José Vladimir de Oliveira

Optimization of Enzymatic Production of Biodiesel from Castor Oil in Organic Solvent Medium

We studied the production of fatty acid ethyl esters from castor oil using n-hexane as solvent and two commercial lipases, Novozym 435 and Lipozyme IM, as catalysts. For this purpose, a Taguchi experimental design was adopted considering the following variables: temperature (35–65°C), water (0–10 wt/wt%), and enzyme (5–20 wt/wt%) concentrations and oil-to-ethanol molar ratio (1∶3 to 1∶10). An empirical model was then built so as to assess the main and cross-variable effects on the reaction conversion and also to maximize biodiesel production for each enzyme. For the system containing Novozym 435 as tatalyst the maximum conversion obtained was 81.4% at 65°C, enzyme concentration of 20 wt/wt%, water concentration of 0 wt/wt%, and oil-to-ethanol molar ratio of 1∶10. When the catalyst was Lipozyme IM, a conversion as high as 98% was obtained at 65°C, enzyme concentration of 20 wt/wt%, water concentration of 0 wt/wt%, and oil-to-ethanol molar ratio of 1∶3.

Extraction of Grape Seed Oil Using Compressed Carbon Dioxide and Propane: Extraction Yields and Characterization of Free Glycerol Compounds

The main objective of this work was to compare the extraction of grape seed oil with compressed carbon dioxide and propane on the extraction yields and chemical characteristics of free glycerol compounds. The experiments were performed in a laboratory scale unit in the temperature range of 30 to 60 degrees C and pressures from 60 to 254 bar. The results showed that propane is a more suitable solvent for grape seed oil extraction than carbon dioxide, as higher extractions yields and a very fast kinetic of extraction were achieved with this solvent. In relation to compressed carbon dioxide extractions, both temperature and density presented a very pronounced and positive effect on the extraction yield. The oils extracted were analyzed qualitatively and quantitatively with regard to the free glycerol compounds, mainly fatty acids, ethyl, and methyl esters. The results showed that these compounds are present in low concentration in vegetable oil (<3%) and that, in general, samples extracted with propane present a smaller amount of peaks of free glycerol compounds in the oil than samples extracted with carbon dioxide.

EVALUATION OF ORIGANUM VULGARE ESSENTIAL OIL AS ANTIMICROBIAL AGENT IN SAUSAGE

This work reports antimicrobial activity of oregano (Origanum vulgare) essential oil against several bacteria in sausage. The in vitro minimum inhibitory concentration (MIC) was determined for 9 selected aerobic heterotrofic bacteria. The antimicrobial activity of distinct concentrations of the essential oil on the basis of the highest MIC found was tested in a food system comprised of fresh sausage. Batch food samples were also inoculated with Escherichia coli with a fixed concentration and the time course of the product was evaluated with respect to the action of the different concentrations of essential oil. Sensory analysis were conducted, and results showed that the addition of oregano essential oil to sausage may be a promising route as bacteriostatic effect was verified for oil concentrations lower than the MIC.

Optimization of alkaline transesterification of soybean oil and castor oil for biodiesel production

This article reports experimental data on the production of fatty acid ethyl esters from refined and degummed soybean oil and castor oil using NaOH as catalyst. The variables investigated were temperature (30–70°C), reaction time (1–3 h), catalyst concentration (0.5–1.5 w/wt%), and oil-to-ethanol molar ratio (1:3–1:9). The effects of process variables on the reaction conversion as well as the optimum experimental conditions are presented. The results show that conversions >95% were achieved for all systems investigated. In general, an increase in reaction temperature, reaction time, and in oil-to-ethanol molar ratio led to an enhancement in reaction conversion, whereas an opposite trend was verified with respect to catalyst concentration.

Chemical characterization and antimicrobial activity of essential oils of salvia L. species

In this work, the essential oils of S. officinalis, S. sclarea, S. lavandulifolia and S. triloba were chemically analyzed by gas chromatography coupled to a mass spectrometry detector (GC/MSD), and their antimicrobial activity was tested against 10 microorganisms using the disk diffusion method and the Minimum Inhibitory Concentration (MIC) technique. The following major compounds were identified in the essential oils: α - and β-thujone, camphor and 1,8-cineole, except in S. sclarea, where linalool, linalyl acetate and α-terpineol were the major constituents. The antimicrobial activity showed significant differences (p < 0.05) only when obtained by the MIC method. Gram-positive microorganisms presented larger sensitivity for the essential oils. The lowest MIC was observed when Staphylococcus aureus was exposed to 2.31 mg.mL-1 of S. lavandulifolia essential oil, while the highest MIC value was obtained when Shigella flexneri was exposed to 9.25 mg.mL-1 of the same essential oil, thus demonstrating that this essential oil may be effective as a bacteriostatic agent against Gram-positive microorganisms.

