Simultaneous determination of Cd and Pb in antibiotics used in sugar-cane fermentation process by GFAAS

A method has been developed for the simultaneous determination of Cd and Pb in antibiotics used in sugar-cane fermentation by GFAAS. The integrated platform of transversely heated graphite atomizer was treated with tungsten to form a coating of tungsten carbide. Six samples of commercial solid antibiotics were analyzed by injecting 20 μL of digested samples into the pretreated graphite platform with co-injection of 5 μL of 1000 mg L-1 Pd as chemical modifier. Samples were mineralized in a closed-vessel microwave-assisted acid-digestion system using nitric acid plus hydrogen peroxide. The pyrolysis and atomization temperatures of the heating program of the atomizer were selected as 600°C and 2200°C, respectively. The calculated characteristic mass for Cd and Pb was 1.6 pg and 42 pg, respectively. Limits of detection (LOD) based on integrated absorbance were 0.02 μg L -1 Cd and 0.7 μg L-1 Pb and the relative standard deviations (n = 10) for Cd and Pb were 5.7% and 8.0%, respectively. The recoveries of Cd and Pb added to the digested samples varied from 91% to 125% (Cd) and 80% to 112% (Pb).

Direct and simultaneous determination of As, Cu, and Pb in Brazilian sugar cane spirits by graphite furnace AAS using tungsten permanent modifier with co-injection of Pd/Mg(N03)2

A method was developed using the multi-element graphite furnace atomic absorption spectrometry technique for the direct and simultaneous determination of As, Cu, and Pb in Brazilian sugar cane spirit (cachaça) samples. Also employed was the end-capped transversely heated graphite atomizer (THGA) with platforms pre-treated with W permanent modifier and co-injection of Pd/Mg(N03)2. Pyrolysis and atomization temperature curves were established in a cachaça medium (1+1; v/v) containing 0.2% (v/v) HN03 and spiked with 20 μg L-1 As and Pb and 200 μg L-1Cu. The effect of the concentration of major elements usually present in cachaça matrices (Ca, Mg, Na, and K) and ethanol on the absorbance of As, Cu, and Pb was investigated. Analytical working solutions of As, Cu, and Pb were prepared in 10% (v/v) ethanol plus 5.0 mg L-1 Ca, Mg, Na, and K. Acidified to 0.2% (v/v) HNO3, these solutions were suitable to build calibration curves by matrix matching. The proposed method was applied to the simultaneous determination of As, Cu, and Pb in commercial sugar cane spirits. The characteristic mass for the simultaneous determination was 16 pg As, 119 pg Cu, and 28 pg Pb. The pretreated tube lifetime was about 450 firings. The limit of detection (LOD) was 0.6 μg L-1As, 9.2 μg L-1 Cu, and 0.3 μg L-1Pb. The found concentrations varied from 0.81 to 4.28 μg L-1As, 0.28 to 382 mg L-1 Cu and 0.82 to 518 μg L-1 Pb. The recoveries of the spiked samples varied from 94-112% (As), 97-111% (Cu), and 95-101% (Pb). The relative standard deviation (n=12) was 6.9%, 7.4%, and 7.7% for As, Cu, and Pb, respectively, present in a sample at 0.87 μgL-1, 0.81 mgL-1, and 38.9 μgL-1concentrations.

Critical parameter determination of sonic flow controller diamond microtubes and micronozzles

In this article, the authors measure throughput of sonic diamond microtubes and micronozzles that can work as passive gas flow controllers and flow meters under choking conditions. The behavior of the outlet pressure through the microdevices using an experimental setup with constant volume and constant temperature was determined in order to obtain the critical throughput, the critical mass flow rate, and the discharge coefficients of the diamond sonic microdevices. © 2007 American Vacuum Society.

Determination of BTEX by GC-MS in air of offset printing plants: Comparison between conventional and ecological inks

The use of inks containing organic solvents by the offset printing process implies in the release of volatile organic compounds to the work environment. Many of these compounds such as benzene, toluene, ethylbenzene, and the xylene isomers (well known by the acronym BTEX) are extremely toxic. In this study, the BTEX concentrations were determined in two different printing plants that use distinct types of inks: the conventional and the so-called ecological, which is manufactured based on vegetal oil. Concentration ranges were 43-84, 15-3,480, 2-133, 5-459, and 2-236 μg m-3 for benzene, toluene, ethylbenzene, m + p-xylene, and o-xylene, respectively, for the conventional printing plant. At the ecological printing plant, concentration ranges were below limit of detection (

