Isolation of a lectin and a galactoxyloglucan from Mucuna sloanei seeds

A lectin and a galactoxyloglucan were characterized from Mucuna sloanei seed cotyledons. The galactoxyloglucan, isolated by water extraction and ethanol precipitation, had Glc:Xyl:Gal proportions in a molar ratio of 1.8:1.7:1.0 and a molar mass (M(w)) of 1.6 x 10(6) g mol(-1). The lectin (sloanin), isolated from the same seed by affinity chromatography on cross-linked Adenanthera pavonina galactomannan, gave two protein bands by SDS-PAGE (36 and 34 kDa) and one peak by gel filtration (63.6 kDa). Its N-terminal sequence indicated similar to 69% identity with soybean agglutinin to leguminous lectins. Circular dichroism (CD) spectra established that sloanin predominantly contains beta-sheet structures. Sloanin has similar to 5.5% carbohydrate and displayed hemagglutinating activity against rabbit and enzyme treated human erythrocytes, inhibited only by D-Gal containing sugars. The interaction between sloanin and storage cell-wall galactoxyloglucan was tested by affinity chromatography and fluorescence spectroscopy. (C) 2009 Elsevier Ltd. All rights reserved.

Catalytic ethanolysis of soybean oil with immobilized lipase from Candida antarctica and (1)H NMR and GC quantification of the ethyl esters (biodiesel) produced

The catalytic ethanolysis of soybean oil with commercial immobilized lipase type B from Candida antarctica to yield ethyl esters (biodiesel) has been investigated. Transesterification was monitored with respect to the following parameters: quantity of biocatalyst, reaction time, amount of water added and turnover of lipase. The highest yields of biodiesel (87% by (1)H NMR; 82.9% by GC) were obtained after a reaction time of 24 h at 32 degrees C in the presence of lipase equivalent to 5.0% (w/w) of the amount of soybean oil present. The production of ethyl esters by enzymatic ethanolysis was not influenced by the addition of water up to 4.0% (v/v) of the alcohol indicating that it is possible to use hydrated ethanol in the production of biodiesel catalyzed by lipase. The immobilized enzyme showed high stability under moderate reaction conditions and retained its activity after five production cycles. The (1)H NMR methodology elaborated for the quantification of biodiesel in unpurified reaction mixtures showed good correlations between the signal areas of peaks associated with the alpha-methylene groups of the ethyl esters and those of the triacyl-glycerides in residual soybean oil. Monoacylglycerides, diacylglycerides and triglycerides could also be detected and quantified in the crude biodiesel using (1)H NMR spectroscopic and GC-FID chromatographic methods. The biodiesel production by enzymatic catalysis was promising. In this case, was produced a low concentration of glycerol (0.74%) and easily removed by water extraction. (C) 2010 Elsevier B.V. All rights reserved.

Deterpenation of Bergamot Essential Oil Using Liquid-Liquid Extraction: Equilibrium Data of Model Systems at 298.2 K

The deterpenation of bergamot essential oil can be performed by liquid liquid extraction using hydrous ethanol as the solvent. A ternary mixture composed of 1-methyl-4-prop-1-en-2-yl-cydohexene (limonene), 3,7-dimethylocta-1,6-dien-3-yl-acetate (linalyl acetate), and 3,7-dimethylocta-1,6-dien-3-ol (linalool), three major compounds commonly found in bergamot oil, was used to simulate this essential oil. Liquid liquid equilibrium data were experimentally determined for systems containing essential oil compounds, ethanol, and water at 298.2 K and are reported in this paper. The experimental data were correlated using the NRTL and UNIQUAC models, and the mean deviations between calculated and experimental data were lower than 0.0062 in all systems, indicating the good descriptive quality of the molecular models. To verify the effect of the water mass fraction in the solvent and the linalool mass fraction in the terpene phase on the distribution coefficients of the essential oil compounds, nonlinear regression analyses were performed, obtaining mathematical models with correlation coefficient values higher than 0.99. The results show that as the water content in the solvent phase increased, the kappa value decreased, regardless of the type of compound studied. Conversely, as the linalool content increased, the distribution coefficients of hydrocarbon terpene and ester also increased. However, the linalool distribution coefficient values were negatively affected when the terpene alcohol content increased in the terpene phase.

Phase equilibria study of systems composed of refined babassu oil, lauric acid, ethanol, and water at 303.2 K

Deacidification of vegetable oils can be performed using liquid-liquid extraction as an alternative method to the classical chemical and physical refining processes. This paper reports experimental data for systems containing refined babassu oil, lauric acid, ethanol, and water at 303.2 K with different water mass fractions in the alcoholic solvent (0, 0.0557, 0.1045, 0.2029, and 0.2972). The dilution of solvent with water reduced the distribution coefficient values, which indicates a reduction in the loss of neutral oil. The experimental data were used to adjust the NRTL equation parameters. The global deviation between the observed and the estimated compositions was 0.0085, indicating that the model can accurately predict the behavior of the compounds at different levels of solvent hydration. (C) 2011 Elsevier Ltd. All rights reserved.

