Aplicações de análises térmicas em fraude de alimentos e estudo de pré-formulação farmacêutica

Detalhes bibliográficos
Ano de defesa: 2017
Autor(a) principal: Brondi, Ariadne Missono lattes
Orientador(a): Trevisan, Marcello Garcia lattes
Banca de defesa: Figueiredo, Eduardo Costa De, Luiz, Jaine Honorato Hortolan, Schiavon, Marco Antônio, Carneiro, Renato Lajarim
Tipo de documento: Tese
Tipo de acesso: Acesso aberto
Idioma: por
Instituição de defesa: Universidade Federal de Alfenas
Programa de Pós-Graduação: Programa de Pós-Graduação em Química
Departamento: Instituto de Química
País: Brasil
Palavras-chave em Português:
Área do conhecimento CNPq:
Link de acesso: https://repositorio.unifal-mg.edu.br/handle/123456789/1184
Resumo: The thermal analysis techniques such as Differential Scanning Calorimetry (DSC), Thermogravimetry (TG) and Differential Thermal Analysis (DTA) are well-known techniques used in the physical-chemical characterization of different materials. The present work describes two different applications of thermal analysis: fraud in food and pharmaceutical pre-formulation study. In the first application, in food fraud, the study of the detection of coffee adulteration by corn was carried out. The adulteration of ground coffee has the purpose of generate higher profits, but also affects tis quality and changes its nutritional properties. In this case the adulteration of coffee by corn was detected and quantified using DSC and Infrared Spectroscopy coupled to PCA (Principal Component Analysis) and PLS (Partial Least Squares) models. The level of adulteration used was between 0.5 to 40% (w/w). The PCA models were able to differentiate adulterated samples from unadulterated ones, even at levels lower than 1% (w/w) of adulterant. PLS models showed a good correlation between predicted and reference values, with RMSECV (Root Mean Square Error of Cross-Validation) lower than 3.5% for the model constructed with DSC data, and 2.7% for the model with infrared spectroscopy data. The second application involves pharmaceutical preformulation studies with the drugs amlodipine besylate and olmesartan medoxomil. Both of drugs are antihypertensives that can be administrated alone, in monotherapy, or in pharmaceutical association. In the development of a new drug is required knowledge of the physicochemical properties of the drug and excipients involved, and the formulation stability, so that the new product does not have properties and characteristics change over time, guaranteeing the safety, efficiency and product quality. At first, DSC data were used to determine the thermokinetic and thermodynamic parameters of the drugs and to perform the drug-excipient compatibility study by analyzing binary mixtures of the drugs and excipients 1:1 (w/w). Binary mixtures of drugs and excipients 1:1 (w/w), and ternary mixtures containing the drugs amlodipine and olmesartan, and excipients 1:1:1 (w/w/w) were analyzed by FTIR with heating. Binary mixtures of each drug with excipient in a proportion of 1:1 (w/w), and ternary mixtures, containing drugs: amlodipine besylate and olmesartan medoxomil, and excipients in a proportion of 1:4:5 (w/w/w), were analyzed by HPLC (High Performance Liquid Chromatography) immediately after preparation and after being stored in stability chamber at 40±1 ºC and 75±5% of relative humity (RH) for 3 and 6 months, and at 40±1 ºC and dry conditions for 3 and 6 months, in order to compare the results obtained by DSC and FTIR. The excipients tested were pregelatinized starch, cellulose, croscarmellose sodium, magnesium stearate, polyvinyl alcohol, titanium dioxide, talc, polyvinylpyrrolidone, lactose and polyethylene glycol. According to the results obtained by DSC, FTIR with heating and HPLC it was possible to observe that the storage conditions are crucial for the stability of the formulation. In all cases, amlodipine proved to be incompatible with starch, olmesartan with PVP and lactose, and the pharmaceutical association with starch, cellulose, croscarmellose sodium, magnesium stearate, polyvinyl alcohol, PVP, lactose and PEG.
