Aplicação de espectroscopia raman e análise multivariada na caracterização e monitoramento in situ da síntese de cocristais de carbamazepina-nicotinamida e ibuprofenonicotinamida
Autor(a) principal: | |
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Data de Publicação: | 2014 |
Tipo de documento: | Dissertação |
Idioma: | por |
Título da fonte: | Repositório Institucional da UFSCAR |
Texto Completo: | https://repositorio.ufscar.br/handle/ufscar/6592 |
Resumo: | In this work, the PAT tools were used (Raman spectroscopy with an in situ analyzer and multivariate tools) to proceed a crystallization monitoring and quantification of cocrystals of carbamazepine nicotinamide (CBZ NCT) and ibuprofen nicotinamide (IBP NCT). At first, it was performed the cocrystals syntheses that would be used as standard cocrystal during the course of this work, employing a method described in the literature. These crystals were characterized by differential scanning calorimetry (DSC), powder X-ray diffraction (PXRD), mid-infrared (MIR) and Raman spectroscopy. After the confirmation of the crystalline structure by the solid state analytical techniques, these crystals were used on a mixture design with three components (cocrystal, coformer A and coformer B) to develop an analytical curve employed in the quantification of the cocrystals. It was evaluated with the solid state analytical technique and quantification chemometrics methods, such as the PLS, which enabled a better cocrystal quantification among its coformers. Raman spectroscopy was the technique that presented the lowest error values, both in calibration and validation stages, with square mean errors of prediction ranging from 1.5 4.5 % for each analyte. For cocrystal synthesis and monitoring, it was used as a crystallization reaction procedure. Thus, it was prepared using a nicotinamide solution in water with a concentration near saturation level. This solution was added to the coformer, in solid state. The reactions were performed at different temperatures and monitored by the Raman spectroscopy. For both cocrystals, it was possible to observe a crystallization with a high yield from 60 °C, being the fact unpublished by the literature, since most of the cocrystallization reactions use organic solvents. The employment of multivariate curve resolution (MCR-ALS) enabled to observe distinctly the main points of the reaction, such as drugs dissolution, crystal nucleation and cocrystal crystallization, which can be easily employed on a routine procedure in the pharmaceutical industry. |
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Soares, Frederico Luis FelipeCarneiro, Renato Lajarimhttp://lattes.cnpq.br/8065852319463976http://lattes.cnpq.br/1064620847107189fa59ccb4-87bf-4263-a62e-c2264e6ac3d92016-06-02T20:36:52Z2014-09-182016-06-02T20:36:52Z2014-02-20SOARES, Frederico Luis Felipe. Raman spectroscopy and multivariate analysis in the characterization and in situ monitoring on synthesis of carbamazepine-nicotinamide and ibuprofen-nicotinamide cocrystals. 2014. 182 f. Dissertação (Mestrado em Ciências Exatas e da Terra) - Universidade Federal de São Carlos, São Carlos, 2014.https://repositorio.ufscar.br/handle/ufscar/6592In this work, the PAT tools were used (Raman spectroscopy with an in situ analyzer and multivariate tools) to proceed a crystallization monitoring and quantification of cocrystals of carbamazepine nicotinamide (CBZ NCT) and ibuprofen nicotinamide (IBP NCT). At first, it was performed the cocrystals syntheses that would be used as standard cocrystal during the course of this work, employing a method described in the literature. These crystals were characterized by differential scanning calorimetry (DSC), powder X-ray diffraction (PXRD), mid-infrared (MIR) and Raman spectroscopy. After the confirmation of the crystalline structure by the solid state analytical techniques, these crystals were used on a mixture design with three components (cocrystal, coformer A and coformer B) to develop an analytical curve employed in the quantification of the cocrystals. It was evaluated with the solid state analytical technique and quantification chemometrics methods, such as the PLS, which enabled a better cocrystal quantification among its coformers. Raman spectroscopy was the technique that presented the lowest error values, both in calibration and validation stages, with square mean errors of prediction ranging from 1.5 4.5 % for each analyte. For cocrystal synthesis and monitoring, it was used as a crystallization reaction procedure. Thus, it was prepared using a nicotinamide solution in water with a concentration near saturation level. This solution was added to the coformer, in solid state. The reactions were performed at different temperatures and monitored by the Raman spectroscopy. For both cocrystals, it was possible to observe a crystallization with a high yield from 60 °C, being the fact unpublished by the literature, since most of the cocrystallization reactions use organic solvents. The employment