Determination of broiler femur parameters at different growth phases

The objective of this experiment was to analyse macroscopically the femur and determine the biochemical values at 8, 22 and 42 days of age, producing basic results that can help to understand the pathogeny of the locomotor problems and the broiler physiologic growth. A total of 60 Cobb male broilers were distributed in three age groups (8, 22 and 42 days of age) of 20 birds. All macroscopic measurements, except the cranial compact layer increased (p<0.05) over the course of the ages. The cranial compact layer presented the biggest measure at 22 days of age. The ash percentage increased (p<0.05) until 22 days of age, but at 42 days of age this values decreased. Calcium and phosphorus percentage in ash increased (p<0.05) until 22 days of age and evidenced constancy from 22 to 42 days of age. The biomechanical adaptation capacity of femur was evidenced by the increase of the macroscopic measures over the course of the ages and the different behavior of cranial compact layer at 22 days of age suggested an adaptation attempt of the immature bone to muscle mass increase. The ash and mineral percentage confirmed that the relative growth occurs with more intensity until 21 days of age. The calcium and phosphorus percentage evidenced the physiologic balance acting on the deposition of these minerals in femur. © Asian Network for Scientific Information, 2011.

Combination of the top-quark mass measurements from the Tevatron collider

The top quark is the heaviest known elementary particle, with a mass about 40 times larger than the mass of its isospin partner, the bottom quark. It decays almost 100% of the time to a W boson and a bottom quark. Using top-antitop pairs at the Tevatron proton-antiproton collider, the CDF and D0 Collaborations have measured the top quark's mass in different final states for integrated luminosities of up to 5.8fb -1. This paper reports on a combination of these measurements that results in a more precise value of the mass than any individual decay channel can provide. It describes the treatment of the systematic uncertainties and their correlations. The mass value determined is 173.18±0.56(stat)±0.75(syst)GeV or 173.18±0.94GeV, which has a precision of ±0.54%, making this the most precise determination of the top-quark mass. © 2012 American Physical Society.

Determination of disease biomarkers in Eucalyptus by comprehensive two-dimensional gas chromatography and multivariate data analysis

In this paper is reported the use of the chromatographic profiles of volatiles to determine disease markers in plants - in this case, leaves of Eucalyptus globulus contaminated by the necrotroph fungus Teratosphaeria nubilosa. The volatile fraction was isolated by headspace solid phase microextraction (HS-SPME) and analyzed by comprehensive two-dimensional gas chromatography-fast quadrupole mass spectrometry (GC. ×. GC-qMS). For the correlation between the metabolic profile described by the chromatograms and the presence of the infection, unfolded-partial least squares discriminant analysis (U-PLS-DA) with orthogonal signal correction (OSC) were employed. The proposed method was checked to be independent of factors such as the age of the harvested plants. The manipulation of the mathematical model obtained also resulted in graphic representations similar to real chromatograms, which allowed the tentative identification of more than 40 compounds potentially useful as disease biomarkers for this plant/pathogen pair. The proposed methodology can be considered as highly reliable, since the diagnosis is based on the whole chromatographic profile rather than in the detection of a single analyte. © 2013 Elsevier B.V..

Cost-effective composite electrode for the fast voltammetric screening and determination of riboflavin (B2) and pyridoxine (B6) in pharmaceuticals

Different solid composites made by mechanical dispersions of graphite particles into heated paraffin (from 65 to 80% graphite, in mass) were prepared and assessed in order to optimize their use in electrochemical and electroanalytical procedures for bioanalysis. Besides these, composites were also evaluated by thermoanalytical techniques aiming to study their conservation and long-term stability (over eight months without special care), among others. Best results were found at 80% m/m graphite in paraffin. Such electrode combines low-cost, stability, sensitivity, ease of maintenance and clearance, besides the possibilities of manufacture in many different forms and shapes (with or without modifications) and applicability in a wide range of pH. Electrochemical studies by different voltammetric techniques involving vitamins from complex B (riboflavin and pyridoxine) leaded to a better understanding about their electrooxidative processes onto carbon-composite electrodes, specially regarding reversibility and pH-dependence. Data were also acquired and optimized with analytical purposes, being square-wave voltammetry in pH 4.2 chosen by its many advantages. Good linearity between peak responses as function of concentration were reached from 5 to 43 μmol L-1 for riboflavin (peak at -0.257 V) and up to 8.5 × 10-4 mol L -1 for pyridoxine (peak at +1.04 V), best studied conditions; limits of detection (at an S/N of 3) for both analites showed to be circa 1.0 mol L-1. Different commercial samples were analyzed for riboflavin (EMS® complex B syrup) and pyridoxine (Citoneurin 5000 Merck® ampoules) providing 96.6% and 98.7% recoveries, respectively.

