Flow-through cell based on an array of gold microelectrodes obtained from modified integrated circuit chips

The construction of a flow-through cell incorporating an array of gold microelectrodes is described and its application to flow injection analysis with amperometric detection is presented, Simple modification of almost any conventional integrated circuit chip, used as an inexpensive source of pre-assembled gold micro-wires, leads to the rapid and successful preparation of arrays of 8-48 elements, the polymeric encapsulation material from the top face of the chip is removed by abrasion until the gold micro-mires (used to interconnect the silicon circuit to the external contact pins of the chip) are disrupted and their transversal (elliptical) sections become exposed. Once polished, the flat and smooth top surface of the gold microelectrode-array chip (MEAC) is provided with a spacer and fitted under pressure against an acrylic block with the reference and auxiliary electrodes, to form the electrochemical (thin-layer) flow cell, while the contact pins are plugged into a standard IC socket, This design ensures autonomous electric contact with each electrode and allows fast dismantling for polishing or substitution, the performance of flow cells with MEACs was investigated utilizing the technique of reverse pulse amperometry without oxygen removal, A method was established for the determination of the copper concentration in sugar cane spirit, regulated by law for beverages, Samples from industrial producers and small-scale (alembic) brewers were compared, With a 24 MEAC, a detection limit of 30 mu g I-l of copper (4.7 x 10(-7) mol l(-1) of Cu-II for 100 mu l injections) was calculated, Routine operation was established at a frequency of 60-90 determinations per hour, Intercomparison with atomic absorption spectrometric determinations resulted in excellent agreement.

Changes in lipid composition in hippocampus early and late after status epilepticus induced by kainic acid in wistar rats

Oxidative damage to biological membranes has been reported as a cause of alterations in many different diseases. We had previously reported lipid peroxidation in the kainic acid model of temporal epilepsy. In this study we evaluated earlier and later modifications in the lipid composition after status epileticus induced by kainic acid. Lipid composition was determined by thin-layer chromatography, in the cortex and hippocampus 12-14 h, 7-8, 75-80, or 140-150 days after the end of status epileticus. In the hippocampus there was a significant change in the lipid protein ratio after status epileticus and this was accompanied by an alteration in lipid composition in all tested times. These results suggested that lipid peroxidation induced by kainic acid could be accompanied by chronic changes in the lipid composition that could be related to the development of seizures.

Isolamento e avaliação da atividade biológica dos alcalóides majoritários de Tabernaemontana angulata Mart. ex Müll. Arg., Apocynaceae

"Isolation and evaluation of the biological activity related to the major alkaloids in Tabernaemontana angulata Mart. ex Mull Arg., Apocynaceae." Introducing-new chemotherapeutic agents is a, great demand. in the control of infections diseases.' Brazil is one of the richest countries in biodiversity and the Laboratorio de Extracao at UNIP has been collecting plants from. the Amazon and Atlantic Rain Forests with the aim of screening for new antibacterial and antitumor plant extracts. Previous studies demonstrated that the ethanol fraction obtained from the crude extract of Tabernaemontana angulata stems showed antibacterial activity against Staphylococcus aureus (ATCC 6538 in the microdilution broth assay. Two alkaloids were the major compounds in the active fraction, verified by thin layer chromatography analysis. In the present study, the total alkaloids were obtained from the crude extract and were fractionated by preparative thin layer chromatography for the isolation of the main components. The isolated. compounds were identified by GC/MS and (1)H-NMR as coronaridine,e and voacangine. The alkaloid fractions obtained from the isolation procedure were tested for antibacterial activity, but no activity was detected.

Evaluation of Different Methods of Optical Impression Making on the Marginal Gap of Onlays Created with CEREC 3D

Objectives: This study evaluated the marginal gaps on several surfaces of onlays created with the Cerec 3D system using one intraoral and two extraoral optical impression methods. Methods: A human molar (#19) was mounted with its adjacent teeth on a typodont (Frasaco) and prepared for a MODL onlay. The typodont was assembled in the mannequin head in order to simulate clinical conditions. The same operator took 36 individual optical impressions using a CEREC 3D camera. For group 1 (IP), a thin layer of titanium dioxide powder (CEREC powder-VITA) was applied directly onto the surface of the preparation for imaging (n=12). For group 2 (EP), a sectional impression was taken with hydrocolloid Identic Syringable (Dux Dental), a die made with polyvinylsiloxane KwikkModel Scan (R-dental Dentalerzeugnisse GmbH) and powdered with titanium dioxide for imaging (n=12). For group 3 (ES), a sectional impression was taken with PVS and a sectional stock tray, a die fabricated in stone (Diamond die- HI-TEC Dental Products) and the die being imaged without powdering (n=12). One operator designed and machined the onlays in Vita Blocks Mark II for Cerec (VITA) using a CEREC 3D. The marginal gaps (pm) were measured with an optical microscope (50x) at 12 points, three on each surface of the MODL. The results were analyzed by two-way ANOVA/Tukey's (p=0.05). Results: The overall mean marginal gaps (mu m) for the three methods were: IP=111.6 (+/- 34.0); EP=161.4 (+/- 37.6) and ES=116.8 (+/- 42.3). IP and ES were equal, but both were significantly less than EP. The pooled mean marginal gaps (mu m) for the occlusal = 110.5 (+/- 39) and lingual = 111.5 (+/- 30.5) surfaces were equivalent and significantly less than the distal = 136.5 (+/- 42.5) and mesial = 161.1 (+/- 43.3). Conclusion: The marginal gap of CEREC 3D onlay restorations was not different when the optical impression was taken intraorally vs extraorally using a stone cast that does not require powdering. The lingual and occlusal surfaces showed the lowest gaps.

