Validació del mètode analític per la determinació d'aminoàcids i carbohidrats d'un producte farmacèutic per HPLC

Per poder desenvolupar un producte farmacèutic és necessari establir un mètode d’anàlisis que permeti determinar i quantificar totes aquelles substàncies que conté, ja sigui referent als principis actius; a les impureses i productes de degradació, conservants, antioxidants,... Grans entitats com la ICH remarquen la importància de validar els mètodes analítics ja que és la via per demostrar que aquell producte compleix les garanties de qualitat prèviament establertes. Així doncs, l’objectiu d’aquest Treball Final de Grau és poder desenvolupar i validar dos mètodes analítics per a la determinació d’aminoàcids i carbohidrats respectivament, d’un producte farmacèutic per cromatografia líquida (HPLC). Per tal de poder concloure que aquell mètode és adequat per la determinació per la qual ha estat desenvolupat, és necessari obtenir resultats que compleixin els criteris d’acceptació corresponents als paràmetres que han de ser avaluats en una validació analítica. Aquests paràmetres són: la precisió, la selectivitat, l’exactitud i la linealitat i el rang. Els resultats d’aquest projecte han demostrat que els dos mètodes desenvolupats són adequats per a la determinació de tres dels principis actius (aminoàcid 1, aminoàcid 2 i carbohidrat 1) que conté el producte farmacèutic d’ús veterinari analitzat; i poden ser validats ja que compleixen els criteris d’acceptació dels paràmetres avaluats que proposa la ICH. El mètode per la determinació de carbohidrats no és vàlid per el carbohidrat 2, ja que durant el desenvolupament es va detectar que una bona part d’aquest passava a carbohidrat 1 (desplaçament de l’equilibri ceto-enòlic que hi ha entre el carbohidrat 1 i el carbohidrat 2 a pHs alts). És per aquest motiu, que es pot concloure que aquest mètode no és vàlid i es recomana seguir investigant per a poder desenvolupar un mètode analític adient.

Análise de extratos de plantas por CCD: uma metodologia aplicada à disciplina "química orgânica"

extracts of the regional plants Annona squamosa and Annona muricata were analysed by silica gel thin-layer chromatography using adequate systems of solvents and spray reagents. Carbohydrates, amino acids, alkaloids, flavonoids and terpenoids were detected in both species. These data agree with those on the literature about phytochemistry of the Annonaceae.

Separação e identificação de constituintes químicos polares dos galhos de Porcelia Macrocarpa

This paper describes a methodology to separate and identify polar compounds as flavonoid and lignan glucosides, amino acids, salt of quaternary ammonium amino acid and carbohydrates from branches of Porcelia macrocarpa (Annonaceae).

A indústria petroquímica no próximo século: como substituir o petróleo como matéria-prima?

The world reserves of petroleum will finish in about 100 years. For a tropical country like Brazil, biomass will be the natural substitute for petroleum. For the best utilization of biomass, it first needs to be separated into its principal components: cellulose, hemicelluloses, lignins, vegetable and essential oils, non-structural carbohydrates, bark and foliage. All feedstocks for the chemical industry can be obtained from these biomass components, as shown in the first part of this paper. In the second part we discuss how the major products from petrochemicals can be obtained from the different biomass components. We show that Brazil can use different strategies, compared to other countries, to obtain petrochemical products, which could result in innovations. However, it is necessary that the government starts to invest immediately in order to keep the petrochemical industries competitive with foreign industries, so that they continue to be one of Brazil's major employers.

Glicídios no mel

A review about composition, origin and importance of carbohydrates in honey is presented. Fructose and glucose are the major carbohydrates, ranging from 65-85 % of the total soluble solids. Other minor carbohydrates, chiefly di- and trisaccharides, have been also identified. Fructose, glucose and sucrose are mainly originated from nectar. Oligosaccharides are mainly formed by trans-alpha-D-glucosylation reactions catalysed by honeybee alpha-D-glucosidase. The profile of carbohydrates can be useful for the identification of the brazilian region in which honey was produced and may also be useful for testing brazilian honey authenticity.

