Quantitative ester analysis in cachaca and distilled spirits by gas chromatography-mass spectrometry (GC-MS)

An analytical procedure for the separation and quantification of ethyl acetate, ethyl butyrate, ethyl hexanoate, ethyl lactate, ethyl octanoate, ethyl nonanoate, ethyl decanoate, isoamyl octanoate, and ethyl laurate in cachaca, rum, and whisky by direct injection gas chromatography-mass spectrometry was developed. The analytical method is simple, selective, and appropriated for the determination of esters in distilled spirits. The limit of detection ranged from 29 (ethyl hexanoate) to 530 (ethyl acetate) mu g L-1, whereas the standard deviation for repeatability was between 0.774% (ethyl hexanoate) and 5.05% (isoamyl octanoate). Relative standard deviation values for accuracy vary from 90.3 to 98.5% for ethyl butyrate and ethyl acetate, respectively. Ethyl acetate was shown to be the major ester in cachaca (median content of 22.6 mg 100 mL(-1) anhydrous alcohol), followed by ethyl lactate (median content of 8.32 mg 100 mL(-1) anhydrous alcohol). Cachaca produced in copper and hybrid alembic present a higher content of ethyl acetate and ethyl lactate than those produced in a stainless-steel column, whereas cachaca produced by distillation in a stainless-steel column present a higher content of ethyl octanoate, ethyl decanoate, and ethyl laurate. As expected, ethyl acetate is the major ester in whiskey and rum, followed by ethyl lactate for samples of rum. Nevertheless, whiskey samples exhibit ethyl lactate at contents lower or at the same order of magnitude of the fatty esters.

Chemical analysis of dairy cattle feed from Brazil

The bovine dairy cattle demand diets of high nutritional value being essential to know chemical composition of feed supplied to cows to achieve high levels of quality, safety and productivity of milk. Different roughages and concentrates from Minas Gerais and Rio Grande do Sul states, Brazil, were analyzed by instrumental neutron activation analysis (INAA) and inductively coupled plasma mass spectrometry (ICP-MS). Concentrate and roughage samples were differentiated by mass fractions of As, Ba, Mg, P, Rb and Sr. Samples of concentrate from both origins were differentiated by mass fractions of As, Cd, Co, Cr, Cs, Ni and Rb.

Lower Extremities Magnetic Resonance Angiography With Blood Pressure Cuff Compression: Quantitative Dynamic Analysis

Purpose: To quantitatively evaluate changes induced by the application of a femoral blood-pressure cuff (BPC) on run-off magnetic resonance angiography (MRA). which is a method generally previously proposed to reduce venous contamination in the leg. Materials and Methods: This study was Health Insurance Portability and Accountability Act (HIPAA)- and Institutional Review Board (IRB)-compliant, We used time-resolved gradient-echo gadolinium (Gd)-enhanced MRA to measure BPC effects on arterial, venous, and soft-tissue enhancement. Seven healthy volunteers (six men) were studied with the BPC applied at the mid-femoral level unilaterally using a 1.5T MR system after intravenous injection of Gd-BOPTA. Different statistical tools were used such as the Wilcoxon signed rank test and a cubic smoothing spline fit. Results: We found that BPC application induces delayed venous filling (as previously described), but also induces significant decreases in arterial inflow, arterial enhancement, vascular-soft tissue contrast, and delayed peak enhancement (which have not been previously measured). Conclusion: The potential benefits from using a BPC for run-off MRA must be balanced against the potential pitfalls, elucidated by our findings.