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spelling Brondi, Ariadne Missonohttp://lattes.cnpq.br/6509414402989975Trevisan, Jerusa Simone GarciaFigueiredo, Eduardo Costa DeLuiz, Jaine Honorato HortolanSchiavon, Marco AntônioCarneiro, Renato LajarimTrevisan, Marcello Garciahttp://lattes.cnpq.br/24730039817438492018-08-02T20:24:18Z2017-01-27BRONDI, Ariadne Missono. Aplicações de análises térmicas em fraude de alimentos e estudo de pré-formulação farmacêutica. 2017. 155 f. Tese (Doutorado em Química) - Universidade Federal de Alfenas, Alfenas, MG, 2017.https://repositorio.unifal-mg.edu.br/handle/123456789/1184The thermal analysis techniques such as Differential Scanning Calorimetry (DSC), Thermogravimetry (TG) and Differential Thermal Analysis (DTA) are well-known techniques used in the physical-chemical characterization of different materials. The present work describes two different applications of thermal analysis: fraud in food and pharmaceutical pre-formulation study. In the first application, in food fraud, the study of the detection of coffee adulteration by corn was carried out. The adulteration of ground coffee has the purpose of generate higher profits, but also affects tis quality and changes its nutritional properties. In this case the adulteration of coffee by corn was detected and quantified using DSC and Infrared Spectroscopy coupled to PCA (Principal Component Analysis) and PLS (Partial Least Squares) models. The level of adulteration used was between 0.5 to 40% (w/w). The PCA models were able to differentiate adulterated samples from unadulterated ones, even at levels lower than 1% (w/w) of adulterant. PLS models showed a good correlation between predicted and reference values, with RMSECV (Root Mean Square Error of Cross-Validation) lower than 3.5% for the model constructed with DSC data, and 2.7% for the model with infrared spectroscopy data. The second application involves pharmaceutical preformulation studies with the drugs amlodipine besylate and olmesartan medoxomil. Both of drugs are antihypertensives that can be administrated alone, in monotherapy, or in pharmaceutical association. In the development of a new drug is required knowledge of the physicochemical properties of the drug and excipients involved, and the formulation stability, so that the new product does not have properties and characteristics change over time, guaranteeing the safety, efficiency and product quality. At first, DSC data were used to determine the thermokinetic and thermodynamic parameters of the drugs and to perform the drug-excipient compatibility study by analyzing binary mixtures of the drugs and excipients 1:1 (w/w). Binary mixtures of drugs and excipients 1:1 (w/w), and ternary mixtures containing the drugs amlodipine and olmesartan, and excipients 1:1:1 (w/w/w) were analyzed by FTIR with heating. Binary mixtures of each drug with excipient in a proportion of 1:1 (w/w), and ternary mixtures, containing drugs: amlodipine besylate and olmesartan medoxomil, and excipients in a proportion of 1:4:5 (w/w/w), were analyzed by HPLC (High Performance Liquid Chromatography) immediately after preparation and after being stored in stability chamber at 40±1 ºC and 75±5% of relative humity (RH) for 3 and 6 months, and at 40±1 ºC and dry conditions for 3 and 6 months, in order to compare the results obtained by DSC and FTIR. The excipients tested were pregelatinized starch, cellulose, croscarmellose sodium, magnesium stearate, polyvinyl alcohol, titanium dioxide, talc, polyvinylpyrrolidone, lactose and polyethylene glycol. According to the results obtained by DSC, FTIR with heating and HPLC it was possible to observe that the storage conditions are crucial for the stability of the formulation. In all cases, amlodipine proved to be incompatible with starch, olmesartan with PVP and lactose, and the pharmaceutical association with starch, cellulose, croscarmellose sodium, magnesium stearate, polyvinyl alcohol, PVP, lactose and PEG.As técnicas de análise térmica, como a Calorimetria Exploratória Diferencial (DSC), Termogravimetria (TG) e Análise Térmica Diferencial (DTA) são técnicas bem conhecidas utilizadas na caracterização físico-química de diferentes materiais. O presente trabalho descreve duas diferentes aplicações das análises térmicas: fraudes de alimentos e estudo de pré-formulação farmacêutica. Na primeira aplicação, em fraude de alimentos, foi realizado o estudo da detecção de adulteração do café por milho. As fraudes em café moído têm a finalidade de gerar mais lucro, mas também afeta a sua qualidade e altera suas propriedades nutricionais. Neste caso a adulteração do café por milho foi detectada e quantificada utilizando DSC e Espectroscopia no Infravermelho juntamente com modelos PCA (Análise de Componentes Principais) e PLS (Quadrados Mínimos Parciais). O nível de adulteração utilizada foi de 0,5 a 40% (m/m). Os