Tempo de vida útil de propelentes base-simples

The purpose of this work was to determine the safe shelf life of single-base propellants. The kinetic parameters relative to the consumption of the stabilizer diphenylamine (DPA) added to the propellant were determined as a function of the storage and ageing time. High Performance Liquid Chromatography (HPLC) with spectrophotometric detection was used to determine the DPA percentage before and after the artificial ageing at 60, 70 and 80 ºC. The experimental data were very well adjusted to a pseudo-first order kinetic model and the respective kinetic constants are 8.0-10-3 day-1 (60 ºC); 1.9-10-2 day-1 (70 ºC); 1.2-10-1 day-1 (80 ºC). The activation energy was calculated as 130 kJ mol-1 and the half-time for depletion of the DPA at the hypothetical temperature of 40 ºC of storage was estimated as being 6 years.

Desenvolvimento e validação de método analítico para determinação simultânea de lamivudina, zidovudina e nevirapina em comprimidos dose-fixa combinada por cromatografia líquida de alta eficiência

An analytical method has been developed and validated for the quantitation of lamivudine, zidovudine and nevirapine in the fixed-dose combination film-coated tablet by high performance liquid chromatography, in accordance with RE No. 899/2003, National Sanitary Surveillance Agency. It was based on an isocratic elution system with a potassium phosphate buffer pH 3.0: acetonitrile (60:40 v/v) mobile phase, C18, 250 x 46 mm column, 10µm particle size, λ 270 nm. The statistically evaluated results have shown that the method is specific, precise, accurate, and robust, ensuring the analytical safety of 3TC, AZT and NVP determination, which emerges as a new therapeutic alternative for antiretroviral treatment.

A multi-screening approach for marine-derived fungal metabolites and the isolation of cyclodepsipeptides from Beauveria felina

Extracts obtained from 57 marine-derived fungal strains were analyzed by HPLC-PDA, TLC and ¹H NMR. The analyses showed that the growth conditions affected the chemical profile of crude extracts. Furthermore, the majority of fungal strains which produced either bioactive of chemically distinctive crude extracts have been isolated from sediments or marine algae. The chemical investigation of the antimycobacterial and cytotoxic crude extract obtained from two strains of the fungus Beauveria felina have yielded cyclodepsipeptides related to destruxins. The present approach constitutes a valuable tool for the selection of fungal strains that produce chemically interesting or biologically active secondary metabolites.

Phytochemical study of Gypsophila trichotoma wend. (Caryophyllaceae)

Phytochemical studies of ethyl acetate extracts from the roots and aerial parts of Gypsophila trichotoma revealed the presence of stigmast-7-en-3-ol, stigmasta-7,22-dien-3-ol (spinasterol), ergost-7-en-3-ol, stigmasta-3,5dien7-one, β-sitosterol, 22,23-dihydrospinasterone, vitexin, orientin, homoorientin and hyperoside. The structures of the compounds were determined by GC/MS and HPLC analyses.

Determinação simultânea dos ácidos orgânicos tartárico, málico, ascórbico e cítrico em polpas de acerola, açaí e caju e avaliação da estabilidade em sucos de caju

The aim of the present study was determining the main organic acids in pulp and juices, as well as evaluating their stability, after opening the package, by liquid chromatography in a C18 column with isocratic elution and UV detection. In açaí pulp tartaric, malic and citric acids were found. Cashew samples presented all of the organic acids evaluated, besides high concentrations of ascorbic and malic acids. Acerola pulp had the highest ascorbic acid concentration. A small decrease in organic acid content during storage was observed. Malic and citric acids seem to be more stable than tartaric and ascorbic acids.

Quantificação simultânea de indicadores biológicos de exposição a solventes orgânicos por cromatografia líquida de alta eficiência

Biological monitoring is very important to guarantee health to workers. This method was developed for simultaneous determination of xylene, toluene, styrene and ethylbenzene metabolites. It involves only dilution and centrifugation of urine samples and improved chromatographic conditions. Analyses show recovery > 95%; r² > 0.99; intermediate precision CV% < 6% and % bias < ±10. Exposed subjects presented at least three metabolites in urine. The method proved to be feasible, reliable and important in biological monitoring, especially in exposure to organic solvent mixtures.