Consequences of warming and resource quality on the stoichiometry and nutrient cycling of a stream shredder

As a result of climate change, streams are warming and their runoff has been decreasing in most temperate areas. These changes can affect consumers directly by increasing their metabolic rates and modifying their physiology and indirectly by changing the quality of the resources on which organisms depend. In this study, a common stream detritivore (Echinogammarus berilloni Catta) was reared at two temperatures (15 and 20°C) and fed Populus nigra L. leaves that had been conditioned either in an intermittent or permanent reach to evaluate the effects of resource quality and increased temperatures on detritivore performance, stoichiometry and nutrient cycling. The lower quality (i.e., lower protein, soluble carbohydrates and higher C:P and N:P ratios) of leaves conditioned in pools resulted in compensatory feeding and lower nutrient retention capacity by E. berilloni. This effect was especially marked for phosphorus, which was unexpected based on predictions of ecological stoichiometry. When individuals were fed pool-conditioned leaves at warmer temperatures, their growth rates were higher, but consumers exhibited less efficient assimilation and higher mortality. Furthermore, the shifts to lower C:P ratios and higher lipid concentrations in shredder body tissues suggest that structural molecules such as phospholipids are preserved over other energetic C-rich macromolecules such as carbohydrates. These effects on consumer physiology and metabolism were further translated into feces and excreta nutrient ratios. Overall, our results show that the effects of reduced leaf quality on detritivore nutrient retention were more severe at higher temperatures because the shredders were not able to offset their increased metabolism with increased consumption or more efficient digestion when fed pool-conditioned leaves. Consequently, the synergistic effects of impaired food quality and increased temperatures might not only affect the physiology and survival of detritivores but also extend to other trophic compartments through detritivore-mediated nutrient cycling.

Ácidos siálicos: da compreensão do seu envolvimento em processos biológicos ao desenvolvimento de fármacos contra o agente etiológico da gripe

Sialic acids are nine-carbon carbohydrates that occur widely in nature and occupy the terminal portions of some glycoproteins and glycolipids of cell membranes. These carbohydrates are closely involved in cell-cell interactions and in processes such as microbial infection, inflammation, etc. Studies on the participation of sialic acids in biological processes have provided comprehension about their role in the infection by the influenza virus, the causal agent of flu. In this article, we present an overview of the importance of sialic acids in the influenza virus infection and how the knowledge of their involvement in this process has allowed the development of selective and efficient drugs against the virus.

Produção, purificação, clonagem e aplicação de enzimas líticas

Lytic enzymes such as beta-1,3 glucanases, proteases and chitinases are able to hydrolyse, respectively, beta-1,3 glucans, mannoproteins and chitin, as well as the cell walls of many yeast species. Lytic enzymes are useful in a great variety of applications including the preparation of protoplasts; the extraction of proteins, enzymes, pigments and functional carbohydrates; pre-treatment for the mechanical rupture of cells; degradation of residual yeast cell mass for the preparation of animal feed; analysis of the yeast cell wall structure and composition; study of the yeast cell wall synthesis and the control of pathogenic fungi. This review presents the most important aspects with respect to lytic enzymes, especially their production, purification, cloning and application.

Efeito do processo de descafeinação com diclorometano sobre a composição química dos cafés arábica e robusta antes e após a torração

The decaffeinated coffee market has been expanding increasingly in the last years. During decaffeination, aroma precursors and bioactive compounds may be extracted. In the present study we evaluate the changes in the chemical composition of C. arabica and C. canephora produced by decaffeination using dichloromethane. A significant change in the chemical composition of both C. arabica and C. canephora species was observed, with differences between species and degrees of roasting. Major changes were observed in sucrose, protein and trigonelline contents after decaffeination. Changes in the levels of total chlorogenic acids and in their isomers distribution were also observed. Lipids and total carbohydrates were not affected as much. The sensory and biological implications of these changes need to be investigated.

