linear na faixa de concentração de 1-5000 ng/mL. Os procedimentos foram validados, avaliando-se os parâmetros de especificidade, linearidade, precisão, exatidão, robustez, limite de detecção e quantificação, incluindo para o método bioanalítico os efeitos de matriz, a recuperação e estudos de estabilidade, cujos resultados cumpriram os requisitos preconizados. Os métodos propostos foram utilizados na análise de produtos farmacêuticos, demonstrando correlação significativa dos resultados (r=0,9999). Além disso, os métodos de extração líquido-líquido e em fase sólida desenvolvidos e otimizados propiciaram significativas percentagens de recuperação do etoricoxibe e do padrão interno nas amostras de plasma. Os procedimentos pesquisados podem ser aplicados para estudos de biodisponibilidade e para aprimorar o controle da qualidade de medicamentos.Universidade Federal de Santa MariaBRFarmáciaUFSMPrograma de Pós-Graduação em Ciências FarmacêuticasDalmora, Sergio Luizhttp://lattes.cnpq.br/4505166045049607Costa, Teresa Cristina Tavares Dallahttp://lattes.cnpq.br/3345924324711668Moreno, Ronilson Agnaldohttp://lattes.cnpq.br/8740270217909480Brum Junior, Liberato2006-08-142006-08-142006-05-31info:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisapplication/pdfapplication/pdfBRUM JUNIOR, Liberato. Development and validation of methodologies for the evaluation of etoricoxib by liquid chromatography and mass spectrometry. 2006. 116 f. Dissertação (Mestrado em Farmacologia) - Universidade Federal de Santa Maria, Santa Maria, 2006.http://repositorio.ufsm.br/handle/1/6000porinfo:eu-repo/semantics/openAccessreponame:Manancial - Repositório Digital da UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSM2022-10-11T12:59:24Zoai:repositorio.ufsm.br:1/6000Biblioteca Digital de Teses e Dissertaçõeshttps://repositorio.ufsm.br/ONGhttps://repositorio.ufsm.br/oai/requestatendimento.sib@ufsm.br||tedebc@gmail.comopendoar:2022-10-11T12:59:24Manancial - Repositório Digital da UFSM - Universidade Federal de Santa Maria (UFSM)false |
dc.title.none.fl_str_mv |
Desenvolvimento e validação de metodologias para avaliação de etoricoxibe por cromatografia líquida e espectrometria de massas Development and validation of methodologies for the evaluation of etoricoxib by liquid chromatography and mass spectrometry |
title |
Desenvolvimento e validação de metodologias para avaliação de etoricoxibe por cromatografia líquida e espectrometria de massas |
spellingShingle |
Desenvolvimento e validação de metodologias para avaliação de etoricoxibe por cromatografia líquida e espectrometria de massas Brum Junior, Liberato Cromatografia líquida Espectrometria de massas Etoricoxibe Validação Plasma humano Produtos farmacêuticos Liquid chromatography Mass spectrometry Etoricoxib Validation Human plasma Pharmaceutical products CNPQ::CIENCIAS DA SAUDE::FARMACIA |
title_short |
Desenvolvimento e validação de metodologias para avaliação de etoricoxibe por cromatografia líquida e espectrometria de massas |
title_full |
Desenvolvimento e validação de metodologias para avaliação de etoricoxibe por cromatografia líquida e espectrometria de massas |
title_fullStr |
Desenvolvimento e validação de metodologias para avaliação de etoricoxibe por cromatografia líquida e espectrometria de massas |
title_full_unstemmed |
Desenvolvimento e validação de metodologias para avaliação de etoricoxibe por cromatografia líquida e espectrometria de massas |
title_sort |
Desenvolvimento e validação de metodologias para avaliação de etoricoxibe por cromatografia líquida e espectrometria de massas |
author |
Brum Junior, Liberato |
author_facet |
Brum Junior, Liberato |
author_role |
author |
dc.contributor.none.fl_str_mv |
Dalmora, Sergio Luiz http://lattes.cnpq.br/4505166045049607 Costa, Teresa Cristina Tavares Dalla http://lattes.cnpq.br/3345924324711668 Moreno, Ronilson Agnaldo http://lattes.cnpq.br/8740270217909480 |
dc.contributor.author.fl_str_mv |
Brum Junior, Liberato |
dc.subject.por.fl_str_mv |
Cromatografia líquida Espectrometria de massas Etoricoxibe Validação Plasma humano Produtos farmacêuticos Liquid chromatography Mass spectrometry Etoricoxib Validation Human plasma Pharmaceutical products CNPQ::CIENCIAS DA SAUDE::FARMACIA |
