Determination of fluoxetine in plasma by gas chromatography-mass spectrometry using stir bar sorptive extraction

This article presents a method employing stir bar sorptive extraction (SBSE) with in situ derivatization, in combination with either thermal or liquid desorption on-line coupled to gas chromatography-mass spectrometry for the analysis of fluoxetine in plasma samples. Ethyl chloroformate was employed as derivatizing agent producing symmetrical peaks. Parameters such as solvent polarity, time for analyte desorption, and extraction time, were evaluated. During the validation process, the developed method presented specificity, linearity (R-2 > 0.99), precision (R.S.D. < 15%), and limits of quantification (LOQ) of 30 and 1.37 pg mL(-1), when liquid and thermal desorption were employed, respectively. This simple and highly sensitive method showed to be adequate for the measurement-of fluoxetine in typical and trace concentration levels. (c) 2008 Elsevier B.V. All rights reserved.

An analysis of quit and dismissal determinants between 1988 and 1999 using the bivariate probit model

Excessive labor turnover may be considered, to a great extent, an undesirable feature of a given economy. This follows from considerations such as underinvestment in human capital by firms. Understanding the determinants and the evolution of turnover in a particular labor market is therefore of paramount importance, including policy considerations. The present paper proposes an econometric analysis of turnover in the Brazilian labor market, based on a partial observability bivariate probit model. This model considers the interdependence of decisions taken by workers and firms, helping to elucidate the causes that lead each of them to end an employment relationship. The Employment and Unemployment Survey (PED) conducted by the State System of Data Analysis (SEADE) and by the Inter-Union Department of Statistics and Socioeconomic Studies (DIEESE) provides data at the individual worker level, allowing for the estimation of the joint probabilities of decisions to quit or stay on the job on the worker’s side, and to maintain or fire the employee on the firm’s side, during a given time period. The estimated parameters relate these estimated probabilities to the characteristics of workers, job contracts, and to the potential macroeconomic determinants in different time periods. The results confirm the theoretical prediction that the probability of termination of an employment relationship tends to be smaller as the worker acquires specific skills. The results also show that the establishment of a formal employment relationship reduces the probability of a quit decision by the worker, and also the firm’s firing decision in non-industrial sectors. With regard to the evolution of quit probability over time, the results show that an increase in the unemployment rate inhibits quitting, although this tends to wane as the unemployment rate rises.

Spectrophotometric determination of ceftazidime in pharmaceutical preparations using neocuproin as a complexing agent

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Validation of an HPLC Method for quantitative Determination of Benzocaine in PHBV-Microparticles and PLA-Nanoparticles

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

Parturition intervals and distributions of parturitions by months of buffalo in Southern and South-eastern Brazil

Reproductive rate is an important component of economic success in livestock production. Parturition interval (IEP) is a direct measure of the productivity of the animal. Long IEP reduce the number of calves produced per year. The objective this study was to determine the distribution of parturitions across month and to evaluate factors affecting IEP. The data included 7,588 parturitions of Murrah, Mediterranean and Carabobo buffalo from 10 herds in Southern and South-eastern Brazil. The analysis of distribution of parturitions evaluated the effects of month, year and their interaction on birth date of calves by using a Chi-Square test in SAS PROC FREQ (SAS Institute, Cary, NC, USA). Parturition intervals (n = 2,630) were evaluated using analysis of variance in SAS PROC GLM. The model for IEP included the fixed effects of season (December to May = 1, June to November = 2), year, season x year, sex of the preceding parturition, age of weaning of the previous calf, and herd. All sources of variation were significant (P<0.0001) except sex of the preceding parturition (P <0.85). The mean IEP was 446.7 +/- 10.4 days, for seasons 1 and 2 IEP were 419.8 +/- 11.3 and 473.6 +/- 40.7 days, respectively, a difference of 54 days. As weaning age increased there was a lengthening of IEP. Buffalo in Brazil showed seasonal parturition with calving concentrated from January to April, although the frequency by month differed across years (P<0.0001). These months also had the lowest calving interval.

