Electrocatalytic and voltammetric determination of sulfhydryl compounds through iron nitroprusside modified graphite paste electrode

Iron nitroprusside Fe(II)NP was incorporated into a carbon paste electrode and the electrochemical studies were performed with cyclic voltammetry. The cyclic voltammogram of Fe(II)NP exhibits two redox couple with formal potential (E0')1 = 0.24 e (E0')2 = 0.85 V vs SCE attributed to Fe(II)/Fe(II) and Fe (II)(CN)5NO/Fe(III)(CN)5NO, respectively. The redox couple with (E0')2 = 0.85 V presents an electrocatalytic response for sulfhydryl compounds. The electrocatalytic oxidation of sulfhydryl compounds by the mediator has been used for the determination of L-cysteine and N-acetylcysteine. The modified graphite paste electrode gives a linear range from 9.2 x 10-4-2.0 x 10-2;; 9.6 x 10-4-1.4 x 10-2mol L-1 for the determination of L-cysteine and N-acetylcysteine, respectively, with detection limit of 1.9 x 10-4 mol L-1;; 1.5 x 10 -4 mol L-1 and relative standard desviations ± 5% and 1.5 x 10-3 mol L-1 ± 4% (n=3). The amperometric sensitivities are 0.024 and 0.027 μA/μmol L-1 for L-cysteine and N-acetylcysteine, respectively. The application of this electrode was tested and a commercial pharmaceutical product (Fluimucil) has been determined.

HPLC-EICD: An Useful Tool for the Pursuit of Novel Analytical Strategies for the Detection of Antioxidant Secondary Metabolites

Living cells are continuously exposed to a variety of challenges that exert oxidative stress and are directly related with senescence and the onset of various pathological conditions such as coronary heart disease, rheumatoid arthritis and cancer. Nevertheless, living organisms have developed a complex antioxidant network to counteract reactive species that are detrimental to life. With the aim of bio-prospecting plant species from the Brazilian Cerrado and Atlantic Forest, we have established a methodology to detect secondary antioxidant metabolites in crude extracts and fractions obtained from plant species. Combining HPLC with an electrochemical detector allowed us to detect micromolecules that showed antioxidant activities in Chimarrhis turbinata (DC) leaf extracts. Comparison with purified flavonoid standards led us to identify the compounds in their natural matrices giving valuable information on their antioxidant capacity.

Thermal Behavior and Spectroscopic Study of Neutral and Cationic Mononuclear Cyclopalladated Compounds

The reactions of the precursor [Pd(N,C-dmba)(MeCN)2](NO 3) (1) (dmba = N,N-dimethylbenzylamine), with the proligands 3,5-dimethylpyrazole (Hdmpz), 2-quinolinethiol (qnSH) and 1,1′- bis(diphenylphosphine)ferrocene (dppf) afforded the compounds [Pd(N,C-dmba)(Hdmpz)(ONO2)]0.5CH2Cl2 (2), [Pd(N,C-dmba)(qnSH)(ONO2)] 0.5CH2Cl2 (3) and [Pd(N,C-dmba)(dppf)](NO3) (4), respectively. The mononuclear species 2,3 and 4 were characterized by elemental analysis, infrared spectroscopy, NMR and thermogravimetric analysis. The IR spectra show bands which are consistent with terminal monodentate nitrate group for 2-3 and ionic nitrate for 4. The 1H and 13C NMR data confirm that coordination of the organic ligands has occurred and the 31P{1H} NMR data for 4 clearly evidences the occurrence in solution of three cyclopalladated species with the dppf acting as a bridging ligand in two cases and as a chelate in one. The thermal behavior of compounds 1-4 suggests that complex 2 is the most stable. The X-ray diffractometry results show the formation of PdO from 1 and 2, Pd2OSO4 from 3, and of a mixture of PdO and Fe 2(PO4)3 from 4, as final decomposition products.