Determinação experimental da viscosidade e condutividade térmica de óleos vegetais

This work reports experimental data of thermal conductivity and dynamic viscosity of the following refined vegetable oils: rice, soybean, corn oil, sunflower, cottonseed, and olive oil. Measurements of thermal properties were carried out in a cell coupled to a thermostatic bath in the temperature range of 20-70 °C, using a single-needle stainless steel sensor. It was experimentally observed that the thermal conductivity decreased slightly with increasing temperature for all samples investigated. The gravimetric method was employed for density data acquisition, and revealed no significant difference among the values obtained. The Brookfield apparatus was employed in measuring the dynamic viscosity and it was verified that a raise in temperature led to a sharp decrease for this property for all samples investigated.

Kinetics of Enzyme-Catalyzed Alcoholysis of Soybean Oil in n-Hexane

This work investigated the production of fatty acid ethyl esters (FAEEs) from soybean oil using n-hexane as solvent and two commercial lipases as catalysts, Novozym 435 and Lipozyme IM. A Taguchi experimental design was adopted considering the variables temperature (35-65 degrees C), addition of water (0-10 wt/wt%), enzyme (5-20 wt/wt%) concentration, and oil-to-ethanol molar ratio (1:3-1:10). It is shown that complete conversion in FAEE is achieved for some experimental conditions. The effects of process variables on reaction conversion and kinetics of the enzymatic reactions are presented for all experimental conditions investigated in the factorial design.

Pressurized liquid extraction of mate tea leaves

The objective of this work is to investigate the influence of process parameters on the pressurized liquid extraction (PLE) of Ilex paraguariensis leaves. A factorial 2(6-2) experimental design was employed using responses as the extraction yield and the chromatographic profile of the extracts. The extraction time, polarity of solvent, amount of sample, numbers of PLE cycles, flushing volume and extraction temperature were selected as independent variables (factors). Results obtained indicated that the solvent polarity was the most significant variable in the study, while the amount of sample and extraction temperature also showed significant effect. The other variables did not present significant influence in the yield of extraction. GC/MS analysis of the extract enabled the identification of saturated hydrocarbons, fatty acids, fatty acid methyl esters, phytosterols and theobromine in the extracts. Quantitative analysis of four compounds presented in the extracts (caffeine, phytol, vitamin E and squalene) was performed by the GC/MS in the SIM mode.

The effect of temperature, pressure, exposure time, and depressurization rate on lipase activity in SCCO2

We investigated the influence of temperature, pressure, exposure time, and decompression rate on lipase activity in high-pressure CO2 medium. A high-pressure, variable-volume view cell was employed in the experiments, varying the temperature from 30 to 70°C in the pressure range of 70–250 bar at various high-pressure exposure times (60–360 min) and adopting several decompression rates (10–200 kg/[m3·min]). The results obtained show that an increase in temperature and density led to an enhancement of enzyme activity losses while the decompression rates had a weak influence on enzyme inactivation.

Identification of organic sulfur compounds in coal bitumen obtained by different extraction techniques using comprehensive two-dimensional gas chromatography coupled to time-of-flight mass spectrometric detection

The determination of organic sulfur compounds (OSC) in coal is of great interest. Technically and operationally these compounds are not easily removed and promote corrosion of equipment. Environmentally, the burning of sulfur compounds leads to the emission of SOx gases, which are major contributors to acid rain. Health-wise, it is well known that these compounds have mutagenic and carcinogenic properties. Bitumen can be extracted from coal by different techniques, and use of gas chromatography coupled to mass spectrometric detection enables identification of compounds present in coal extracts. The OSC from three different bitumens were tentatively identified by use of three different extraction techniques: accelerated solvent extraction (ASE), ultrasonic extraction (UE), and supercritical-fluid extraction (SFE). Results obtained from one-dimensional gas chromatography (1D GC) coupled to quadrupole mass spectrometric detection (GC–qMS) and from two-dimensional gas chromatography with time-of-flight mass spectrometric detection (GCu2009×u2009GC–TOFMS) were compared. By use of 2D GC, a greater number of OSC were found in ASE bitumen than in SFE and UE bitumens. No OSC were identified with 1D GC–qMS, although some benzothiophenes and dibenzothiophenes were detected by use of EIM and SIM modes. GCu2009×u2009GC–TOFMS applied to investigation of OSC in bitumens resulted in analytical improvement, as more OSC classes and compounds were identified (thiols, sulfides, thiophenes, naphthothiophenes, benzothiophenes, and benzonaphthothiophenes). The roof-tile effect was observed for OSC and PAH in all bitumens. Several co-elutions among analytes and with matrix interferents were solved by use of GC×GC.