Production of lubricating base oil from slop wax by different subsequent refining techniques

Different subsequent refining techniques including solvent dewaxing and solvent extraction have been used to produce lubricating base oil from slop wax waste by-product. The solvent dewaxing technique was performed using two different solvent mixtures of methyl ethyl ketone and toluene with and without benzene at different dilution solvent ratios and at different dewaxing temperatures. The solvent extraction technique was carried out using N-methyl-2-pyrrolidone solvent at 90 °C and at constant dilution solvent ratio of 3:1 by weight. The resulting data revealed that the highest yield of lubricating base oil having the lowest pour point (−6 °C) and the highest iso- and cyclo-paraffins to n-paraffins ratio (5.11) is obtained by solvent dewaxing process only. While the lowest yield of lubricating base oil having the highest pour point (−1 °C) and the lowest iso- and cyclo-paraffins to n-paraffins ratio (4.08) is obtained using solvent dewaxing followed by solvent extraction process. These lubricating base oil products, especially the one that having the lowest pour point (−6 °C) matches the principal characteristics of AX 973853 type of premium low viscosity textile machinery oils obtained by Mobile Velocite Oil Company.     

Decolorization of Brilliant Blue G dye mediated by degradation of the microbial consortium of Galactomyces geotrichum and Bacillus sp.

A consortium-GB containing two microorganisms Galactomyces geotrichum MTCC 1360 and Bacillus sp. VUS was able to degrade sulfur-containing dye Brilliant Blue G, optimally at pH 9 and temperature at 50 °C. The ability of consortium-GB to work at higher temperature and pH ranges will help in using this consortium for removal of the dye from textile effluent. Malt extract, peptone and beef extract were found to be the best additional carbon and nitrogen sources. Brilliant Blue G caused enhancement of the riboflavin reductase among the enzyme activities studied. Biodegradation was confirmed by analyzing the product using UV–vis, HPLC, and FTIR. The GC–MS study revealed a pathway of Brilliant Blue G with release of (4-ethoxy-phenyl)-phenyl-amine and 3-ethylaminomethyl-benzenesulfonic acid as final metabolites formed by the consortium-GB. GC–MS analysis indicated the formation of 3-{[ethyl-(3-methyl-cyclohexa-2,5-dienyl)-amino]-methyl}-benzenesulfonic acid as a product by G. geotrichum MTCC 1360 alone and (4-benzylidene-3-methyl-cyclohexa-2,5-dienylidene)-methyl-amine by Bacillus sp. VUS alone. Phytotoxicity revealed nontoxic nature of the metabolites. These results indicate the high potential of the consortium-GB to serve as an excellent biomass for the use in Brilliant Blue G dye removal.     

Characterization of laurel fruit oil from Madeira Island,Portugal

The fixed oil extracted from Laurus spp. fruit from Madeira Island, Portugal, is used in local traditional medicine for a wide variety of health complaints. Physical properties, density and refractive index, as well as the TAG FA composition, sterols, and waxes were determined. The oil was found to have an unusually high content of volatiles (ca. 10%), with trans-ocimene and germacrene D predominating. Oleic (30%) and linoleic (20%) acids were the main unsaturated FA, whereas lauric (18%) and palmitic (up to 22.5%) acids were the main saturated FA in the neutral lipid fraction. The oil had a sterol content on the same order as olive oil, with β-sitosterol (84%) predominating. Two sesquiterpene lactones, dehydrocostuslactone and costunolide, accounted for 5% of the overall composition. Madeira laurel oil is not currently used as an edible oil because of its very strong flavor. Its claimed medicinal properties have not yet been validated, and this is the first report on the characterization of the commercial product.     

Bioleaching of iron from highly contaminated Kaolin clay by Aspergillus niger

Kaolin is a clay mineral that has a wide application in the industry specially, in paper, ceramic, and porcelain manufacturing. One of the most important factors that affects the value of this raw material is its brightness. Unfortunately, with the iron oxides deposit on mineral particles during kaolin formation, much of this clay has become unusable for industries. So, several chemical methods have been applied in mineral processing plants to reduce these contaminants, but finding a more sustainable approach like biological methods have always attracted a great attention. In this work bioleaching of iron from a highly contaminated kaolin sample was carried out using two different strains of Aspergillus niger, and the effects of strain type, pulp density, and time of clay addition on the iron removal were investigated by employing a 2³ full factorial design. Finally, it is concluded that strain type has the most significant effect on the response; also, the highest removal extent was 42.8% that was obtained by using the strain isolated from pistachio shell, and at the pulp density of 20 g/l when the clay was added at the beginning of the experiments.     

The removal of pesticide residues from wool wax by solvent extraction

A range of suitable solvents for the removal of dieldrin and diazinon residues from wool wax by solvent-solvent extraction was evaluated. Extraction of a 10% solution of wool wax in hexane with N,N-dimethylformamide was shown to be the most effective. These solvents were then used to meanure the partition coefficients of 36 organochlorine, organophosphorus, and pyrethroid pesticides that have the potential to be found in wool wax. Repeated batchwise extraction of a raw wool wax, which had been spiked to produce typical pesticide residue levels, yielded a high-quality wax in which all pesticide residues had been reduced to below detectable levels. The treated wool wax was lighter in color with a lower acid number and a lower free alcohol content and had excellent water absorption characteristics. All detergents associated with the recovery of wool wax from an aqueous scour were also removed.     