of multivariate curve resolution (MCR-ALS) enabled to observe distinctly the main points of the reaction, such as drugs dissolution, crystal nucleation and cocrystal crystallization, which can be easily employed on a routine procedure in the pharmaceutical industry.Neste trabalho foram utilizadas ferramentas do PAT (por meio da espectroscopia Raman com analisador in situ e ferramentas multivariadas) para realizar o monitoramento da cristalização e a quantificação dos cocristais de carbamazepina nicotinamida (CBZ NCT) e ibuprofeno nicotinamida (IBP NCT). Inicialmente, realizou-se a síntese dos cocristais, que seriam utilizados como padrão durante o trabalho, empregando-se um método descrito na literatura. Estes foram caracterizados por calorimetria diferencial de varredura (DSC), difração de raios-X (DRX), espectroscopias no infravermelho médio (IR) e Raman. Com a confirmação nova estrutura cristalina, pelos métodos analíticos de estado sólido, estes cristais foram utilizados em um planejamento de misturas com três componentes (cocristal, coformador A e coformador B) para desenvolver uma curva analítica usada na quantificação dos cocristais. Foi identificada a técnica analítica de estado sólido, que em conjunto com métodos quimiométricos de quantificação, como o PLS, possibilitaram uma melhor quantificação do cocristal em meio ao seus coformadores. A espectroscopia Raman foi a técnica que apresentou os menores valores de erro, tanto na etapa de calibração, quanto na etapa de predição, obtendo erros quadráticos médios de predição variando entre 1,5 4,5 % de cada analito. Para a síntese e monitoramento dos cocristais, utilizou-se um procedimento de reação de cristalização. Dessa forma, preparou-se uma solução aquosa de nicotinamida com concentração próxima a saturação. Essa solução foi adicionada ao outro coformador. As reações foram realizadas em diferentes temperaturas e monitoradas com espectroscopia Raman. Para ambos os cocristais, foi possível observar uma cocristalização com alto rendimento a partir de 60 °C, sendo este fato inédito na literatura, uma vez que a maior parte dos procedimentos de cocristalização utiliza solventes orgânicos. O emprego da resolução de curvas multivariadas (MCR-ALS) possibilitou observar distintamente os pontos de dissolução dos fármacos, nucleação e cristalização do cocristal, podendo ser empregado facilmente em uma procedimento de rotina na indústria farmacêutica.Financiadora de Estudos e Projetosapplication/pdfporUniversidade Federal de São CarlosPrograma de Pós-Graduação em Química - PPGQUFSCarBRQuímica analíticaCocristaisMonitoramentoQuimiometriaCarbamazepinaIbuprofenoCIENCIAS EXATAS E DA TERRA::QUIMICAAplicação de espectroscopia raman e análise multivariada na caracterização e monitoramento in situ da síntese de cocristais de carbamazepina-nicotinamida e ibuprofenonicotinamidaRaman spectroscopy and multivariate analysis in the characterization and in situ monitoring on synthesis of carbamazepine-nicotinamide and ibuprofen-nicotinamide cocrystalsinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesis-1-17727504b-c3a5-48cf-a36e-390bbf474c99info:eu-repo/semantics/openAccessreponame:Repositório Institucional da UFSCARinstname:Universidade Federal de São Carlos (UFSCAR)instacron:UFSCARORIGINAL6149.pdfapplication/pdf8760680https://repositorio.ufscar.br/bitstream/ufscar/6592/1/6149.pdfb15fcdb823e1f3450039918a56af46a3MD51TEXT6149.pdf.txt6149.pdf.txtExtracted texttext/plain0https://repositorio.ufscar.br/bitstream/ufscar/6592/4/6149.pdf.txtd41d8cd98f00b204e9800998ecf8427eMD54THUMBNAIL6149.pdf.jpg6149.pdf.jpgIM Thumbnailimage/jpeg9489https://repositorio.ufscar.br/bitstream/ufscar/6592/5/6149.pdf.jpg8b345f0fd4da743cd9945821fffaf8bcMD55ufscar/65922023-09-18 18:30:39.683oai:repositorio.ufscar.br:ufscar/6592Repositório 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 |
Aplicação de espectroscopia raman e análise multivariada na caracterização e monitoramento in situ da síntese de cocristais de carbamazepina-nicotinamida e ibuprofenonicotinamida |
dc.title.alternative.eng.fl_str_mv |
Raman spectroscopy and multivariate analysis in the characterization and in situ monitoring on synthesis of carbamazepine-nicotinamide and ibuprofen-nicotinamide cocrystals |
title |
Aplicação de espectroscopia raman e análise multivariada na caracterização e monitoramento in situ da síntese de cocristais de carbamazepina-nicotinamida e ibuprofenonicotinamida |
spellingShingle |
Aplicação de espectroscopia raman e análise multivariada na caracterização e monitoramento in situ da síntese de cocristais de carbamazepina-nicotinamida e ibuprofenonicotinamida Soares, Frederico Luis Felipe Química analítica Cocristais Monitoramento Quimiometria Carbamazepina Ibuprofeno CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Aplicação de espectroscopia raman e análise multivariada na caracterização e monitoramento in situ da síntese de cocristais de carbamazepina-nicotinamida e ibuprofenonicotinamida |
title_full |
