Orientador: Ronei Jesus Poppi / Tese (doutorado) - Universidade Estadual de Campinas, Instituto de Química / Made available in DSpace on 2018-08-24T05:27:34Z (GMT). No. of bitstreams: 1 Breitkreitz_MarciaCristina_D.pdf: 4580305 bytes, checksum: 77a15e51b9d1be694cc7c5db18fa63bb (MD5) Previous issue date: 2013 / Resumo: Este trabalho teve como objetivo demonstrar como a espectroscopia NIR e Raman de imagem, juntamente com diversos métodos quimiométricos podem auxiliar a tomada de decisões durante o desenvolvimento farmacêutico de formulações de fármacos pouco solúveis em água, tendo como modelo a atorvastatina cálcica. Foram avaliados dois excipientes inovadores, o Gelucire® 44/14 e o Soluplus® que serviram de base para o desenvolvimento das formulações. O Gelucire® 44/14 foi utilizado para o preparo de dispersões sólidas pelos métodos da fusão e da evaporação do solvente e formulações do tipo SEDDS (Self-Emulsifying drug Delivery Sytems), enquanto o Soluplus® foi utilizado para o preparo de dispersões sólidas pelo método da evaporação do solvente. Nas dispersões preparadas pelo método da fusão foram observados aglomerados do fármaco, enquanto o método de evaporação do solvente apresentou melhor homogeneidade na distribuição dos componentes, porém a amostra se apresentou enrijecida após a secagem. Com as formulacoes SEDDS foi possível contornar estes problemas. Foram obtidas dispersões sólidas homogêneas de atorvastatina em Soluplus® utilizando etanol como solvente e lactose como diluente. As imagens foram geradas por calibração univariada, análise de componentes principais (PCA), regressão em mínimos quadrados clássicos (CLS) e regressão em mínimos quadrados parciais (PLS) e os resultados foram comparados. O método CLS foi estudado com mais detalhes devido às suas vantagens para utilização na pesquisa farmacêutica. Os principais fatores que levaram à problemas de exatidão com este método foram identificados e procedimentos para contorná-los foram apresentados e discutidos. / Abstract: The aim of this work was to demonstrate how NIR and Raman image spectroscopy associated with different chemometric methods can support decision making during pharmaceutical development of formulations of low water soluble drugs, using atorvastatin calcium as a model drug. Two innovative excipientes were used, Gelucire® 44/14 and Soluplus®. The former was used to prepare solid dispersions by both hot melt and solvent evaporation methods and to formulate Self Emulsifying Drug Delivery Systems (SEDDS). The latter was used to prepare solid dispersions by the solvent evaporation method. In solid dispersions prepared by the hot melt method it was observed lumps of the drug, whereas the solvent evaporation method presented more homogeneous distribution of the components, even though the sample became stiffened after drying. By preparing SEDDS formulations, it was possible to overcome these problems. A homogeneous solid dispersion of atorvastatin in Soluplus® was achieved by using ethanol as solvent and lactose as diluent. Chemical images were generated by univariate calibration, principal component analysis (PCA), classical least squares (CLS) and partial least squares (PLS). The capability of these methods to generate chemical images were compared. CLS method was studied more carefully due to its advantages for pharmaceutical research use. The main features that lead to accuracy issues were identified both in Raman and in NIR spectroscopy and procedures to overcome them were presented and discussed. / Doutorado / Quimica Analitica / Doutora em Ciências

The master thesis deals with determination of selected biochemicals (lignin, carotenoids, water) content in Norway spruce needles using laboratory and imaging spectroscopy. The first part of thesis summarizes literature dealing with methods of estimating lignin and other biochemicals content. Three types of data are used in this thesis: 1. spectra measured by contact probe and ASD FieldSpec 4 Wide Res spectroradiometer, 2. spectra measured by integrating sphere and spectroradiometer and 3. aerial hyperspectral image data acquired by APEX sensor. The most useful transformation methods - first derivative and continuum removal are applied to the spectrum. Further the linear relationship between measured spectrum and content of biochemicals is analysed. Stepwise multiple linear regression is applied to select suitable wavelengths for modeling of biochemicals content in spruce needles. The model is also calculated and applied on the level of image hyperspectral data. Maps of lignin content in Norway spruce are the final output of these part of this. Next part of the thesis compares spectra measured by contact probe and spectra measured by integrating sphere. Diffrerence between the studied areas based on biochemicals content in spruce needles and several chemical elements in the soil and based on...

The main purpose of this thesis is to use Image Spectroscopy as a tool to monitor the environmental conditions in a region affected by anthropogenic activities via estimating both geochemical and biochemical parameters on a regional scale. The research has been carried on the Sokolov lignite mine, NW Bohemia, a region affected by long-term extensive mining. The thesis is divided into two thematic parts. First part is devoted to applications of Image Spectroscopy into Acid Mine Drainage mapping and its related issues (chapters 2 and 3). In chapter 2 the equivalent mineral end-members were successfully derived from the ASTER image data (Advanced Space-borne Thermal Emission and Reflection Radiometer satellite data). In the chapter 3 the pH was estimated on the basis of mineral and image spectroscopy. The Multi Range Spectral Feature Fitting (MRSFF) technique was utilized for mineral mapping and the multiple regression model using the fit images, the results of MRSFF, as inputs was constructed to estimate the surface pH and statistical significant accuracy was attained. In the second thematic part (chapters 4-6) Image Spectroscopy is applied into monitoring of vegetation stress. A new statistical method was developed to assess the physiological status of macroscopically undamaged foliage of Norway...

The aim of this study was to propose a non-destructive method for measuring Pinus sylvestris seedlings, to determine whether water stress would be evident in laboratory spectra of pines, to compare whether the response of pines would differ by ecotype, and to investigate whether two ecotypes of Pinus sylvestris could be distinguished using laboratory and image spectroscopy. For these purposes, hyperspectral images of seed orchards from August 2020 were processed and a three-month laboratory experiment was conducted, in which stress from water deficit was induced in two-year-old pine seedlings from the upland and hilly ecotypes. Spectral data were analysed using mixed statistical models, analysis of variance, principal component analysis, training of supervised pixel classifiers, vegetation indices, and linear regression. Based on the analyses, it was found that water stress can be detected in severely stressed Pinus sylvestris seedlings. The most sensitive spectral bands to water content were observed in the region between 1000-2500 nm. The initial response to water stress did not differ by ecotype, but a faster recovery was observed at the upland ecotype after the period of draught. The two Pinus sylvestris ecotypes were distinguished with high accuracy from both laboratory and image spectral...