Flow injection amperometric determination of persulfate in cosmetic products using a Prussian Blue film-modified electrode

A flow-injection system with a glassy carbon disk electrode modified with Prussian Blue film is proposed for the determination of persulfate in commercial samples of hair bleaching boosters by amperometry. The detection was obtained by chronoamperometric technique and the sample is injected into the electrochemical cell in a wall jet configuration. Potassium chloride at concentration of 0.1 mol L-1 acted as sample carrier at a flow rate of 4.0 mL min-1 and supporting-electrolyte. For 0.025 V (vs. Ag/AgCl) applied voltage, the proposed system handles ca. 160 samples per hour (1.0 10-4 - 1.0 10-3 mol L-1 of persulfate), consuming about 200 μL sample and 11 mg KCl per determination. Typical linear correlations between electrocatalytic current and persulfate concentration was ca. 0.9998. The detection limit is 9.0 10-5 mol L-1 and the calculated amperometric sensibility 3.6 103 μA L mol -1. Relative standard deviation (n =12) of a 1.0 10-4 mol L-1 sample is about 2.2%. The method was applied to persulfate determination in commercial hair-bleaching samples and results are in agreement with those obtained by titrimetry at 95% confidence level and good recoveries (95 - 112%) of spiked samples were found. © 2003 by MDPI.

Evaluation of the mixtures ammonium phosphate/magnesium nitrate and palladium nitrate/magnesium nitrate as modifiers for simultaneous determination of Cd, Cr, Ni and Pb in mineral water by GFAAS

A method is described for the simultaneous determination of Cd, Cr, Ni and Pb in mineral water samples by graphite furnace atomic absorption spectrometry with a transversely heated graphite atomizer (THGA) and a longitudinal Zeeman-effect background correction system. The electrothermal behavior of analytes during pyrolysis and atomization steps was studied without modifier, in presence of 5 μg Pd and 3 μg Mg(NO3)2 and in presence of 50 μg NH4H2PO4 and 3 μg Mg(NO3)2. A volume of 20 μL of a 0.028 mol L -1 HNO3 solution containing 50 μg L-1 Ni and Pb, 10 μg L-1 Cr and 5 μg L-1 Cd was dispensed into the graphite tube at 20°C. The mixture palladium/magnesium was selected as the optimum modifier. The pyrolysis and atomization temperatures were fixed at 1000°C and 2300°C, respectively. The characteristic masses were calculated as 2.2 pg Cd, 10 pg Cr, 42 pg Ni and 66 pg Pb and the lifetime of the graphite tube was around 600 firings. Limits of detection based on integrated absorbance were 0.02 μg L-1Cd, 0.94 μg L-1 Cr, 0.45 μg L-1 Ni and 0.75 μg L-1 Pb, which exceeded the requirements of Brazilian Food Regulation that establish the maximum permissible level for Cd, Cr, Ni and Pb at 3 μg L-1, 50 μg L-1, 20 μg L-1 and 10 μg L-1, respectively. The recoveries of Cd, Cr, Ni and Pb added to mineral water samples varied within the 93-108%, 96-104%, 87-101% and 98-108% ranges, respectively. Results of analysis of standard reference materials (National Institute of Standards and Technology: 1640-Trace Elements in Natural Water; 1643d-Trace Elements in Water) were in agreement with certified values at the 95% confidence level.

Measurement of the pp(-)-> W gamma plus X cross section at root s=1.96 TeV and WW gamma anomalous coupling limits

The WWγ triple gauge boson coupling parameters are studied using pp̄rarr; νγ+X(=e,μ) events at s=1.96 TeV. The data were collected with the D0 detector from an integrated luminosity of 162pb-1 delivered by the Fermilab Tevatron Collider. The cross section times branching fraction for pp̄→W(γ)+X→ νγ+X with ETγ>8 GeV and ΔR γ> 0.7 is 14.8±1.6(stat)±1.0(syst) ±1.0(lum)pb. The one-dimensional 95% confidence level limits on anomalous couplings are -0.88<Δκγ<0.96 and -0. 20<λγ<0.20. © 2005 The American Physical Society.

Spectrophotometric determination of methyldopa in pharmaceutical formulations

A new, simple, precise, rapid and low-cost spectrophotometric method for methyldopa determination in pharmaceutical preparations is described. This method is based on the complexation reaction of methyldopa with molybdate. Absorbance of the resulting yellow coloured product is measured at 410 nm. Beer's Law is obeyed in a concentration range of 50 - 200 μg ml -1 methyldopa with an excellent correlation coefficient (r = 0.9999). No interference was observed from common excipients in formulations. The results show a simple, accurate, fast and readily applied method to the determination of methyldopa in pharmaceutical products. The analytical results obtained for these products by the proposed method are in agreement with those of the Brazilian Pharmacopoeia procedure at 95% confidence level.

