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Braz. J. Pharm. Sci. (Online) ; 59: e20918, 2023. tab, graf
Article in English | LILACS | ID: biblio-1429951


Abstract Solubility of pharmaceutical drugs in organic solvents is one of the important parameters to understand the equilibrium concentration of solute-solvent, which helps optimize and design crystallization conditions to obtain the desired product crystals. In the present study, Chlorzoxazone (CHZ) is used as a model pharmaceutical compound to investigate the equilibrium solubility, the influence of solvent and the operating conditions on the shape, and the size distribution. The solubility of CHZ is determined in organic solvents like Isopropanol, Ethanol, and 2-Ethoxyethylacetate, Ethylacetate and Ethyllactate using shake flask method from -5ºC to 60ºC. The solubility of CHZ in these solvents shows an increasing trend as the temperature increases in the following order: ethyllactate + water (0.5+0.5) < ethylacetate < isopropanol < ethanol < 2-ethoxyethylacetate < ethyllactate + water (0.75+0.25). The solvents, isopropanol, ethanol, and ethyl lactate, produce needle-shaped crystals, while 2-ethoxyethylacetate and ethyl acetate tend to produce plate shaped crystals. CHZ crystals obtained from 2-ethoxyethylacetate tend to have plate shaped crystals with a lower aspect ratio and are selected for batch cooling crystallization experiments performed at different cooling rates, and agitation. It is found that the agitation at 300 rpm and the cooling rate 0.2ºC/min produce more uniform crystal size distribution

Solvents/classification , Chlorzoxazone/analysis , Crystallization/classification , Solubility , Pharmaceutical Preparations/administration & dosage
Braz. J. Pharm. Sci. (Online) ; 56: e18993, 2020. graf
Article in English | LILACS | ID: biblio-1249146


A repetitive batch process was employed followed by membrane ultrafiltration system to produce low-cost cyclodextrins (CDs) using commercial enzymes Toruzyme® cyclomaltodextrin glucanotransferase (CGTase) and its kinetic parameters were determined. The ultrafiltration system enabled the removalof inhibitory products from the reaction medium, allowing the enzyme to be recovered for reuse. A 10 kDa membrane was used to separate the different CDs produced by the CGTase. The substrates evaluated were maltodextrin, corn starch and cassava starch at 5, 10 and 15% (w/V), in the presence and absence of 10% (V/V) ethanol. After reaction for 132 h, 10% (w/V) cassava starch in the presence of ethanol provided the best results with 32.1 mg/mL of ß-CD. Maximum production occurred after 72 h of reaction, with a yield of 87.4% of ß-CD and an α-CD, ß-CD and γ-CD production ratio of 1:1:0.08 g, respectively. When eight repetitive batches of 72 h followed by ultrafiltration and crystallization of ß-CD were performed, 2.1 g of precipitate was obtained with a purity of 67.6% ß-CD. The supernatant from the crystallization process was lyophilized and resulted in 35.3% α-CD. The developed model can be used industrially for the production of low cost CDs from easily obtained raw material

Ultrafiltration/instrumentation , Models, Economic , Low Cost Technology/analysis , Cyclodextrins/pharmacology , Starch and Fecula , Crystallization/classification
Braz. j. pharm. sci ; 46(4): 679-685, Oct.-Dec. 2010. ilus, graf, tab
Article in English | LILACS | ID: lil-622867


With the purpose of enabling the analysis by digital methods of particles of multisource pharmaceutical raw materials, this study analyzed different crystal habits of ampicillin particles, by grouping the external shapes obtained from 3 different solvents (acetonitrile, ethanol, and methanol), thereby reducing the number of descriptors necessary to adequately represent each shape. For this purpose, a selection of morphological descriptors was used including: circularity, roughness, roundness, compactness, aspect ratio, effective diameter, solidity, convexity, fractal dimension, and 10 Complex Fourier descriptors. These measures cover highly diverse morphological properties and define the crystal habit of a particle. Principal Component Analysis (PCA) and the Cluster Analysis (CA) were the grouping techniques used, which demonstrated the possibility of using between 2 and 4 descriptors instead of the 18 proposed initially.