Serum iron analysis of adults receiving three different iron compounds

Iron deficiency is one of the most prevalent nutritional problems in the world. Iron compounds are used for the prevention and treatment of this deficiency. A double-blind randomized crossover study with 12 volunteers was carried out to compare the effect of three iron compounds, ferrous glycine chelate (GLY), ferric EDTA (EDTA), and ferrous sulfate (FS) on serum iron, and to examine serial serum iron levels. The products were offered as tablets, and blood samples were drawn hourly for 4 hours. FS produced higher serum iron levels than EDTA or GLY (P <0.05). Data for GLY and EDTA were similar. The areas under the curve (AUC) for serum iron for the different compounds gave AUCFS > AUCGLY = AUCEDTA (P < 0.05). Iron from FS had a significantly greater bioavailability than for the other two compounds. © 2004 Elsevier Inc. All rights reserved.

Contribuição ao estudo farmacognóstico da mutamba (Guazuma ulmifolia - Sterculiaceae)

Guazuma ulmifolia Lam., Sterculiaceae, popularly known as mutamba, has a wide geographical distribution, ranging from Mexico to Southern Brazil. The interest in its chemical properties is due to its popular use for hair loss treatment. This activity can be attributed to tannins that have many pharmacological activities such anti-inflammatory, anti-ulcerogenic, anti-microbial, anti-viral, capillary protective action and radical scavenging properties. In the microscopic analysis of barks and leaves, large secretor ducts could be detected among the parenchyma cells, as well as star shaped trichoms on the epidermis. One of the aims of the anatomical study was to detect tissues with polyphenolic compounds. The results indicated two tissues rich in these compounds: the phloematic region and the periderm. Chemical analyses were carried out on the bark and showed the presence of the following chemical groups: flavonoids, tannins, saponins and mucilages.

A new neolignan and antioxidant phenols from Nectandra grandiflora

The EtOH crude extract from the leaves of Nectandra grandiflora collected in the Atlantic Forest, Brazil, showed antioxidant activity towards β-carotene in a TLC assay. The bioassay-guided fractionation led to the isolation of protocatechuic acid and two flavonol glycosides: afzelin and quercetrin, which showed free radical scavenging activity towards DPPH (ΔA 32, 16 and 73% at 50 μmol L-1) and were compared to commercial antioxidants rutin (81% at 50 μmol L-1) and BHT (9% at 50 μmol L-1), used as standard compounds. Additionally, three inactive neolignans, including the new bicycle[3.2.1]octane neolignan 2′-oxo-piperol B were obtained and characterized by spectrometric methods. ©2005 Sociedade Brasileira de Química.

Synthesis, characterization and thermal behaviour of solid-state compounds of 4-methoxybenzoate with some bivalent transition metal ions

Solid-state M-4-MeO-Bz compounds, where M stands for bivalent Mn, Co, Ni, Cu and Zn and 4-MeO-Bz is 4-methoxybenzoate, have been synthesized. Simultaneous thermogravimetry-differential thermal analysis (TG-DTA), differential scanning calorimetry (DSC), X-ray powder diffractometry, infrared spectroscopy, elemental analysis and complexometry were used to characterize and to study the thermal behaviour of these compounds. The results led to have information about the composition, dehydration, thermal stability and thermal decomposition of the isolated compounds. © 2005 Akadémiai Kiadó, Budapest.

Saponinas triterpênicas de Tocoyena brasiliensis Mart. (Rubiaceae)

The present communication reports the isolation and identification of four triterpenoid saponins from the chloroform extract of the leaves of Tocoyena brasiliensis: 3-O-β-D-quinovopyranosyl quinovic acid, 3-O-β-D- quinovopyranosyl cincholic acid, 3-O-β-D-glucopyranosyl quinovic acid and the 28-O-β-D-glucopyranosyl ester derivative of quinovic acid as binary mixtures, respectively. From the ethanol extract a flavonoid identified as ramnazin-3-O-rutinoside was obtained. The structures of these compounds were assigned by data analysis of ID and 2D NMR spectrometry and comparison with data recorded in the literature for these compounds.

Evaluation of the effects of different extraction methods for main volatile compounds from Bambusa textilis leaves

Bambusa textilis is widely used in popular medicine to treat all kinds of wound inflammation, chronic fever, pulmonary and infectious diseases. The aim of this study was to compare the chemical composition of the extracts of B. textilis leaves obtained by three different extraction methods: solid/liquid extraction, Soxhlet and Clevenger system using gas chromatography with flame ionization detector (GC-FID) and gas chromatography with mass spectrometry (GC-MS) analyses. The analytical characteristics of the extracts showed some differences and the GC-MS analysis indicated the presence of higher concentrations of nitro compounds and alkalis. © VSP 2005.