Quantitative CT analysis of the glabellar and anterior nasal spine regions for the placement of implants for nasal prosthesis retention

Objectives: The aim of this study was to determine the precision of the measurements of 2 craniometric anatomic points-glabella and anterior nasal spine-in order to verify their possibility as potential locations for placing implants aimed at nasal prostheses retention. Methods: Twenty-six dry human skulls were scanned in a high-resolution spiral tomography with 1-mm axial slice thickness and 1-mm interval reconstruction using a bone tissue filter. Images obtained were stored and transferred to an independent workstation containing e-film imaging software. The measurements (in the glabella and anterior nasal fossa) were made independently by 2 observers twice for each measurement. Data were submitted to statistical analysis (parametric t test). Results: The results demonstrated no statistically significant difference between interobserver and intraobserver measurements (P > .05). The standard error was found to be between 0.49 mm and 0.84 mrn for measurements in bone protocol, indicating a high /eve/ of precision. Conclusions: The measurements obtained in anterior nasal spine and glabella were considered precise and reproducible. Mean values of such measurements pointed to the possibility of implant placement in these regions, particularly in the anterior nasal spine.

Chemical analysis of the essential oil extracted from the seeds of Licaria puchury-major

The essential oil from seeds of Licaria puchury-major was isolated by hydrodistillation. The chemical composition of the oil was analyzed by GC and GUMS. Sixteen compounds were identified, representing 91.4% of the total oil. The major components were safrole (58.4%), dodecanoic acid (13.7%) and alpha-terpineol (8.4%). Oxygenated monoterpenoids were the main group of compounds.

Determination of Cr, Fe, Co, Ni, Cu, Zn, As and Pb in liquid chemical waste by energy dispersive X-ray fluorescence

A method for simultaneous determination of Cr, Fe, Co, Ni, Cu, Zn, As e Pb in liquid chemical waste using Energy Dispersive X-Ray Fluorescence (EDXRF) technique was evaluated. A small sample amount (200 mu L) was dried on a 6.35 mu m thickness Mylar film at 60 degrees C and the analyses were carried out using an EDXRF spectrometer operated with an X-ray Mo tube (Zr filter) at 30 kV/20 mA. The acquisition time was 300 s and the Ga element was utilized as internal standard at 25 mg/L for quantitative analysis. The method trueness was assessed by spiking and the detection limit for those elements ranged from 0.39 to 1.7 mg/L. This method is notable because it assists the choice of the more appropriated waste treatment procedure, in which inter elemental interference is a matter of importance. In addition, this inexpensive method allows a non-destructive determination of the elements from (19)K to (92)U simultaneously.

Quantitative analysis of aluminum dross by the Rietveld method

Aluminum white dross is a valuable material principally due to its high metallic aluminum content. The aim of this work is to develop a method for quantitative analysis of aluminum white dross with high accuracy. Initially, the material was separated into four granulometric fractions by means of screening. Two samples of each fraction were obtained, which were analyzed by means of X-ray fluorescence and energy dispersive spectroscopy in order to determine the elements present in the samples. The crystalline phases aluminum, corundum, spinel, defect spinel, diaoyudaoite, aluminum nitride, silicon and quartz low were identified by X-ray diffraction. The quantitative phase analysis was performed by fitting the X-ray diffraction profile with the Rietveld method using the GSAS software. The following quantitative results were found: 77.8% aluminum, 7.3% corundum, 2.6% spinel, 7.6% defect spinel, 1.8% diaoyudaoite, 2.9% aluminum nitride, and values not significant of quartz and silicon.

THE EFFECT OF REFRIGERATED STORAGE ON SENSORY PROFILE AND PHYSICAL-CHEMICAL CHARACTERISTICS OF MINIMALLY PASTEURIZED ORANGE JUICE

Minimal pasteurization of orange juice (OJ) consists of using minimum holding time and temperature to ensure partial inactivation of pectin methylesterase (PME). This process produces juice with preserved sensory attributes and has a better acceptance by consumers when compared with commercially pasteurized OJ. Sensory profile and physical-chemical characteristics of minimally processed OJ was determined, during refrigerated storage, for two OJ blends with different pH values and the same level of PME thermal inactivation. A selected and trained sensorial panel (n = 16) performed sensory analysis, based on a quantitative descriptive analysis, twice a week for 30 days, evaluating the attributes of appearance (suspended particles and color intensity), odor (natural orange and fermented orange) and flavor (orange characteristic, fermented orange, acid and bitter taste). Storage presented great effect on OJ sensory profile; however, it was not noticeable on physical-chemical characteristics.