Mortalidade e prognóstico específico em pacientes com insuficiência renal aguda

A variety of systems of risk factor stratification have been studied to predict the outcome in acute renal failure (ARF). OBJECTIVES. Assess and compare mortality and the Acute Tubular Necrosis Individual Severity Score (ATN-ISS) in patients with AFR treated in a university hospital. METHODS. A prospective analysis was made of 103 patients with a diagnosis of intrinsic ARF admitted to the Hospital das Clinicas da Faculdade de Medicina de Botucatu, UNESP. Patients were followed up until recovery of renal function or death. The Score ATN-ISS was recorded during the first hours of the assessment by a nephrologist. Results were reported as median or mean ± SD, with statistical significance of p<0.05. RESULTS. Fifty-one percent of patients were male with a mean age of 58 ± 36 years. Forty-four percent died in the hospital. Mortality was higher in patients from the surgical wards (52.7%) and in patients who were treated with dialysis (63.8%). The score ATN-ISS showed a good confidence level, with high discriminatory power (area under the curve of 0.95) and good accuracy. CONCLUSIONS. Mortality in this study was comparable to that found in literature. The ATN-ISS was shown to be a prognostic index with a high confidence level that could be routinely applied by nephrologists to patients with AFR.

Influence of light curing source on microhardness of composite resins of different shades

Introduction: The evolution of light curing units can be noticed by the different systems recently introduced. The technology of LED units promises longer lifetime, without heating and with production of specific light for activation of camphorquinone. However, further studies are still required to check the real curing effectiveness of these units. Purpose: This study evaluated the microhardness of 4 shades (B-0.5, B-1, B-2 and B-3) of composite resin Filtek Z-250 (3M ESPE) after light curing with 4 light sources, being one halogen (Ultralux - Dabi Atlante) and three LED (Ultraled - Dabi Atlante, Ultrablue - DMC and Elipar Freelight - 3M ESPE). Methods: 192 specimens were distributed into 16 groups, and materials were inserted in a single increment in cylindrical templates measuring 4mm x 4mm and light cured as recommended by the manufacturer. Then, they were submitted to microhardness test on the top and bottom aspects of the cylinders. Results: The hardness values achieved were submitted to analysis of variance and to Tukey test at 5% confidence level. It was observed that microhardness of specimens varied according to the shade of the material and light sources employed. The LED appliance emitting greater light intensity provided the highest hardness values with shade B-0.5, allowing the best curing. On the other hand, appliances with low light intensity were the least effective. It was also observed that the bottom of specimens was more sensitive to changes in shade. Conclusion: Light intensity of LED light curing units is fundamental for their good functioning, especially when applied in resins with darker shades.

Effect of rotary instrumentation and of the association of calcium hydroxide and chlorhexidine on the antisepsis of the root canal system in dogs

This study aimed at evaluating the antisepsis of the root canal system (RCS) and periapical region (PR) provided by rotary instrumentation associated with chlorhexidine + calcium hydroxide as intracanal medicament. Chronic periapical lesions were induced in 26 pre-molar roots in two dogs. After microbiological sampling, automatic instrumentation using the Profile system and irrigation with 5.25% sodium hypochlorite solution, with a final rinse of 14.3% EDTA followed by profuse irrigation with physiological saline were carried out in 18 root canals. After drying the canals, a paste based on calcium hydroxide associated with a 2% chlorhexidine digluconate solution was placed inside them. After 21 days, the medication was removed, leaving the root canals empty and coronally sealed. After 96 hours, a final microbiological sample was obtained, followed by histomicrobiological processing by the Brown & Brenn method. Eight untreated root canals represented the control group (C-G). Based on the Mann-Whitney test at a confidence level of 5% (p < 0.05), the procedures of antisepsis used offered significant efficacy (p < 0.05) resulting in 100.0% of the canals free of microorganisms. In the C-G, an elevated incidence of various microbial morphotypes was confirmed in all sites of the RCS, with the presence of microbial colonies in the periapical region. In contrast, the experimental group showed a similar pattern of infection in the RCS, although less intense and a reduced level of periapical infection (p < 0.05). It was concluded that adequate instrumentation followed by the application of calcium hydroxide + chlorhexidine offered significant elimination of microorganisms.