Extracts from pitanga (Eugenia uniflora L.) leaves: Influence of extraction process on antioxidant properties and yield of phenolic compounds

Different extraction processes were employed to extract the polyphenolic compounds from pitanga (Eugenia uniflora L) leaves: a one-step process using water, ethanol or supercritical CO(2) as solvents, and a two-step process using supercritical CO(2) followed by either water or ethanol. The total polyphenolic compounds, total flavonoids and antioxidant activity were determined in all the extracts obtained. The process performance was evaluated with respect to three variables: global extraction yield, concentration and yield of both polyphenols and flavonoids in the extracts. For the one-step extraction, the results showed that the extraction yield increased with solvent polarity. For the two-step process, the results suggested that water was more efficient in extracting the phenolic compounds from E. uniflora when the matrix was previously extracted with scCO(2). With respect to the antioxidant activity, the ethanolic extracts obtained from both processes, using either the DPPH radical scavenging method or the beta-carotene bleaching method, presented high antioxidant activities. (C) 2010 Elsevier B.V. All rights reserved.

Liquid-liquid equilibria for systems composed of refined soybean oil, free fatty acids, ethanol, and water at different temperatures

Soybean oil can be deacidified by liquid-liquid extraction with ethanol. In the present paper, the liquid-liquid equilibria of systems composed of refined soybean oil, commercial linoleic acid, ethanol and water were investigated at 298.2 K. The experimental data set obtained from the present study (at 298.2 K) and the results of Mohsen-Nia et al. [1] (at 303.2 K) and Rodrigues et al. [2] (at 323.2 K) were correlated by applying the non-random two liquid (NRTL) model. The results of the present study indicated that the mutual solubility of the compounds decreased with an increase in the water content of the solvent and a decrease in the temperature of the solution. Among variables, the water content of the solvent had the strongest effect on the solubility of the components. The maximum deviation and average variance between the experimental and calculated compositions were 1.60% and 0.89%, indicating that the model could accurately predict the behavior of the compounds at different temperatures and degrees of hydration. (C) 2010 Elsevier B.V. All rights reserved.

Vegetable Oils Deacidification by Solvent Extraction: Liquid-Liquid Equilibrium Data for Systems Containing Sunflower Seed Oil at 298.2 K

Liquid-liquid equilibrium experimental data for refined sunflower seed oil, artificially acidified with commercial oleic acid or commercial linoleic acid and a solvent (ethanol + water), were determined at 298.2 K. This set of experimental data and the experimental data from Cuevas et al.,(1) which were obtained from (283.2 to 333.2) K, for degummed sunflower seed oil-containing systems were correlated using NRTL and UNIQUAC models with temperature-dependent binary parameters. The deviation between experimental and calculated compositions presented average values of (1.13 and 1.41) % for NRTL and UNIQUAC equations, respectively, indicating that the models were able to correctly describe the behavior of compounds under different temperature and solvent hydration.

Response surface methodology applied to the analysis of rice bran oil extraction process with ethanol

P>Vegetable oils can be extracted using ethanol as solvent. The main goal of this work was to evaluate the ethanol performance on the extraction process of rice bran oil. The influence of process variables, solvent hydration and temperature was evaluated using the response surface methodology, aiming to maximise the soluble substances and gamma-oryzanol transfer and minimise the free fatty acids extraction and the liquid content in the underflow solid. It can be noted that oil solubility in ethanol was highly affected by the water content. The free fatty acids extraction is improved by increasing the moisture content in the solvent. Regarding the gamma-oryzanol, it can be observed that its extraction is affected by temperature when low level of water is added to ethanol. On the other hand, the influence of temperature is minimised with high levels of water in the ethanol.

Extraction of free fatty acids from peanut oil and avocado seed oil: Liquid-liquid equilibrium data at 298.2 K

The present paper reports phase equilibrium experimental data for two systems composed by peanut oil or avocado seed oil + commercial oleic acid + ethanol + water at 298.2 K and different water contents in the solvent. The addition of water to the solvent reduces the loss of neutral oil in the alcoholic phase and improves the solvent selectivity. The experimental data were correlated by the NRTL and UNIQUAC models. The global deviations between calculated and experimental values were 0.63 % and 1.08 %, respectively, for the systems containing avocado seed oil. In the case of systems containing peanut oil those deviations were 0.65 % and 0.98 %, respectively. Such results indicate that both models were able to reproduce correctly the experimental data, although the NRTL model presented a better performance.