Physicochemical composition of pure and adulterated royal jelly

The physicochemical composition of pure royal jelly as well as of some adulterated samples was analyzed by determining moisture, ash, lipids, nitrogen/proteins, carbohydrates, starch and 10- HDA (10-hydroxy-2-decenoic acid). The solubility in alkaline medium was used to detect the main frauds for adulterating royal jelly which comprise addition of yogurt, water, egg white, sweet condensed milk mixed with propolis, unripe banana and corn starch slurry.

Síntese de amidas e sulfonamidas de beta-D-galactopiranosilamina e beta-lactosilamina e avaliação de suas interações com lectinas de Erythrina cristagalli e de Ricinus communis

We report herein the synthesis of some beta-D-galactopyranosylamine and beta-lactosylamine amides and sulfonamides. The interactions of these compounds with lectins from the seeds of Erythrina cristagalli (LEC) and Ricinus communis (RCA120) were evaluated in a hemagglutination inhibitory activity assay. D-Galactose and lactose were used as reference compounds. The beta-lactosylamine amides and sulfonamides were nearly as active as lactose in inhibiting LEC mediated hemagglutination and were less active against RCA120 agglutinin. The beta-D-galactopyranosylamine amides and sulfonamides were, with one exception, considerably less active than D-galactose in the assay with both lectins.

Potencialidades e oportunidades na química da sacarose e outros açúcares

Non-renewable biomass, such as coal, oil and natural gas are not only energy sources but also important starting materials for the production of a variety of chemicals ranging from gasoline, diesel oil and fine chemicals. In this regard, carbohydrates, the most abundant class of enantiopure organic compounds, are very suitable for generation of chemicals of great practical value. Their bulk-scale availability associated with low cost make them unique starting materials for organic preparative purpose. They are a most attractive alternative for construction of enantiopure target molecules by asymmetric synthesis. This review addresses, in addition to the use of low molecular weight carbohydrates, issues related to renewable biomass from photosynthesis and alternatives for the production of bulk and fine chemicals.

Validação de metodologia para a caracterização química de bagaço de cana-de-açúcar

In this work, a methodology for the characterization of sugar cane bagasse was validated. Bagasse pre-treated with steam in a 5000 L reactor at a pressure of 15.3 kgf/cm², during 7 min, was used to test the methodology. The methodology consisted of the hydrolysis of the material with H2SO4 at 72% v/v, for the quantification of carbohydrates, organic acid, furfural and hydroxymethylfurfural by HPLC; insoluble lignin and ash by gravimetry; and soluble lignin by spectrophotometry. Linearity, repeatability, reproducibility and accuracy of the results obtained in two Research Laboratories were determined, and were considered to be suitable for the validation of the methodology.

Um método verde, rápido e simples para determinar o valor energético de farinhas e cereais matinais

The Energy Value (EV) corresponds to the sum of the energetic contributions from food macronutrients (proteins, carbohydrates and fats) and is required on the labels of pre-packaged foods. The determinations of these parameters are based on distinct analytical procedures, each one being time-consuming, laborious and producing residues. This work presents multivariate models to determine the EV contents of industrialized foods for human consumption by using X-ray fluorescence spectra of samples with known parameters, determined through conventional methods. The proposed method is an alternative to conventional analytical methods and does not require any reagent, given the demands of the "green chemistry".

Método para determinação de carboidratos empregado na triagem de adulterações em café

The objective in this work was to validate a chromatography method for the determination of total carbohydrates in soluble coffee, using a HPLC-UV-VIS with postcolumn derivatization system, in order to verify adulterant additions. The validated method was accurate and robust. Adulteration could be observed by increasing xylose and glucose levels in samples with addition of coffee husks and starchy products while decreasing of galactose and mannose characteristic carbohydrates presenting in high concentration in soluble coffees produced by arabica and robusta coffee beans.