Otimização de método para determinação de flavonóis e flavonas em frutas por cromatografia líquida de alta eficiência utilizando delineamento estatístico e análise de superfície de resposta

This work optimized the HPLC conditions for the simultaneous determination of luteolin, apigenin, myricetin, quercetin and kaempferol in aglycone form, as well defined the best conditions for hydrolysis/extraction of these flavonoids in fruits, using the statistical central composite design and response surface analysis. A reverse phase method was developed using a gradient of methanol/water acidified with 0.3% formic acid as mobile phase and a photodiode array detector. The samples were extracted with methanol/water (50:50 v/v) at 90 ºC. The optimum time and HCl concentration varied for the different fruits investigated, demonstrating the necessity of optimizing these conditions for each fruit analyzed. Good recovery (87.1 to 96.3%), repeatability and linearity were obtained.

Nutrimetabolomics fingerprinting to identify biomarkers of bread exposure in a free-living population from the PREDIMED study cohort

Bread is one of the most widely consumed foods. Its impact on human health is currently of special interest for researchers. We aimed to identify biomarkers of bread consumption by applying a nutrimetabolomic approach to a free-living population. An untargeted HPLC q-TOF-MS and multivariate analysis was applied to human urine from 155 subjects stratified by habitual bread consumption in three groups: non-consumers of bread (n = 56), white-bread consumers (n = 48) and whole-grain bread consumers (n = 51). The most differential metabolites (variable importance for projection ≥1.5) included compounds originating from cereal plant phytochemicals such as benzoxazinoids and alkylresorcinol metabolites, and compounds produced by gut microbiota (such as enterolactones, hydroxybenzoic and dihydroferulic acid metabolites). Pyrraline, riboflavin, 3-indolecarboxylic acid glucuronide, 2,8-dihydroxyquinoline glucuronide and N-α-acetylcitrulline were also tentatively identified. In order to combine multiple metabolites in a model to predict bread consumption, a stepwise logistic regression analysis was used. Receiver operating curves were constructed to evaluate the global performance of individual metabolites and their combination. The area under the curve values [AUC (95 % CI)] of combined models ranged from 77.8 % (69.1 86.4 %) to 93.7 % (89.4 98.1 %), whereas the AUC for the metabolites included in the models had weak values when they were evaluated individually: from 58.1 % (46.6 69.7 %) to 78.4 % (69.8 87.1 %). Our study showed that a daily bread intake significantly impacted on the urinary metabolome, despite being examined under uncontrolled free-living conditions. We further concluded that a combination of several biomarkers of exposure is better than a single biomarker for the predictive ability of discriminative analysis.

Nutrimetabolomics fingerprinting to identify biomarkers of bread exposure in a free-living population from the PREDIMED study cohort

Bread is one of the most widely consumed foods. Its impact on human health is currently of special interest for researchers. We aimed to identify biomarkers of bread consumption by applying a nutrimetabolomic approach to a free-living population. An untargeted HPLC q-TOF-MS and multivariate analysis was applied to human urine from 155 subjects stratified by habitual bread consumption in three groups: non-consumers of bread (n = 56), white-bread consumers (n = 48) and whole-grain bread consumers (n = 51). The most differential metabolites (variable importance for projection ≥1.5) included compounds originating from cereal plant phytochemicals such as benzoxazinoids and alkylresorcinol metabolites, and compounds produced by gut microbiota (such as enterolactones, hydroxybenzoic and dihydroferulic acid metabolites). Pyrraline, riboflavin, 3-indolecarboxylic acid glucuronide, 2,8-dihydroxyquinoline glucuronide and N-α-acetylcitrulline were also tentatively identified. In order to combine multiple metabolites in a model to predict bread consumption, a stepwise logistic regression analysis was used. Receiver operating curves were constructed to evaluate the global performance of individual metabolites and their combination. The area under the curve values [AUC (95 % CI)] of combined models ranged from 77.8 % (69.1 86.4 %) to 93.7 % (89.4 98.1 %), whereas the AUC for the metabolites included in the models had weak values when they were evaluated individually: from 58.1 % (46.6 69.7 %) to 78.4 % (69.8 87.1 %). Our study showed that a daily bread intake significantly impacted on the urinary metabolome, despite being examined under uncontrolled free-living conditions. We further concluded that a combination of several biomarkers of exposure is better than a single biomarker for the predictive ability of discriminative analysis.