Central nifedipine-induced alterations in salivary flow and compounds: Role of nitric oxide

The aim of this study was to examine the role of nifedipine and Nitric Oxide (NO) on salivary flow and compounds (salivary amylase, saliva total proteins, saliva calcium, sodium and potassium). Male Holtzman rats weighting 200-250 g were anesthetized with zoletil 50 mg kg -1 (tiletamine chloridrate 125.0 mg and zolazepan chloridrate 125.0 mg) into quadriceps muscle and stainless steel cannulas were implanted into their lateral ventricle of the brain (LV). Animals in divided group were injected with nifedipine (50 μg μL -1) alone and in combination with 7-nitroindazol (7-NIT) (40 μg μL -1), neuronal NO Sinthase Inhibitor (nNOSI) and Sodium Nitroprussate (SNP) (30 μg μL -1) NO donor agent. As a secretory stimuli, pilocarpine dissolved in isotonic was administered intraperitoneally (ip) at a dosage of 10 mg kg -1 body weight. Saliva was collected for 7 min with four cotton balls weighing approximately 20 mg each, two of which were placed on either side of the oral cavity, with the other two placed under the tongue. Nifedipine treatment induced a reduction in saliva secretion rate and concentration of amylase, total protein and calcium without changes in sodium and potassium concentration in comparison with controls. Co-treatment of animals with nifedipine and SNP retained flow rate and concentration of amylase, total protein and calcium in normal levels. Co-treatment of animals with nifedipine and 7-NIT potentiated the effect of nifedipine on the reduction of saliva secretion and concentrations of amylase, total protein and calcium. Nifedipine (dihydroperidine) calcium-channel blocker widely in use is associated with salivary dysfunction acting in the central nervous system structures. NO might be the mechanism for protective effect against the nifedipine-induce salivary dysfunction, acting in the CNS. © 2006 Asian Network for Scientific Information.

Metal-insulator transition in Nd1-xEuxNiO 3 compounds

Polycrystalline Nd1-xEuxNiO3 (0≤x≤0.5) compounds were synthesized in order to investigate the character of the metal-insulator (MI) phase transition in this series. Samples were prepared through the sol-gel route and subjected to heat treatments at ∼1000 °C under oxygen pressures as high as 80bar. X-ray diffraction (XRD) and neutron powder diffraction (NPD), electrical resistivity ρ(T), and magnetization M(T) measurements were performed on these compounds. The NPD and XRD results indicated that the samples crystallize in an orthorhombic distorted perovskite structure, space group Pbnm. The analysis of the structural parameters revealed a sudden and small expansion of ∼0.2% of the unit cell volume when electronic localization occurs. This expansion was attributed to a small increase of ∼0.003 of the average Ni-O distance and a simultaneous decrease of ∼-0.5° of the Ni-O-Ni superexchange angle. The ρ(T) measurements revealed a MI transition occurring at temperatures ranging from TMI∼193 to 336K for samples with x ≤ 0 and 0.50, respectively. These measurements also show a large thermal hysteresis in NdNiO3 during heating and cooling processes, suggesting a first-order character of the phase transition at TMI. The width of this thermal hysteresis was found to decrease appreciably for the sample Nd 0.7Eu0.3NiO3. The results indicate that cation disorder associated with increasing substitution of Nd by Eu is responsible for changing the first-order character of the transition in NdNiO3. © 2006 IOP Publishing Ltd.