Analysis of peptides in prohormone convertase 1/3 null mouse brain using quantitative peptidomics

P>Neuropeptides are produced from larger precursors by limited proteolysis, first by endopeptidases and then by carboxypeptidases. Major endopeptidases required for these cleavages include prohormone convertase (PC) 1/3 and PC2. In this study, quantitative peptidomics analysis was used to characterize the specific role PC1/3 plays in this process. Peptides isolated from hypothalamus, amygdala, and striatum of PC1/3 null mice were compared with those from heterozygous and wild-type mice. Extracts were labeled with stable isotopic tags and fractionated by HPLC, after which relative peptide levels were determined using tandem mass spectrometry. In total, 92 peptides were found, of which 35 were known neuropeptides or related peptides derived from 15 distinct secretory pathway proteins: 7B2, chromogranin A and B, cocaine- and amphetamine-regulated transcript, procholecystokinin, proenkephalin, promelanin concentrating hormone, proneurotensin, propituitary adenylate cyclase-activating peptide, proSAAS, prosomatosatin, provasoactive intestinal peptide, provasopressin, secretogranin III, and VGF. Among the peptides derived from these proteins, similar to 1/3 were decreased in the PC1/3 null mice relative to wild-type mice, similar to 1/3 showed no change, and similar to 1/3 increased in PC1/3 null. Cleavage sites were analyzed in peptides that showed no change or that decreased in PC1/3 mice, and these results were compared with peptides that showed no change or decreased in previous peptidomic studies with PC2 null mice. Analysis of these sites showed that while PC1/3 and PC2 have overlapping substrate preferences, there are particular cleavage site residues that distinguish peptides preferred by each PC.

Peptidomic Analysis of Human Cell Lines

Peptides have been proposed to function in intracellular signaling within the cytosol. Although cytosolic peptides are considered to be highly unstable, a large number of peptides have been detected in mouse brain and other biological samples. In the present study, we evaluated the peptidome of three diverse cell lines: SH-SY5Y, MCF7, and HEIC293 cells. A comparison of the peptidomes revealed considerable overlap in the identity of the peptides found in each cell line. The majority of the observed peptides are not derived from the most abundant or least stable proteins in the cell, and approximately half of the cellular peptides correspond to the N- or C- termini of the precursor proteins. Cleavage site analysis revealed a preference for hydrophobic residues in the PI position. Quantitative peptidomic analysis indicated that the levels of most cellular peptides are not altered in response to elevated intracellular calcium, suggesting that calpain is not responsible for their production. The similarity of the peptidomes of the three cell lines and the lack of correlation with the predicted cellular degradome implies the selective formation or retention of these peptides, consistent with the hypothesis that they are functional in the cells.

PIXE analysis of chromium phytoaccumulation by the aquatic macrophytes Eicchornia crassipes

The uptake of hexavalent chromium in free living floating aquatic macrophytes Eicchornia crassipes cultivated in non-toxic chromium-doped hydroponic solutions is presented. A Cr-uptake bioaccumulation experiment was carried out using healthy macrophytes grown in a temperature controlled greenhouse. Six samples of nutrient media and plants were collected during the 23 day experiment. Roots and leaves were acid digested with the addition of an internal Gallium standard, for thin film sample preparation and quantitative Cr analysis by PIXE method. The Cr(6+) mass uptake by the macrophytes reached up to 70% of the initial concentration, comparable to former results and literature data. The Cr-uptake data were described using a non-structural first order kinetic model. Due to low cost and high removal efficiency, living aquatic macrophytes E. crassipes are a viable biosorbent in an artificial wetland of a water effluent treatment plant. (c) 2009 Elsevier B.V. All rights reserved.