Thermodynamic and statistical analysis of soybean oil extraction process using renewable solvent

The main goal of this work was to evaluate thermodynamic parameters of the soybean oil extraction process using ethanol as solvent. The experimental treatments were as follows: aqueous solvents with water contents varying from 0 to 13% (mass basis) and extraction temperature varying from 50 to 100 degrees C. The distribution coefficients of oil at equilibrium have been used to calculate enthalpy, entropy and free energy changes. The results indicate that oil extraction process with ethanol is feasible and spontaneous, mainly under higher temperature. Also, the influence of water level in the solvent and temperature were analysed using the response surface methodology (RSM). It can be noted that the extraction yield was highly affected by both independent variables. A joint analysis of thermodynamic and RSM indicates the optimal level of solvent hydration and temperature to perform the extraction process.

Rapid and direct determination of glyphosate and aminomethylphosphonic acid in water using anion-exchange chromatography with coulometric detection

A simple, rapid, and low-cost coulometric method for direct detection of glyphosate and aminomethylphosphonic acid (AMPA) in water samples using anion-exchange chromatography and coulometric detection with copper electrode is presented. Under optimized conditions, the limits of detection (LODs) (S/N = 3) were 0.038 mu g ml(-1) for glyphosate and 0.24 mu g ml(-1) for AMPA, without any preconcentration method. The calibration curves were linear and presented an excellent correlation coefficient. The method was successfully applied to the determination of glyphosate and AMPA in water samples without any kind of extraction, clean-up, or preconcentration step. No interferent was found in the water, like this, the recovery was, practically, 100%. (c) 2008 Elsevier B.V. All rights reserved.

Pendimethalin determination in natural water, baby food and river sediment samples using electroanalytical methods

This work describes the electroanalytical determination of pendimethalin herbicide levels in natural waters, river sediment and baby food samples, based on the electro-reduction of herbicide on the hanging mercury drop electrode using square wave voltammetry (SWV). A number of experimental and voltammetric conditions were evaluated and the best responses were achieved in Britton-Robinson buffer solutions at pH 8.0, using a frequency of 500 s(-1). a scan increment of 10 mV and a square wave amplitude of 50 mV. Under these conditions, the pendimethalin is reduced in an irreversible process, with two reduction peaks at -0.60 V and -0.71 V. using a Ag/AgCl reference system. Analytical curves were constructed and the detection limit values were calculated to be 7.79 mu g L(-1) and 4.88 mu g L(-1), for peak 1 and peak 2, respectively. The precision and accuracy were determinate as a function of experimental repeatability and reproducibility, which showed standard relative deviation values that were lower than 2% for both voltammetric peaks. The applicability of the proposed methodology was evaluated in natural water, river sediments and baby food samples. The calculated recovery efficiencies demonstrate that the proposed methodology is suitable for determining any contamination by pendimethalin in these samples. Additionally, adsorption isotherms were used to evaluate information about the behavior of pendimethalin in river sediment samples. (C) 2010 Elsevier B.V. All rights reserved.

Development of a new stir bar sorptive extraction coating and its application for the determination of six pesticides in sugarcane juice

In this article, a novel polydimethylsiloxane/activated carbon (PDMS-ACB) material is proposed as a new polymeric phase for stir bar sorptive extraction (SBSE). The PDMS-ACB stir bar, assembled using a simple Teflon (R)/glass capillary mold, demonstrated remarkable stability and resistance to organic solvents for more than 150 extractions. The SBSE bar has a diameter of 2.36 mm and a length of 2.2 cm and is prepared to contain 92 mu L of polymer coating. This new PDMS-ACB bar was evaluated for its ability to determine the quantity of pesticides in sugarcane juice samples by performing liquid desorption (LD) in 200 mu L of ethyl acetate and analyzing the solvent through gas chromatography coupled with mass spectrometry (GC-MS). A fractional factorial design was used to evaluate the main parameters involved in the extraction procedure. Then, a central composite design with a star configuration was used to optimize the significant extraction parameters. The method used demonstrated a limit of quantification (LOQ) of 0.5-40 mu g/L, depending on the analyte detected; the amount of recovery varied from 0.18 to 49.50%, and the intraday precision ranged from 0.072 to 8.40%. The method was used in the analysis of real sugarcane juice samples commercially available in local markets.

Evaluation of the QuEChERS Method and Gas Chromatography-Mass Spectrometry for the Analysis Pesticide Residues in Water and Sediment

A method for the determination of pesticide residues in water and sediment was developed using the QuEChERS method followed by gas chromatography - mass spectrometry. The method was validated in terms of accuracy, specificity, linearity, detection and quantification limits. The recovery percentages obtained for the pesticides in water at different concentrations ranged from 63 to 116%, with relative standard deviations below 12%. The corresponding results from the sediment ranged from 48 to 115% with relative standard deviations below 16%. The limits of detection for the pesticides in water and sediment were below 0.003 mg L(-1) and 0.02 mg kg(-1), respectively.