modelos PCA foram capazes de diferenciar amostras adulteradas de não adulteradas, inclusive em níveis inferiores a 1% (m/m) de adulterante. Os modelos PLS apresentaram boa correlação entre os valores previstos e de referência, com RMSECV (Erro quadrático médio de validação cruzada) inferior a 3,5% para o modelo construído com os dados de DSC, e 2,7% para o modelo com dados de Espectroscopia no Infravermelho. A segunda aplicação envolve estudos de pré-formulação farmacêutica, tendo como alvos os fármacos besilato de anlodipino e olmesartana medoxomila. Ambos são medicamentos antihipertensivos que podem ser administrados isoladamente, em monoterapia, ou em associação farmacêutica. No desenvolvimento de um novo medicamento é necessário o conhecimento de propriedades físico-químicas do fármaco e dos excipientes envolvidos, e a estabilidade da formulação, a fim de que o novo medicamento não tenha suas propriedades e características alteradas ao longo do tempo, garantindo a segurança, eficácia e qualidade do produto. Primeiramente, os dados obtidos por DSC foram utilizados para determinar os parâmetros termocinéticos e termodinâmicos dos fármacos, e realizar o estudo de compatibilidade fármaco-excipiente, pela análise de misturas binárias 1:1 (m/m) dos fármacos e excipientes. Por FTIR com aquecimento foram analisadas misturas binárias 1:1 (m/m) dos fármacos e excipientes, e misturas ternárias 1:1:1 (m/m) contendo os fármacos anlodipino e olmesartana, e excipientes. Misturas binárias de cada fármaco com os excipientes na proporção 1:1 (m/m), e misturas ternárias, contendo os fármacos: besilato de anlodipino e olmesartana medoxomila, e excipientes na proporção 1:4:5 (m/m/m), foram analisadas por HPLC (Cromatografia Líquida de Alta Eficiência) logo após o seu preparo e após serem armazenadas em câmara de estabilidade a 40±1 ºC e 75±5% de umidade relativa (UR) por 3 e 6 meses, e a 40±1 ºC a seco por 3 e 6 meses, com a finalidade de confrontar os resultados obtidos por DSC e FTIR. Os excipientes testados foram amido pré-gelatinizado, celulose, croscarmelose sódica, estearato de magnésio, álcool polivinílico, dióxido de titânio, talco, polivinilpirrolidona, lactose e polietilenoglicol. De acordo com os resultados obtidos por DSC, FTIR com aquecimento e HPLC foi possível observar que as condições de armazenamento são cruciais para a estabilidade da formulação. Sendo que em todos os casos o anlodipino se mostrou incompatível com o amido, a olmesartana com o PVP e lactose, e a associação farmacêutica com amido, celulose, croscarmelose, estearato de magnésio, álcool polivinílico, PVP, lactose e PEG.Coordenação de Aperfeiçoamento de Pessoal de Nível Superior - CAPESapplication/pdfporUniversidade Federal de AlfenasPrograma de Pós-Graduação em QuímicaUNIFAL-MGBrasilInstituto de Químicainfo:eu-repo/semantics/openAccesshttp://creativecommons.org/licenses/by-nc-nd/4.0/Análise termicaAnálise MultivariadaFraudeCaféPreparação FarmacêuticasCombinação Besilato de Anlodipino e Olmesartana MedoxomilaQUIMICA::QUIMICA ANALITICAAplicações de análises térmicas em fraude de alimentos e estudo de pré-formulação farmacêuticainfo:eu-repo/semantics/doctoralThesisinfo:eu-repo/semantics/publishedVersion1328253078826782306600600600-86616021054614395492075167498588264571reponame:Repositório Institucional da Universidade Federal de Alfenas - RiUnifalinstname:Universidade Federal de Alfenas (UNIFAL)instacron:UNIFALBrondi, Ariadne MissonoLICENSElicense.txtlicense.txttext/plain; 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dc.title.pt-BR.fl_str_mv Aplicações de análises térmicas em fraude de alimentos e estudo de pré-formulação farmacêutica
title Aplicações de análises térmicas em fraude de alimentos e estudo de pré-formulação farmacêutica
spellingShingle Aplicações de análises térmicas em fraude de alimentos e estudo de pré-formulação farmacêutica
Brondi, Ariadne Missono
Análise termica
Análise Multivariada
Fraude
Café
Preparação Farmacêuticas
Combinação Besilato de Anlodipino e Olmesartana Medoxomila
QUIMICA::QUIMICA ANALITICA
title_short Aplicações de análises térmicas em fraude de alimentos e estudo de pré-formulação farmacêutica
title_full Aplicações de análises térmicas em fraude de alimentos e estudo de pré-formulação farmacêutica
title_fullStr Aplicações de análises térmicas em fraude de alimentos e estudo de pré-formulação farmacêutica
title_full_unstemmed Aplicações de análises térmicas em fraude de alimentos e estudo de pré-formulação farmacêutica
title_sort Aplicações de análises térmicas em fraude de alimentos e estudo de pré-formulação farmacêutica
author Brondi, Ariadne Missono
author_facet Brondi, Ariadne Missono
author_role author
dc.contributor.author.fl_str_mv Brondi, Ariadne Missono
dc.contributor.advisor1Lattes.fl_str_mv http://lattes.cnpq.br/6509414402989975
dc.contributor.advisor-co1.fl_str_mv Trevisan, Jerusa Simone Garcia