topic |
Cromatografia líquida Espectrometria de massas Etoricoxibe Validação Plasma humano Produtos farmacêuticos Liquid chromatography Mass spectrometry Etoricoxib Validation Human plasma Pharmaceutical products CNPQ::CIENCIAS DA SAUDE::FARMACIA |
description |
Etoricoxib is a non-steroidal anti-inflammatory drug, from the coxibs group, that represents a second-generation of COX-2 inhibitors, used for the treatment of arthritis and pain. The methodologies for the evaluation of etoricoxib in pharmaceutical products and plasma were developed and validated in the present work. The reversed-phase liquid chromatography (RP-LC) analysis was carried out using a Synergi fusion C18 column (150 mm x 4.6 mm), maintained at a controlled-ambient temperature. The mobile phase consisted of phosphoric acid 0.01 M, pH 3.0/acetonitrile (62:38, V/V), run at a flow rate of 1.0 mL/min with detection at 234 nm. The chromatographic separation was obtained within 7.0 min and it was linear in the concentration range of 0.02-150 µg/mL. The liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated using a Luna C18 column (50 mm x 3.0 mm), maintained at 40 ºC and the mobile phase consisted of acetonitrile:water (95:5, V/V)/ 0.1% acetic acid (90:10, V/V), run at flow rate of 0.4 mL/min. The mass spectrometer, equipped with electrospray positive source, was used in multiple reaction monitoring mode (MRM), monitoring the transitions of 359.3>280.0 and 332.0>95.0, for etoricoxib and piroxicam (internal standard), respectively. The chromatographic separation was obtained within 2.0 min and it was linear in the concentration range of 1-5000 ng/mL. The procedures were validated evaluating parameters such as the specificity, linearity, precision, accuracy, robustness, limit of detection and limit of quantitation. Besides, for the bioanalytical method, the matrix effects, recovery and stability studies were also analyzed, giving results within the acceptable range. The proposed methods were applied for the analysis of pharmaceutical products, showing significant correlation (r=0.9999) of the results. Moreover, the liquid-liquid and solid phase extraction methods developed and optimized allowed high mean recoveries of etoricoxib and internal standard from the plasma samples. The procedures can be applied for the biovailability studies and for the quality control of pharmaceutical products. |
publishDate |
2006 |
dc.date.none.fl_str_mv |
2006-08-14 2006-08-14 2006-05-31 |
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.uri.fl_str_mv |
BRUM JUNIOR, Liberato. Development and validation of methodologies for the evaluation of etoricoxib by liquid chromatography and mass spectrometry. 2006. 116 f. Dissertação (Mestrado em Farmacologia) - Universidade Federal de Santa Maria, Santa Maria, 2006. http://repositorio.ufsm.br/handle/1/6000 |
identifier_str_mv |
BRUM JUNIOR, Liberato. Development and validation of methodologies for the evaluation of etoricoxib by liquid chromatography and mass spectrometry. 2006. 116 f. Dissertação (Mestrado em Farmacologia) - Universidade Federal de Santa Maria, Santa Maria, 2006. |
url |
http://repositorio.ufsm.br/handle/1/6000 |
dc.language.iso.fl_str_mv |
por |
language |
por |
dc.rights.driver.fl_str_mv |
info:eu-repo/semantics/openAccess |
eu_rights_str_mv |
openAccess |
dc.format.none.fl_str_mv |
application/pdf application/pdf |
dc.publisher.none.fl_str_mv |
Universidade Federal de Santa Maria BR Farmácia UFSM Programa de Pós-Graduação em Ciências Farmacêuticas |
publisher.none.fl_str_mv |
Universidade Federal de Santa Maria BR Farmácia UFSM Programa de Pós-Graduação em Ciências Farmacêuticas |
dc.source.none.fl_str_mv |
reponame:Manancial - Repositório Digital da UFSM instname:Universidade Federal de Santa Maria (UFSM) instacron:UFSM |
instname_str |
Universidade Federal de Santa Maria (UFSM) |
instacron_str |
UFSM |
institution |
UFSM |
reponame_str |
Manancial - Repositório Digital da UFSM |
collection |
Manancial - Repositório Digital da UFSM |
repository.name.fl_str_mv |
Manancial - Repositório Digital da UFSM - Universidade Federal de Santa Maria (UFSM) |
repository.mail.fl_str_mv |
atendimento.sib@ufsm.br||tedebc@gmail.com |
_version_ |
1805922051384410112 |