Determination of methyldopa in pharmaceutical formulations by combined spot test-diffuse reflectance spectroscopy

This paper describes a very simple and rapid quantitative reflectance spot test procedure for the determination of methyldopa in pharmaceutical formulations. This method is based on the complexation reaction of methyldopa with molybdate ions yielding a yellow stable complex on filter paper. Reflectance measurements were carried out at 410 nm. Under optimal conditions, the calibration graphs obtained for methyldopa by plotting the optical density of the reflectance signal (A R) vs. the log of the concentration were linear from 6.30 × 10 -3 to 1.89 × 10 -2 mol L -1, with a correlation coefficient of 0.998. The detection limit was 2.74 × 10 -3 mol L -1 (R.S.D. = 1.02%) for methyldopa. The common excipients used as additives in pharmaceuticals do not interfere in the proposed method. The method was applied to determine metyldopa in commercial pharmaceutical formulations. The results obtained by the proposed method compare favorably with those obtained by an official procedure at 95% confidence level. ©2006 Sociedade Brasileira de Química.

Effect of 10% carbamide peroxide dental bleaching on microhardness of filled and unfilled sealant materials

Purpose: The purpose of this study was to quantitatively evaluate the effect of 10% carbamide peroxide on the microhardness of pit and fissure sealant materials. Methods: Fluroshield, Vitroseal Alfa, and one unfilled (Clinpro) sealants were placed in Teflon matrices (4 mm in diameter by 2 mm in height) and polymerized for 40 seconds. A total of 20 specimens were prepared for each material, in which half were assigned as the control group (stored in artificial saliva and no bleaching treatment). For the remaining half, Clarigel Gold bleaching agent (10% carbamide peroxide) was placed over the specimen surface for 4 hours/day during 4 weeks. When specimens were not under bleaching treatment, they were kept in artificial saliva. Afterwards, specimens were subjected to Knoop microhardness testing using a 25-g load for 5 seconds. Five measurements were made on the sealants' surfaces and then calculated in Knoop hardness values. The data were statistically analyzed by two-way analysis of variance and Tukey's tests with a 5% confidence level. Results: The results of this in vitro study showed that the application of a carbamide peroxide-based bleaching material significantly affected the microhardness values of filled sealant materials. The bleaching agent did not affect the microhardness of the unfilled sealant. CLINICAL SIGNIFICANCE: The results of this in vitro study suggest that the bleaching agents altered the surface hardness of filled sealant restorative materials. This could possibly lead to increased wear and surface roughness. © 2006, Copyright the authors.

Comparative studies of the sample decomposition of green and roasted coffee for determination of nutrients and data exploratory analysis

The contents of some nutrients in 35 Brazilian green and roasted coffee samples were determined by flame atomic absorption spectrometry (Ca, Mg, Fe, Cu, Mn, and Zn), flame atomic emission photometry (Na and K) and Kjeldahl (N) after preparing the samples by wet digestion procedures using i) a digester heating block and ii) a conventional microwave oven system with pressure and temperature control. The accuracy of the procedures was checked using three standard reference materials (National Institute of Standards and Technology, SRM 1573a Tomato Leaves, SRM 1547 Peach Leaves, SRM 1570a Trace Elements in Spinach). Analysis of data after application of t-test showed that results obtained by microwave-assisted digestion were more accurate than those obtained by block digester at 95% confidence level. Additionally to better accuracy, other favorable characteristics found were lower analytical blanks, lower reagent consumption, and shorter digestion time. Exploratory analysis of results using Principal Component Analysis (PCA) and Hierarchical Cluster Analysis (HCA) showed that Na, K, Ca, Cu, Mg, and Fe were the principal elements to discriminate between green and roasted coffee samples. ©2007 Sociedade Brasileira de Química.

Compressive fatigue in titanium dental implants submitted to fluoride ions action

The aim of this study was to assess the influence of a fluoridated medium on the mechanical properties of an internal hexagon implant-abutment set, by means of compression, mechanical cycling and metallographic characterization by scanning electronic microscopy. Five years of regular use of oral hygiene with a sodium fluoride solution content of 1500 ppm were simulated, immersing the samples in this medium for 184 hours, with the solutions being changed every 12 hours. Data were analyzed at a 95% confidence level with Fisher's exact test. After the action of fluoride ions, a negative influence occurred in the mechanical cycling test performed in a servohydraulic machine (Material Test System-810) set to a frequency of 15 Hz with 100,000 cycles and programmed to 60% of the maximum resistance of static compression test. The sets tended to fracture by compression on the screw, characterized by mixed ruptures with predominance of fragile fracture, as observed by microscopy. An evidence of corrosion by pitting on sample surfaces was found after the fluoride ions action. It may be concluded that prolonged contact with fluoride ions is harmful to the mechanical properties of commercially pure titanium structures.

