Compostos bioativos e atividade antioxidante do café conilon submetido a diferentes graus de torra

The bioactive compounds and antioxidant activity presented by Conilon coffee (C. Canephora) variety, produced in the Espírito Santo State, Brazil, were quantified. The light roast coffee showed the highest level of total phenols, trigonelline, caffeic and chlorogenic acids. The proanthocyanidin level was the highest for dark roast coffee, while caffeine level didn't show significative changes for the light and middle roast coffees. All the Conilon coffee extracts showed antioxidant activity depending on bioactive compounds concentration and roasting degree. The coffee samples submitted to a light roasting degree showed the highest antioxidant activity.

Atividade antioxidante de extratos e taninos condensados das folhas de Maytenus ilicifolia Mart. ex Reiss.

Maytenus ilicifolia (Celastraceae) is a native plant of South America and popularly known as "espinheira-santa". The aim of this study was to evaluate the antioxidant capacity of extracts and isolated compounds from this plant. The antioxidant activity of the crude and semipurified extracts and isolated compounds was evaluated through DPPH-radical and phosphomolybdenum-complex assays. By both methods, the ethyl-acetate fraction demonstrated better antioxidant capacity compared with vitamin C and trolox. In the compounds, the higher the number of hydroxyls, the greater the antioxidant activity. In addition, stereochemistry influenced antioxidant activity, i.e., compounds with 2R,3R showed greater activity than those with 2R,3S.

Cromatografia gasosa bidimensional abrangente (GC × GC)

This paper presents the fundamental principles, instrumentation and selected applications of comprehensive two-dimensional gas chromatography (GC × GC). In this technique, introduced in 1991, two capillary columns are coupled and proper modulating interfaces continuously collect the eluate from the first column, transferring it to the second column. The result is a geometric increment in the chromatographic resolution, ensuring separation of extremely complex mixtures in time periods shorter or comparable to those of analysis using conventional gas chromatography and with better detectabilities and sensitivities.

Atividade antioxidante do extrato de sementes de limão (Citrus limon) adicionado ao óleo de soja em teste de estocagem acelerada

The aim of this work was to evaluate antioxidant activity of lemon seeds added to soybean oil, submitted to accelerated incubator-storage test and to determine its synergistic effect with the synthetic antioxidant TBHQ. The treatments Control, TBHQ (50 mg/kg), LSE (2,400 mg/kg Lemon Seed Extract), Mixture 1 (LSE + 50 mg/kg TBHQ) and Mixture 2 (LSE + 25 mg/kg TBHQ) were prepared and subjected to the accelerated incubator-storage test at 60 ºC for 12 days; samples were taken every 3 days and analyzed regarding peroxide value and conjugated dienes. The results showed that antioxidant activity of the tested treatments were: TBHQ = Mixture 1 = Mixture 2 > LSE > Control.

Determinação de 3,4-metilenodioximetanfetamina (MDMA) em comprimidos de Ecstasy por cromatografia líquida de alta eficiência com detecção por fluorescência (CLAE-DF)

This paper describes the development and validation of simple and selective analytical method for determination of 3.4-methylenedioxymethamphetamine (MDMA) in Ecstasy tablets, using high performance liquid chromatography with fluorescence detection. Analysis was performed in a reversed phase column (LiChrospher 100 C18, 150 x 4.6 mm, 5 µm), isocratic elution with phosphate buffer 25 mmol/L pH 3.0 and acetonitrile (95:5, v/v). The method presents adequate linearity, selectivity, precision and accuracy. MDMA concentration in analyzed tablets showed a remarkable variability (from 8.5 to 59.5 mg/tablet) although the tablet weights were uniform, indicating poor manufacturing control thus imposing additional health risks to the users.

Efeito de matriz na quantificação de agrotóxicos por cromatografia gasosa

The lack of accuracy of a chromatographic method can be associated with the matrix effect. This effect is observed in pesticide quantification by gas chromatography when the chromatographic signals of standards prepared in solvents are compared with those of the analyte in extracts of complex matrices. In the competition between the matrix components and the pesticides for the active sites of the liner, a larger amount of pesticides is transferred to the column, giving apparent extractions above 100%. In this work, we discuss factors that contribute to the matrix effect and present some attempts to overcome the problem.

Determinação de ácido valpróico em soro por cromatografia líquida de alta eficiência com detector de arranjo de diodos (CLAE-DAD), após derivatização com brometo de fenacila

Valproic acid (VA) is a drug used to control seizures in several epileptic conditions. In VA pharmacotherapy, therapeutic drug monitoring is recommended to obtain adequate seizure control and avoid toxicity. The aim of this study was to validate a method for the determination of valproic acid in serum, employing high performance liquid chromatography with diode array detection (HPLC-DAD), after derivatization with phenacyl bromide. The calibration curve (y=0.0133x-0.0025) presented good linearity with r²=0.9999. Accuracy (101-115%), intra-assay precision (4.53-8.15%) and inter-assay precision (3.15-6.77%) were acceptable. The quantification limit was 2.0 µg/mL. The method presented similar results to enzyme immunoassay.