Prediction of Crude Oil Properties and Chemical Composition by Means of Steady-State and Time-Resolved Fluorescence

Steady-state and time-resolved fluorescence measurements are reported for several crude oils and their saturates, aromatics, resins, and asphaltenes (SARA) fractions (saturates, aromatics and resins), isolated from maltene after pentane precipitation of the asphaltenes. There is a clear relationship between the American Petroleum Institute (API) grade of the crude oils and their fluorescence emission intensity and maxima. Dilution of the crude oil samples with cyclohexane results in a significant increase of emission intensity and a blue shift, which is a clear indication of the presence of energy-transfer processes between the emissive chromophores present in the crude oil. Both the fluorescence spectra and the mean fluorescence lifetimes of the three SARA fractions and their mixtures indicate that the aromatics and resins are the major contributors to the emission of crude oils. Total synchronous fluorescence scan (TSFS) spectral maps are preferable to steady-state fluorescence spectra for discriminating between the fractions, making TSFS maps a particularly interesting choice for the development of fluorescence-based methods for the characterization and classification of crude oils. More detailed studies, using a much wider range of excitation and emission wavelengths, are necessary to determine the utility of time-resolved fluorescence (TRF) data for this purpose. Preliminary models constructed using TSFS spectra from 21 crude oil samples show a very good correlation (R(2) > 0.88) between the calculated and measured values of API and the SARA fraction concentrations. The use of models based on a fast fluorescence measurement may thus be an alternative to tedious and time-consuming chemical analysis in refineries.

Evaluation of physico-chemical and phytochemical characteristics of different tinctures of barbatimao (Stryphnodendron barbatiman)

As a consequence of the large distribution and use of medicinal plants, the industries are producing products based on plant species in various pharmaceutical forms, which have been commercialized in pharmacies and natural products homes. However, there is no guarantee for the vast majority of these products, as to their effctiveness, safety, and quality, which may cause risks to the health of consumers. There it is important the establishment of standardized protocols of quality control for phytotherapeutic products. Tinctures of barbatimao are available in the Brazilian market proceeding from diverse manufacturers. With the purpose to evaluate the difference between the quality of tinctures of barbatimao proceeding from four manufactures, a comparative study of ph ysico-chenfical andphylocheinical characteristics was carried out. For physico-chemical analysis, the pH, density, dry residue and tannins content were evaluated. The phytochemical analysis was made using thin layer chromatography. The differences observed in physico-chemical and phytochemical characteristics had evidenced the lack of standardization in the production of these tinctures.

A simple analysis of the changes during evaporation of a commercial emulsion of unknown composition

Optical microscopy and centrifugation were used to observe the Structural changes during evaporation of a commercial skin lotion of unknown composition. The degree of evaporation was determined from the changed weight of a microscope slide with the emulsion on a defined area and thickness, the evaporation loss versus time being measured by a balance under an infrared lamp. The results revealed not only which parts of the emulsion were most prone to evaporation without chemical analysis, but also gave surprising information as to which kind of structures would appear after extensive evaporation. The importance of these changes for the action of a skin lotion is briefly discussed.

ANALYSIS OF PRESSURE FLUCTUATIONS DURING WATER EVAPORATION IN SPOUTED BED

The aim of this work was to study the behaviour of conventional spouted beds during water evaporation and to analyze the pressure fluctuations at the maximum water evaporative capacity for different bed heights and air flow rates. The results showed that spout pressure drop could not indicate the proximity of maximum evaporative capacity; however this condition is denoted by a minimum in fountain height. The standard deviation and amplitude of the pressure fluctuations also showed a minimum point at the maximum water evaporation capacity. The frequency domain analysis of pressure fluctuations revealed that the dry bed has a dominant frequency varying from 6 to 8.2 Hz and that the peak of dominant frequency tends to disappear with the increase in water feed rate.