A simplified reflectometric method for the rapid determination of dipyrone in pharmaceutical formulations

This paper describes a simple, portable and environmentally friendly method for the rapid determination of dipyrone in pharmaceuticals by using diffuse reflectance spectroscopy. The proposed method is based on the reflectance measurements of the orange compound produced from the spot test reaction between dipyrone and p-dimethylaminocinnamaldehyde (p-DAC), in acid medium, using a filter paper as solid support. Experimental design methodologies were used to optimize the measurement conditions. All reflectance measurements were carried out at 510 nm and the linear range was from 1.42 × 10-4-2.85 × 10-3 mol L-1, with a correlation coefficient of 0.999. The limit of detection (LOD) and the limit of quantification (LOQ) were 1.20 × 10-5 mol L-1 and 4.00 × 10-5 mol L-1, respectively. The intraday precision and interday precision were studied for 10 replicate analyses of 7.90 × 10-4 mol L-1 dipyrone solution. The coefficients of variation were 1.1 and 0.9%, respectively. The proposed method was applied successfully to the determination of dipyrone in commercial brands of pharmaceuticals. No interferences were observed from the common excipients in formulations. The results obtained by the proposed method were favorably compared with those given by the Brazilian Pharmacopoeia procedure at 95% confidence level. ©2007 Sociedade Brasileira de Química.

Search for Randall-Sundrum gravitons with 1 fb(-1) of data from p(p)over-bar collisions at root s=1.96 TeV

We search for decays of Kaluza-Klein excitations of the graviton in the Randall-Sundrum model of extra dimensions to e+e- and in 1 fb-1 of pp collisions at s=1.96 TeV collected by the D0 detector at the Fermilab Tevatron. We set 95% confidence level upper limits on the production cross section times branching fraction, which translate into lower limits on the mass of the lightest excitation between 300 and 900 GeV for values of the coupling k/M Pl between 0.01 and 0.1. © 2008 The American Physical Society.

A simple spectrophotometric method for the determination of methyldopa using p-chloranil in the presence of Hydrogen Peroxide

A simple, rapid and sensitive spectrophotometric method has been developed for the determination of methyldopa in pharmaceutical formulations. The method is based on the reaction between tetrachloro-p-benzoquinone (p-chloranil) and methyldopa, accelerated by hydrogen peroxide (H 2O 2), producing a violet-red compound (λmax = 535 nm) at ambient temperature (25.0 ± 0.2°C). Experimental design methodologies were used to optimize the measurement conditions. Beer's law is obeyed in a concentration range from 2.10 × 10 -4 to 2.48 × 10 -3 mol L -1 (r = 0.9997). The limit of detection was 7.55 × 10 -6 mol L -1 and the limit of quantification was 2.52 × 10 -5 mol L -1. The intraday precision and interday precision were studied for 10 replicate analyses of 1.59 × 10 -3 mol L -1 methyldopa solution and the respective coefficients of variation were 0.7 and 1.1%. The proposed method was successfully applied to the determination of methyldopa in commercial brands of pharmaceuticals. No interferences were observed from the common excipients in the formulations. The results obtained by the proposed method were favorably compared with those given by the Brazilian Pharmacopoeia procedure at 95% confidence level.

Evaluation of creatine kinase (CK) and aspartate aminotransferase (AST) activities after laparoscopic or conventional ovariectomy in queens

Creatine kinase (CK) and aspartate aminotransferase (AST) are mainly muscle-specific enzymes, which can be associated with muscle tissue damage. The aim of this study was to assess the activities of CK and AST during the postoperative period, after conventional (G1) and videolaparoscopic ovariectomy (G2), in queens. A further group (G3) was subjected to anaesthesia only. Results demonstrate that there were significant differences between groups. The highest levels of CK were recorded in Gl, however at a confidence level of p < 0.05 there was no significant difference between groups during the first 6 hours after surgery. A significant (p < 0.05) increase of CK values was identified between 0h and 3h in both groups (Gl and G2). Regarding AST activity there was no significant variation between groups, but again there was a significant difference between values at 0h and 3h after surgery. In conclusion, ovariectomy performed by videolap-aroscopy seems to cause less muscle damage when compared to the conventional method. © 2009 by Verlag Hans Huber, Hogrefe AG, Bem.