Derivados oleananos e ursanos e sua importância na descoberta de novos fármacos com atividade antitumoral, anti-inflamatória e antioxidante

Oleanolic and ursolic acids are triterpenes that exist abundantly in the plant kingdom. They show antitumor activity and their cytotoxic activity was already evaluated against a broad range of cell lines. The inhibition of enzymes involved in the metabolism of DNA and the induction of apoptosis are known events that have been related to the antitumour activity of these triterpenes. The antiinflamatory and antioxidant activities also seem to play an important role in their antitumour activity. In this review, it is presented an overview of the importance of the potential antitumour, antiinflamatory and antioxidant activities of these triterpenoid derivatives. Also, we propose a structural-activity relationship to triterpenes containing oleanane or ursane skeleton and their cytotoxic activity.

Cromatografia de afinidade por íons metálicos imobilizados (IMAC) de biomoléculas: aspectos fundamentais e aplicações tecnológicas

Immobilized Metal Ion Affinity Cromatography - IMAC - is a group-specific based adsorption applied to the purification and structure-function studies of proteins and nucleic acids. The adsorption is based on coordination between a metal ion chelated on the surface of a solid matrix and electron donor groups at the surface of the biomolecule. IMAC is a highly selective, low cost, and easily scaled-up technique being used in research and commercial operations. A separation process can be designed for a specific molecule by just selecting an appropriate metal ion, chelating agent, and operational conditions such as pH, ionic strength, and buffer type.

Comparação entre métodos de quantificação em cromatografia gasosa: um experimento para cursos de química

This article describes an experiment designed to teach quantitative determination in gas chromatography (GC) in Organic and Analytical Chemistry practical classes. The experiment consisted of extracting and analyzing eugenol from clove seeds to perform a quantitative approach aimed at comparing results obtained by external and internal calibration procedures. Therefore, this experiment proved to be very effective tool to enhance students awareness on the need to understand different types of calibration in GC and on how to avoid common experimental errors, and to find the best ways to eliminate their interference during the quantitative analysis phase.

Constituintes químicos e atividade antioxidante de extratos das folhas de Terminalia fagifolia Mart. et Zucc

Phytochemical investigation of ethanolic leaves extracts of T. fagifolia led to the isolation of (+)-catechin, sitosterol-3-O-β-D-glucopyranoside, α- and β-tocopherol, a mixture of lupeol, α- and β-amyrin, sitosterol and a mixture of glicosid flavonoids (CP-13). The structures of these compounds were identified by ¹H and 13C NMR spectral analysis and comparison with literature data. Absolute configuration of the catechin was determinate by circular dichroism. Antioxidant activity (EC50), evaluated by 2,2-diphenyl-1-picrylhidrazyl (DPPH) assay system, decreased in the order: (+)-catechin > hydroalcoholic fraction > CP-13 > aqueous fraction > EtOH extract.

Extracción de compuestos con actividad antioxidante de frutos de guayaba cultivada en Vélez-Santander, Colombia

The effects of the extraction system (50% methanol or 50% methanol pH 2.0), volume/material ratio, temperature, time and extractions with 70% acetone were evaluated in the total phenolic compounds (TPC) extraction and in antioxidant activities (AA) using FRAP and ABTS assays in guava fruit. The best yield was obtained when 0.5 g of guava were extracted first with 20 mL 50% methanol and then four times with 20 mL 70% acetone during 30 min at 50 °C. Among the different trials guava fruit exhibited high levels of AA as well as TPC.

Composição fenólica, atividade antibacteriana e antioxidante da própolis vermelha brasileira

Propolis is a resinous hive product collected by honeybees from various plant sources. It has a complex chemical composition, constituted by various phenolic compounds. Extracts of increasing polarity (n-hexane, chloroform, and ethanol) were obtained from a sample of red propolis from the state of Alagoas. Assays were carried out for determination of contents of phenolics, along with antibacterial and antioxidant activities. The EEP, fractions and sub-fractions showed strong biological activities and were related with phenolic the content compounds contents. The sub-fractions were more bioactive than the EEP and fractions, demonstrating that the antioxidant and antibacterial activities are not a result of synergistic effect between the various chemical compounds in propolis.

Comparação de diferentes abordagens para avaliação da incerteza na cromatografia gasosa do gás natural

The evaluation of uncertainty associated with an analytic result is an essential part of the measurement process. Recently, several approaches to evaluate the uncertainty in measurement have been developed. Here, the gas chromatography assay uncertainty for natural gas is compared by some of these approaches: the guide to the expression of uncertainty in measurement (GUM) approach, top-down approach (reproducibility estimate from an inter-laboratory study), Barwick & Ellison (data from validation), study of variability and fuzzy approach. The comparison shows that GUM, Barwick & Ellison and fuzzy approaches lead to comparable uncertainty evaluations, which does not happen with the top-down approach and study of variability by the absence of data normality.

Determinação de resíduos de pesticidas em plasma bovino por cromatografia gasosa-espectrometria de massas

An analytical method for the isolation based on matrix solid-phase dispersion technique and gas chromatographic determination of pesticides in cattle plasma is presented. It was fortified 0.25 g of plasma with pesticides and blended with 1 g each C18 and Na2SO4. The homogenized matter was transferred to a SPE cartridge, which contained 1 g of activated florisil with 5 mL acetonitrile. The analites were eluted under vaccum with 15 mL acetonitrile, the extract was analyzed by gas chromatography-mass spectrometry. The limit of quantification of the method was 0.04 mg L-1 for chlorphenvinfos and fipronil and 0.02 mg L-1 for cypermethrin..