Avaliação do potencial antioxidante do pólen apícola produzido na região sul do Brasil

The contents of total phenolics, flavonoids, and antioxidant activity of bee pollen ethanolic extract were determined and compared to those of commercial antioxidants. Bee pollen extract from the state of Rio Grande do Sul presented antioxidant activity statistically equal to that of α -tocopherol and higher than those of BHT and BHA. A statistically significant correlation was observed between the antioxidant activity and the total phenolics and total flavonoids contents of bee pollen extracts. HPLC technique made the identification of high contents of rutin and myricetin possible, which may partially explain the high antioxidant activity of Brazilian bee pollen.

Desenvolvimento e validação de método por cromatografia líquida de alta eficiência para determinação simultânea das impurezas timina e timidina na matéria-prima estavudina

A HPLC method was developed to quantify thymine and thymidine impurities in stavudine bulk drug. The separation was carried out in isocratic mode using methanol/water (20:80) as mobile phase, a C18 column and UV detection at 266 nm. The method provided selectivity based on peak purities and resolution among peaks. It was linear over the range of 0.5-5.0 µg/mL. The quantitation limits were 0.021 µg/mL for thymine and 0.134 µg/mL for thymidine. The average accuracies of three concentrations ranged from 97.06 to 102.61% and precision was close to 1%. The method showed robustness, remaining unaffected by deliberate variations in relevant parameters.

Avaliação do potencial antioxidante de extratos ativos de plantas obtidos por extração com fluido supercrítico

The aim of this work was to evaluate the antioxidant properties of ginger and rosemary extracts, obtained by supercritical extraction. The extracts were characterized by HPLC, GC-MS, phenolic compounds content and antioxidant activity. The main active compounds were identified and high content of phenolic compounds was observed. The extracts presented high antioxidant activity against the free radicals ABTS•+ (350 and 200 mM Trolox/g, for ginger and rosemary, respectively) and DPPH•+ (145 and 80 mM Trolox/g, for ginger and rosemary, respectively). These results suggested that the attained extracts are potential substitutes of synthetic antioxidants used in chemical, food and pharmaceutical industries.

Desenvolvimento de um procedimento biamperométrico para determinação de sacarina em produtos dietéticos

In this work was developed a method for the determination of saccharin in dietary products by a biamperometric titration, using two silver electrodes as working electrodes and silver nitrate as titrant. It were used products as juices (light) and sweeteners with saccharin in concentrations ranged from 8.73 x 10-5 mol L-1 to 1.0 x 10-2 mol L-1, and the results were in close agreement with those data found using a HPLC method at a confidence level of 95%. The main advantages of the proposed method are its simplicity, rapid and low cost.

Performance characteristics of bioassay UV-spectrophotometry and high perfomance liquid chromatographic determination of gatifloxacin in tablets

The microbiological bioassay, UV-spectrophotometry and HPLC methods for assaying gatifloxacin in tablets were compared. Validation parameters such as linearity, precision, accuracy, limit of detection and limit of quantitation were determined. Beer's law was obeyed in the ranges 4.0-14.0 μg/mL for HPLC and UV-spectrophotometric method, and 4.0-16.0 μg/mL for bioassay. All methods were reliable within acceptable limits for antibiotic pharmaceutical preparations being accurate, precise and reproducible. The bioassay and HPLC are more specific than UV-spectrophotometric analysis. The application of each method as a routine analysis should be investigated considering cost, simplicity, equipment, solvents, speed, and application to large or small workloads.

Determinação simultânea de creatinina e indicadores biológicos de exposição ao tolueno, estireno e xilenos em urina por cromatografia líquida de alta eficiência

A simple liquid chromatographic method for the simultaneous determination of creatinine, hippuric acid, mandelic acid, phenylglyoxylic acid and o, m and p-methylhippuric acids was developed and validated. Sample preparation was only dilution with water (1:10), followed by centrifugation. Analysis was performed in a reversed phase column (Lichrospher RP 8ec), 250 x 4.0 mm, with isocratic elution with phosphate buffer pH 2.3 and acetonitrile (90:10, v/v). The method presents adequate linearity, precision and accuracy and allows the simultaneous determination of the biomarkers of exposure to toluene, xylene and styrene together with creatinine, reducing cost and laboratory time.