Synthesis and electrochemical behavior of single-crystal magnetite nanoparticles

Water-dispersed magnetite nanoparticle synthesis from iron(II) chloride in dimethyl sulfoxide (DMSO)-water solution at different DMSO-water ratios in alkaline medium was reported. TEM and XRD results suggest a single-crystal formation with mean particle size in the range 4-27 nm. Magnetic nanoparticles are formed by the oxidative hydrolysis reaction from green rust species that leads to FeOOH formation, followed by autocatalysis of the adsorbed available Fe(II) on the FeOOH surfaces. The available hydroxyl groups seem to be dependent on the DMSO-water ratio due to strong molecular interactions presented by the solvent mixture. Goethite phase on the magnetite surface was observed by XRD data only for sample synthesized in the absence of DMSO. In addition, cyclic voltammetry with carbon paste electroactive electrode (CV-CPEE) results reveal two reduction peaks near 0 and +400 mV associated with the presence of iron(III) in different chemical environments related to the surface composition of magnetite nanoparticles. The peak near +400 mV is related to a passivate thin layer surface such as goethite on the magnetite nanoparticle, assigned to the intensive hydrolysis reaction due to strong interactions between DMSO-water molecules in the initial solvent mixture that result in a hydroxyl group excess in the medium. Pure magnetite phase was only observed in the samples prepared at 30% (30W) and 80% (80W) water in DMSO in agreement with the structured molecular solvent cluster formation. The goethite phase present on the, magnetite nanoparticle surface like a thin passivate layer only was detectable using CV-CPEE, which is a very efficient, cheap, and powerful tool for surface characterization, and it is able to determine the passivate oxyhydroxide or oxide thin layer presence on the nanoparticle surface.

Review of Fluconazole Properties and Analytical Methods for Its Determination

Fluconazole, -(2.4-diflurofenil)--(1H-triazol-1-methyl)-1H-1,2,4-triazol-1-ethanol, is an antifungal of triazoles class. It shows activity against species of Candida sp., and it is indicated in cases of oropharyngeal candidiasis, esophageal, vaginal, and deep infection. Fluconazole is a selective inhibitor of ergosterol, a steroid exclusive of the cell membrane of fungal cells. Fluconazole is highly absorbed by the gastrointestinal tract, and it spreads easily by body fluids. The main adverse reactions related to the use of fluconazole are nausea, vomiting, headache, rash, abdominal pain, diarrhea, and alopecia in patients undergoing prolonged treatment with a dose of 400 mg/day. In the form of raw material, pharmaceutical formulations, or biological material, fluconazole can be determined by methods such as titration, spectrophotometry, and thin-layer, gas, and liquid chromatography. This article discusses the pharmacological and physical-chemical properties of fluconazole and also the methods of analysis applied to the determination of the drug.

Anomalous metamagnetic-like transition in a FeRh/Fe3Pt interface occurring at T approximate to 120 K in the field-cooled-cooling curves for low magnetic fields

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

ESTABILIDADE TERMICA DO PARACETAMOL EM SOLUCAO: CROMATOGRAFIA EM CAMADA DELGADA (CCD) - ESPECTROFOTOMETRIA ULTRAVIOLETA

The interference practised by the products in degradation of paracetemol when there is the application of spectrophotometry UV is the main obstruction to the execution of studies of thermic stability. The application of chromatography in slender layer to the isolation of paracetamol, besides being the excessively hard to apply was satisfactory to the desired proposal. The type and extension of degradation suffered by paracetamol in solution suggest the convenient inclusion, in the formulations, of one system antioxidant. This practice makes possible the blockage of the oxidation of p-aminophenol, produced by the hydrolytic degradation of paracetamol; this fact propitiated the diminution of the number of products of degradation in the medicine, making the use more secure. On the other hand, considering especially the methodological necessities of the present work, the presence of one antioxidant system facilitated the separation of paracetamol through the Thin Layer Chromatography and consequently optimized its quantification by Spectrophotometry UV during the study of thermic stability. The formulation proposed revealed excellent stability.

Thermal decomposition of acetylsalicylic acid (aspirin)

The thermal decomposition of aspirin in air and dry air flux was investigated. Thermogravimetry-derivative thermogravimetry (TG-DTG), differential scanning calorimetry (DSC), nuclear magnetic resonance (NMR), infrared absorption spectra and thin layer chromatography have been used to study the thermal decomposition of this compound. The results permit the identification of some compounds revealed in the first step of the TG-DTA curves, and also suggest the thermal decomposition mechanism.