Com o objetivo de possibilitar a análise, por meio de métodos digitais, de partículas de matérias-primas farmacêuticas de múltiplas fontes, analisaram-se diferentes cristais de partículas de ampicilina através do agrupamento de formas externas obtidas de três diferentes solventes (acetonitrila, etanol e metanol), reduzindo, desse modo, o número de descritores necessários para representar adequadamente cada forma. Com esse propósito, utilizou-se seleção de descritores morfológicos, incluindo: circularidade, aspereza, arredondamento, compactação, relação de aspecto, diâmetro efetivo, solidez, convectividade, dimensão fractal e 10 descritores complexos de Fourier. Essas medidas cobrem diversas propriedades morfológicas e definem a cristalinidade de uma partícula. As análises do componente principal (PCA) e por grupamento (CA) foram as técnicas de agrupamento utilizadas, que demonstraram a possibilidade de utilizar entre 2 e 4 descritores ao invés dos 18, inicialmente propostos.

Ampicillin/chemistry , Crystallization/classification , Multivariate Analysis , Subject Headings , Fourier Analysis , Solid Waste Characteristics
Arq. bras. oftalmol ; 71(2): 228-233, mar.-abr. 2008. ilus, tab
Article in Portuguese | LILACS | ID: lil-483031


OBJETIVO: Verificar a reprodutibilidade da classificação dos padrões do teste de cristalização do filme lacrimal utilizando cinco examinadores diferentes e comparar os padrões de cristalização de pacientes portadores da síndrome de Sjõgren com os de indivíduos não portadores de doenças da superfície ocular. MÉTODOS: Análise da cristalização da lágrima de 29 pacientes com Sjõgren e 45 pacientes sem doenças da superfície ocular, através de microscópio com luz polarizada, utilizando a classificação de Rolando. Para fins estatísticos foi estudada a curva ROC (Receiver Operating Characteristic) para determinar a melhor nota de corte do exame que separa indivíduos normais dos portadores da síndrome, índice de concordância Kappa (p<0,0001) para averiguar a reprodutibilidade da classificação dos padrões de cristalização e tabelas de contingência para comparação dos resultados entre os grupos. RESULTADOS: Com os padrões agregados (I com II e III com IV) a concordância dos examinadores foi alta (Kappa=0,82 a 0,97 e p<0,0001). Por meio da curva ROC obtivemos nota de corte de 2,50 para o diagnóstico de Sjõgren. Na comparação entre os grupos, o grupo normal recebeu predominantemente classificações de padrões I e II, ao passo que o grupo com Sjõgren, padrões III e IV. CONCLUSÕES: Houve concordância com a literatura quanto aos padrões encontrados nos pacientes com Sjõgren e nos pacientes sem doença da superfície ocular. A classificação do teste de cristalização é reprodutível quando utilizada a classificação de Rolando.

PURPOSE: To verify the reproducibility of Rolando's classification of the tear ferning test using five different examiners and to compare the patterns of crystallization found in Sjõgren's syndrome patients and normal subjects. METHODS: Tear ferning analysis of 29 patients with Sjõgren's syndrome and of 45 patients without ocular disease were done using polarized light microscopy and the Rolando classification for tear ferning. Five examiners classified the ferning patterns of all the patients. ROC curve (Receiver Operating Characteristic) was used to find out the best score for the correct syndrome diagnosis. Kappa index (p<0.0001) was used to compare the results of the examiners among them and check the test's reproducibility. Charts were drawn to compare the two groups' results. RESULTS: Throught the ROC curve the score of 2.50 for diagnosis of Sjõgren's syndrome was stabilished. Considering the aggregated patterns I with II and III with IV, the examinors' level of pattern agreement was excellent (Kappa ranging from 0.82 to 0.97, p<0.0001). The group with Sjõgren's syndrome was classified mostly as patterns III and IV and the patients without ocular disease mostly as I and II. CONCLUSION: The patterns associated with Sjõgren's syndrome and normal patients matched the ones in the literature. The tear ferning test classification is reproductible when the Rolando classification was used for Sjõgren's syndrome patients.

Adult , Aged , Female , Humans , Male , Middle Aged , Diagnostic Techniques, Ophthalmological , Sjogren's Syndrome/diagnosis , Tears/chemistry , Crystallization/classification , Epidemiologic Methods , Observer Variation