Ultrastructural characteristics of spermatogenesis in Pallas's mastiff bat, Molossus molossus (Chiroptera: Molossidae)

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Voltammetric Determination of Phosphate in Brazilian Biodiesel Using Two Different Electrodes

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Determination of nitrite in meat products and water using dapsone with combined spot test/diffuse reflectance on filter paper

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Spot-test identification and rapid quantitative sequential analysis of dipyrone

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

Rapid and sensitive method for the determination of acetaldehyde in fuel ethanol by high-performance liquid chromatography with UV-Vis detection

A high-performance liquid chromatography (HPLC) method for the determination of acetaldehyde in fuel ethanol was developed. Acetaldehyde was derivatized with 0.900 mL 2,4-dinitrophenylhydrazine (DNPHi) reagent and 50 mu L phosphoric acid 1 mol L-1 at a controlled room temperature of 15 degrees C for 20 min. The separation of acetaldehyde- DNPH (ADNPH) was carried out on a Shimadzu Shim-pack C-18 column, using methanol/LiCl(aq) 1.0 mM (80/20, v/v) as a mobile phase under isocratic elution and UV-Vis detection at 365 nm. The standard curve of ADNPH was linear in the range 3-300 amg L-1 per injection (20 mu L) and the limit of detection (LOD) for acetaldehyde was 2.03 mu g L-1, with a correlation coefficient greater than 0.999 and a precision (relative standard deviation, RSD) of 5.6% (n=5). Recovery studies were performed by fortifying fuel samples with acetaldehyde at various concentrations and the results were in the range 98.7-102%, with a coefficient of variation (CV) from 0.2% to 7.2%. Several fuel samples collected from various gas stations were analyzed and the method was successfully applied to the analysis of acetaldehyde in fuel ethanol samples.

The relations between different levels of government in Brazil

Includes bibliography

Voltammetric determination of phosphate in brazilian biodiesel using two different electrodes

The presence of contaminants, such as phosphate, in biodiesel, has several drawbacks for instance: current engines perform poorly, fuel tanks deteriorate, catalytic conversion is damaged, and particles emission is increased. Therefore, biodiesel quality control is extremely important for biodiesel acceptance and commercialization worldwide. In this context, a bare glassy carbon electrode (GCE) and another chemically modified electrode with iron hexacyanoferrate (Prussian Blue – PB) were developed for determination of phosphate in biodiesel. The LODs of 6.44 and 1.19 mg kg−1, and LOQs of 21.43 and 3.97 mg kg−1 were obtained for the bare GCE and the PB-modified GCE, respectively. The methodology was employed for analysis of Brazilian biodiesel samples, and it led to satisfactory results, demonstrating its potential application for biodiesel quality control. Additionally, recovery and interference tests were conducted, which revealed that the developed methods are suitable for analysis of phosphate in biodiesel samples.

Degradation, residual determination, and cholinesterase activity of triclorfon in Piaractus mesopotamicus Holmberg (Pacu) 1887

The aim of this study was to determine the no-observable-adverse-effect concentration (NOAEC) for trichlorfon, an antiparasitic agent used in aquaculture, in Piractus mesopotamicus (pacu) using acetylcholinesterase (AChE) activity as an end point. Fish were exposed 24 h/d for 15 d to different concentrations of trichlorfon in tanks of water for which a curve of dissipation was previously determined. Analysis of trichlorfon in water and fish plasma using gas chromatography with electron capture detection (GC-ECD) enabled measurement of limit of detection (LOD) and limit of quantification (LOQ), respectively, to be 3 and 10 ppb. Thirty-six hours after trichlorfon dilution in water, the concentration was below the LOD, and data showed that plasma concentrations did not exceed the LOQ. Apart from the 6.25 g/L, all concentrations of trichlorfon significantly inhibited plasma and brain AChE activity compared to controls. The AChE activity levels returned to control values in 7 d. These data may be useful to determine the concentration of trichlorfon that destroys parasites without producing adverse effects in fish.

Electroanalytical determination of bumetanide employing a biomimetic sensor for detection of doping in sports

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Analysis of Steroids using Solid Phase Microextraction-Gas Chromatography-Mass Spectrometry-Mass Spectrometry (SPME-GC-MS-MS)

Direct immersion SPME-GC-MS-MS was used for the analysis of steroids in water at part-per-trillion(ppt) and lower concentrations. The method was validated and extended to real sample analysis. The method were linear from 0.01 to 5 ng/ml with precision less than 10% relative standard deviation for a steroid mixture at 1 ng/ml. Limit of quantitation and limit of detection was found to be 200- 1200 pg/L and 30-200 pg/L respectively and recoveries ranged from 88-103 %. To understand the extraction efficiency of the fiber, a depletion study was performed. The fiber/ sample partition coefficients for the steroids were determined to be 1.0 x 104 to 1.5 x 104 . The extraction was performed without derivatization or the use of an internal standard. SPMEGC-MS-MS effectively demonstrated ultra-trace level detection of steroids in water.