Aplicação de espectroscopia raman e análise multivariada na caracterização e monitoramento in situ da síntese de cocristais de carbamazepina-nicotinamida e ibuprofenonicotinamida |
title_fullStr |
Aplicação de espectroscopia raman e análise multivariada na caracterização e monitoramento in situ da síntese de cocristais de carbamazepina-nicotinamida e ibuprofenonicotinamida |
title_full_unstemmed |
Aplicação de espectroscopia raman e análise multivariada na caracterização e monitoramento in situ da síntese de cocristais de carbamazepina-nicotinamida e ibuprofenonicotinamida |
title_sort |
Aplicação de espectroscopia raman e análise multivariada na caracterização e monitoramento in situ da síntese de cocristais de carbamazepina-nicotinamida e ibuprofenonicotinamida |
author |
Soares, Frederico Luis Felipe |
author_facet |
Soares, Frederico Luis Felipe |
author_role |
author |
dc.contributor.authorlattes.por.fl_str_mv |
http://lattes.cnpq.br/1064620847107189 |
dc.contributor.author.fl_str_mv |
Soares, Frederico Luis Felipe |
dc.contributor.advisor1.fl_str_mv |
Carneiro, Renato Lajarim |
dc.contributor.advisor1Lattes.fl_str_mv |
http://lattes.cnpq.br/8065852319463976 |
dc.contributor.authorID.fl_str_mv |
fa59ccb4-87bf-4263-a62e-c2264e6ac3d9 |
contributor_str_mv |
Carneiro, Renato Lajarim |
dc.subject.por.fl_str_mv |
Química analítica Cocristais Monitoramento Quimiometria Carbamazepina Ibuprofeno |
topic |
Química analítica Cocristais Monitoramento Quimiometria Carbamazepina Ibuprofeno CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.cnpq.fl_str_mv |
CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
In this work, the PAT tools were used (Raman spectroscopy with an in situ analyzer and multivariate tools) to proceed a crystallization monitoring and quantification of cocrystals of carbamazepine nicotinamide (CBZ NCT) and ibuprofen nicotinamide (IBP NCT). At first, it was performed the cocrystals syntheses that would be used as standard cocrystal during the course of this work, employing a method described in the literature. These crystals were characterized by differential scanning calorimetry (DSC), powder X-ray diffraction (PXRD), mid-infrared (MIR) and Raman spectroscopy. After the confirmation of the crystalline structure by the solid state analytical techniques, these crystals were used on a mixture design with three components (cocrystal, coformer A and coformer B) to develop an analytical curve employed in the quantification of the cocrystals. It was evaluated with the solid state analytical technique and quantification chemometrics methods, such as the PLS, which enabled a better cocrystal quantification among its coformers. Raman spectroscopy was the technique that presented the lowest error values, both in calibration and validation stages, with square mean errors of prediction ranging from 1.5 4.5 % for each analyte. For cocrystal synthesis and monitoring, it was used as a crystallization reaction procedure. Thus, it was prepared using a nicotinamide solution in water with a concentration near saturation level. This solution was added to the coformer, in solid state. The reactions were performed at different temperatures and monitored by the Raman spectroscopy. For both cocrystals, it was possible to observe a crystallization with a high yield from 60 °C, being the fact unpublished by the literature, since most of the cocrystallization reactions use organic solvents. The employment of multivariate curve resolution (MCR-ALS) enabled to observe distinctly the main points of the reaction, such as drugs dissolution, crystal nucleation and cocrystal crystallization, which can be easily employed on a routine procedure in the pharmaceutical industry. |
publishDate |
2014 |
dc.date.available.fl_str_mv |
2014-09-18 2016-06-02T20:36:52Z |
dc.date.issued.fl_str_mv |
2014-02-20 |
dc.date.accessioned.fl_str_mv |
2016-06-02T20:36:52Z |
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 |
SOARES, Frederico Luis Felipe. Raman spectroscopy and multivariate analysis in the characterization and in situ monitoring on synthesis of carbamazepine-nicotinamide and ibuprofen-nicotinamide cocrystals. 2014. 182 f. Dissertação (Mestrado em Ciências Exatas e da Terra) - Universidade Federal de São Carlos, São Carlos, 2014. |
dc.identifier.uri.fl_str_mv |
https://repositorio.ufscar.br/handle/ufscar/6592 |
identifier_str_mv |
SOARES, Frederico Luis Felipe. Raman spectroscopy and multivariate analysis in the characterization and in situ monitoring on synthesis of carbamazepine-nicotinamide and ibuprofen-nicotinamide cocrystals. 2014. 182 f. Dissertação (Mestrado em Ciências Exatas e da Terra) - Universidade Federal de São Carlos, São Carlos, 2014. |
url |
https://repositorio.ufscar.br/handle/ufscar/6592 |
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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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BR |
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Universidade Federal de São Carlos |
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