Antimicrobial endodontic compounds do not modulate alkylation-induced genotoxicity and oxidative stress in vitro

Objective: To investigate if formocresol, paramonochlorophenol, or calcium hydroxide modulate the genotoxic effects induced by the oxidatively damaging agent hydrogen peroxide (H 2O 2) or the alkylating agent methyl methanesulfonate (MMS) in vitro by using single cell gel (comet) assay. Study design: Chinese hamster ovary (CHO) cells in culture were exposed directly to formocresol, paramonochlorophenol, or calcium hydroxide (adjusted to 100 μg/mL) for 1 hour at 37°C. Subsequently the cultures were incubated with increasing concentrations (0-10 μmol/L) of MMS in phosphate-buffered solution (PBS) for 15 minutes at 37°C or of H 2O 2 at increasing concentrations (0-100 μmol/L) in distilled water for 5 minutes on ice. The negative control cells were treated with PBS for 1 hour at 37°C. The parameter from the comet assay (tail moment) was assessed by the Kruskal-Wallis nonparametric test followed by a post hoc analysis (Dunn test). Results: Clear concentration-related effects were observed for the genotoxin-exposed CHO cells. Increase of MMS-induced DNA damage was not significantly altered by the presence of the compounds tested. Similarly, no significant changes were observed when hydrogen peroxide was used with the endodontic compounds evaluated. Conclusion: Formocresol, paramonochlorophenol, and calcium hydroxide are not able to modulate alkylation-induced genotoxicity or oxidative DNA damage as depicted by the single cell gel (comet) assay. © 2006 Mosby, Inc. All rights reserved.

Assessment of DNA damage by extracts and fractions of Strychnos pseudoquina, a Brazilian medicinal plant with antiulcerogenic activity

Strychnos pseudoquina St. Hil. is a native plant of the Brazilian Savannah, used in popular medicine to treat a number of conditions. Since it contains large quantities of alkaloids with proven antiulcer activity, we tested the genotoxic potential of crude extracts and fractions containing alkaloids and flavonoids from the leaves of this plant, on Salmonella typhimurium and performed the micronucleus test on peripheral blood cells of mice treated in vivo. The results showed that the methanol extract of the leaves of S. pseudoquina is mutagenic to the TA98 (-S9) and TA100 (+S9, -S9) strains of Salmonella. The dichloromethane extract was not mutagenic to any of the tested strains. Fractions enriched with alkaloids or flavonoids were not mutagenic. In vivo tests were done on the crude methanol extract in albino Swiss mice, which were treated, by gavage, with three different doses of the extract. The highest dose tested (1800 mg/kg b.w.) induced micronuclei after acute treatment, confirming the mutagenic potential of the methanol extract of the leaves of S. pseudoquina. In high doses, constituents of S. pseudoquina compounds act on DNA, causing breaks and giving rise to micronuclei in the blood cells of treated animals. © 2006 Elsevier Ltd. All rights reserved.

Amphibian secretions for drug discovery studies: A search for new antiparasitic and antifungal compounds

The antiparasitic and antifungal activities of nine amphibian skin secretions were studied in different in vitro models. Seven secretions presented a considerable antiprotozoan activity and one showed promising results against Candida sp. These results can be the basis for the development of new drugs, especially for neglected parasitic diseases. © 2007 Bentham Science Publishers Ltd.

Efeito de poliaminas exógenas no crescimento inical in vitro e nos teores de fenóis, poliaminas e atividade da peroxidase em Aloe vera (L.) Burm.

Lateral shoots of the Aloe vera (L.) Burm. cultivated in vitro, without addition vegetal regulators, for 90 days, were inoculated in MS culture-medium, containing or not spermine and/or spermidine. After 30 days of cultivation, the plants were submitted to biochemical analysis together with micropropagated plants - that were under in vitro cultivation for 90 days - (denominated as characterization), and matrix plants (in vivo). The levels of free polyamines, total phenols, total flavonoids, and the activity of peroxidase were evaluated in the biochemical analyses. The exogenous application of spermidine have promoted large number of shoots. Spermidine and spermine have promoted, when associated, an increase in the number of shoots as well as an increase of the contents of putrescine and and flavonoids. The putrescine has presented the most significant alterations, enabling to be utilized as marker of morphogenesis in the micropropagated Aloe vera. Tissues under active growth have presented high activity of peroxidase as well as those with greater rate of oxidation. In these tissues, there were noticed also higher contents of total flavonoids, indicating the need of antioxidative compounds. The action of polyamines jointly tseemed to be benefic for the shooting of micropropagated Aloe vera.