Measurement of the ratio of the inclusive 3-jet cross section to the inclusive 2-jet cross section in pp collisions at root s=7 TeV and first determination of the strong coupling constant in the TeV range

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Determination of pantoprazole in human plasma by LC-MS-MS using lansoprazole as internal standard

An analytical method based on liquid chromatography with positive ion electrospray ionization (ESI) coupled to tandem mass spectrometry detection was developed for the determination of pantoprazole (CAS 102625-70-7) in human plasma using lansoprazole (CAS 103577-45-3) as the internal standard. The analyte and internal standard were extracted from the plasma samples by liquid/liquid extraction using diethyl-ether/dichloromethane (70:30; v/v) and chromatographed on a C-8 analytical column. The mobile phase consisted of acetonitrile/water/methanol (57:25:18; v/v/v) + 10 mmol/l acetic acid + 20 mmol/l ammonium acetate. The method has a chromatographic total run time of 4.5 min and was linear within the range 5.0-5,000 ng/mL. Detection was performed on a triple quadrupole tandem mass spectrometer by Multiple Reaction Monitoring (MRM). The intra- and inter-run precisions calculated from quality control (QC) samples were 4.2% and 3.2%, respectively. The accuracies as determined from QC samples were -5.0% (intra-run) and 2.0% (inter-run). The method herein described was employed in a bioequivalence study of two tablet formulations of pantoprazole.

Determination of lead in eye shadow and blush by high-resolution continuum source graphite furnace atomic absorption spectrometry employing directSolid sampling

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Metalloproteomic profile determination of muscle samples from nile Tilapia (Oreochromis niloticus) using AAS and ESI-MS/MS after 2D-PAGE separation

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Measurement of the inclusive 3-jet production differential cross section in proton-proton collisions at 7 TeV and determination of the strong coupling constant in the TeV range

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Specific determination of maximal lactate steady state in soccer players

The aim of this study was to establish the validity of the anaerobic threshold (AT) determined on the soccer-specific Hoff circuit (AT(Hoff)) to predict the maximal lactate steady-state exercise intensity (MLSSHoff) with the ball. Sixteen soccer players (age: 16.0 +/- 0.5 years; body mass: 63.7 +/- 9.0 kg; and height: 169.4 +/- 5.3 cm) were submitted to 5 progressive efforts (7.0-11.0 km.h(-1)) with ball dribbling. Thereafter, 11 players were submitted to 3 efforts of 30 minutes at 100, 105, and 110% of AT(Hoff). The AT(Hoff) corresponded to the speed relative to 3.5 mmol.L-1 lactate concentration. The speed relative to 4.0 mmol.L-1 was assumed to be AT(Hoff4.0), and the AT(HoffBI) was determined through bisegmented adjustment. For comparisons, Student's t-test, intraclass correlation coefficient (ICC), and Bland and Altman analyses were used. For reproducibility, ICC, typical error, and coefficient of variation were used. No significant difference was found between AT test and retest determined using different methods. A positive correlation was observed between AT(Hoff) and AT(Hoff4.0). The MLSSHoff (10.6 +/- 1.3 km.h(-1)) was significantly different compared with AT(Hoff) (10.2 +/- 1.2 km.h(-1)) and AT(HoffBI) (9.5 +/- 0.4 km.h(-1)) but did not show any difference from LAn(Hoff4.0) (10.7 +/- 1.4 km.h(-1)). The MLSSHoff presented high ICCs with AT(Hoff) and AT(Hoff4.0) (ICC = 0.94; and ICC = 0.89; p <= 0.05, respectively), without significant correlation with AT(HoffBI). The results suggest that AT determined on the Hoff circuit is reproducible and capable of predicting MLSS. The AT(Hoff4.0) was the method that presented a better approximation to MLSS. Therefore, it is possible to assess submaximal physiological variables through a specific circuit performed with the ball in young soccer players.

Determination of the mercury fraction linked to protein of muscle and liver tissue of Tucunaré (Cichla spp.) from the Amazon Region of Brazil

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)