dc.contributor.referee1.fl_str_mv Figueiredo, Eduardo Costa De
dc.contributor.referee2.fl_str_mv Luiz, Jaine Honorato Hortolan
dc.contributor.referee3.fl_str_mv Schiavon, Marco Antônio
dc.contributor.referee4.fl_str_mv Carneiro, Renato Lajarim
dc.contributor.advisor1.fl_str_mv Trevisan, Marcello Garcia
dc.contributor.authorLattes.fl_str_mv http://lattes.cnpq.br/2473003981743849
contributor_str_mv Trevisan, Jerusa Simone Garcia
Figueiredo, Eduardo Costa De
Luiz, Jaine Honorato Hortolan
Schiavon, Marco Antônio
Carneiro, Renato Lajarim
Trevisan, Marcello Garcia
dc.subject.por.fl_str_mv Análise termica
Análise Multivariada
Fraude
Café
Preparação Farmacêuticas
Combinação Besilato de Anlodipino e Olmesartana Medoxomila
topic Análise termica
Análise Multivariada
Fraude
Café
Preparação Farmacêuticas
Combinação Besilato de Anlodipino e Olmesartana Medoxomila
QUIMICA::QUIMICA ANALITICA
dc.subject.cnpq.fl_str_mv QUIMICA::QUIMICA ANALITICA
description The thermal analysis techniques such as Differential Scanning Calorimetry (DSC), Thermogravimetry (TG) and Differential Thermal Analysis (DTA) are well-known techniques used in the physical-chemical characterization of different materials. The present work describes two different applications of thermal analysis: fraud in food and pharmaceutical pre-formulation study. In the first application, in food fraud, the study of the detection of coffee adulteration by corn was carried out. The adulteration of ground coffee has the purpose of generate higher profits, but also affects tis quality and changes its nutritional properties. In this case the adulteration of coffee by corn was detected and quantified using DSC and Infrared Spectroscopy coupled to PCA (Principal Component Analysis) and PLS (Partial Least Squares) models. The level of adulteration used was between 0.5 to 40% (w/w). The PCA models were able to differentiate adulterated samples from unadulterated ones, even at levels lower than 1% (w/w) of adulterant. PLS models showed a good correlation between predicted and reference values, with RMSECV (Root Mean Square Error of Cross-Validation) lower than 3.5% for the model constructed with DSC data, and 2.7% for the model with infrared spectroscopy data. The second application involves pharmaceutical preformulation studies with the drugs amlodipine besylate and olmesartan medoxomil. Both of drugs are antihypertensives that can be administrated alone, in monotherapy, or in pharmaceutical association. In the development of a new drug is required knowledge of the physicochemical properties of the drug and excipients involved, and the formulation stability, so that the new product does not have properties and characteristics change over time, guaranteeing the safety, efficiency and product quality. At first, DSC data were used to determine the thermokinetic and thermodynamic parameters of the drugs and to perform the drug-excipient compatibility study by analyzing binary mixtures of the drugs and excipients 1:1 (w/w). Binary mixtures of drugs and excipients 1:1 (w/w), and ternary mixtures containing the drugs amlodipine and olmesartan, and excipients 1:1:1 (w/w/w) were analyzed by FTIR with heating. Binary mixtures of each drug with excipient in a proportion of 1:1 (w/w), and ternary mixtures, containing drugs: amlodipine besylate and olmesartan medoxomil, and excipients in a proportion of 1:4:5 (w/w/w), were analyzed by HPLC (High Performance Liquid Chromatography) immediately after preparation and after being stored in stability chamber at 40±1 ºC and 75±5% of relative humity (RH) for 3 and 6 months, and at 40±1 ºC and dry conditions for 3 and 6 months, in order to compare the results obtained by DSC and FTIR. The excipients tested were pregelatinized starch, cellulose, croscarmellose sodium, magnesium stearate, polyvinyl alcohol, titanium dioxide, talc, polyvinylpyrrolidone, lactose and polyethylene glycol. According to the results obtained by DSC, FTIR with heating and HPLC it was possible to observe that the storage conditions are crucial for the stability of the formulation. In all cases, amlodipine proved to be incompatible with starch, olmesartan with PVP and lactose, and the pharmaceutical association with starch, cellulose, croscarmellose sodium, magnesium stearate, polyvinyl alcohol, PVP, lactose and PEG.
publishDate 2017
dc.date.issued.fl_str_mv 2017-01-27
dc.date.accessioned.fl_str_mv 2018-08-02T20:24:18Z
dc.type.driver.fl_str_mv info:eu-repo/semantics/doctoralThesis
dc.type.status.fl_str_mv info:eu-repo/semantics/publishedVersion
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identifier_str_mv BRONDI, Ariadne Missono. Aplicações de análises térmicas em fraude de alimentos e estudo de pré-formulação farmacêutica. 2017. 155 f. Tese (Doutorado em Química) - Universidade Federal de Alfenas, Alfenas, MG, 2017.
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