Isolation of erucic acid from rapeseed oil by lipase-catalyzed hydrolysis

Three lipases were compared for their ability to hydrolyze high erucic acid rapeseed oil, with the objective of concentrating the erucic acid in a single glyceride fraction. Lipase fromPseudomonas cepacia released all fatty acids rapidly and did not result in selective distribution of erucic acid.Geotrichum candidum lipase released C20 and C22 fatty acids extremely slowly, resulting in their accumulation in the di- and triglyceride fractions. Less than 2% of the total erucic acid was found in the free fatty acid (FFA) fraction. Lipase fromCandida rugosa released erucic acid more slowly than C20 and C18 fatty acids at 35°C but only resulted in a limited accumulation of the erucic acid in the di- and triglyceride fractions. However, when hydrolysis catalyzed byC. rugosa lipase was carried out below 20°C, the reaction mixture solidified and was composed solely of FFAs and diglycerides. The diglyceride fraction contained approximately 95% erucic acid while about 20% of the total erucic acid was found in the FFA fraction. It is concluded that hydrolysis at low temperature withC. rugosa lipase results in a higher purity of erucic acid in the glyceride fraction than can be obtained withG. candidum lipase, but with considerable loss of erucic acid to the FFA fraction.     

Comparative analysis of allelopathic effects produced by four forestry species during decomposition process in their soils in Galicia (NW Spain)

The development of toxicity produced by vegetable litter of four forest species (Quercus robur L.,Pinus radiata D.Don.,Eucalyptus globulus Labill, andAcacia melanoxylon R.Br.) was studied during the decomposition process in each of the soils where the species were found. The toxicity of the extracts was measured by the effects produced on germination and growth ofLactuca saliva L. var. Great Lakes seeds. The phenolic composition of the leaves of the four species was also studied using high-performance liquid chromatographic analysis (HPLC). It was verified that toxicity was clearly reflected in the first stages of leaf decomposition inE. globulus andA. melanoxylon, due to phytotoxic compounds liberated by their litter. At the end of half a year of decomposition, inhibition due to the vegetable material was not observed, but the soils associated with these two species appeared to be responsible for the toxic effects. On the other hand, the phenolic profiles are quite different among the four species, and greater complexity in the two toxic species (E. globulus andA. melanoxylon) was observed.     

Removal of pesticides from wool wax by continuous countercurrent dual-solvent extraction

Pesticide residues in raw wool wax were removed to below detectable levels by continuous countercurrent extraction with hexane and N,N-dimethylformamide (DMF) in a pilot-scale mixer-settler contactor. The disengagement of the phases in the settling compartments was promoted by the addition of a small amount of formic acid (3% vol/vol) to the DMF-rich feed. Empirical equations were developed to predict the effect on the pesticide partition coefficients of the wool wax concentration, the presence of small amounts of water, ethanol, and/or isopropanol in the solvents, and the temperature used in the contactor. These empirical equations were included in equations that describe the concentration of the pesticides in the different stages of the contactor and were used to develop a spreadsheet model that accurately predicted the mixer-settler’s performance. The raffinate wool wax produced by this process after conventional neutralization met all BP and USP specifications for pharmaceutical lanolin.     

Supercritical CO2 extraction of Plumula nelumbinis oil: Experiments and modeling

Supercritical CO₂ extraction of Plumula nelumbinis oil was investigated at temperatures of 308–338 K and pressures of 15–45 MPa. The yield of the extracted oil was 0.128 g/g material at optimal conditions, in which gamma-sitosterol, unsaturated fatty acids and gamma-tocopherol had higher relative concentrations as determined by GC–MS. The broken and intact cell (BIC) model, with reduced adjustable parameters, was utilized to simulate the SFE process. The values of average absolute relative deviation (AARD) were in the range 2.34–10.9%, indicating that the improved method had a similar effect to the BIC model when three parameters were adjusted. The parameters obtained during the modeling had clear physical meanings and were used to gain an in-depth understanding of the SFE process theoretically.     

Purification of docosahexaenoic acid from tuna oil by a two-step enzymatic method: Hydrolysis and selective esterification

Purification of docosahexaenoic acid (DHA) was attempted by a two-step enzymatic method that consisted of hydrolysis of tuna oil and selective esterification of the resulting free fatty acids (FFA). When more than 60% of tuna oil was hydrolyzed with Pseudomonas sp. lipase (Lipase-AK), the DHA content in the FFA fraction coincided with its content in the original tuna oil. This lipase showed stronger activity on the DHA ester than on the eicosapentaenoic acid ester and was suitable for preparation of FFA rich in DHA. When a mixture of 2.5 g tuna oil, 2.5 g water, and 500 units (U) of Lipase-AK per 1 g of the reaction mixture was stirred at 40°C for 48 h, 83% of DHA in tuna oil was recovered in the FFA fraction at 79% hydrolysis. These fatty acids were named tuna-FFA-Ps. Selective esterification was then conducted at 30°C for 20 h by stirring a mixture of 4.0 g of tuna-FFA-Ps/lauryl alcohol (1:2, mol/mol), 1.0 g water, and 1,000 U of Rhizopus delemar lipase. As a result, the DHA content in the unesterified FFA fraction could be raised from 24 to 72 wt% in an 83% yield. To elevate the DHA content further, the FFA were extracted from the reaction mixture with n-hexane and esterified again under the same conditions. The DHA content was raised to 91 wt% in 88% yield by the repeated esterification. Because selective esterification of fatty acids with lauryl alcohol proceeded most efficiently in a mixture that contained 20% water, simultaneous reactions during the esterification were analyzed qualitatively. The fatty acid lauryl esters (L-FA) generated by the esterification were not hydrolyzed. In addition, L-FA were acidolyzed with linoleic acid, but not with DHA. These results suggest that lauryl DHA was generated only by esterification.     

Characterization of Antifungal Metabolites Produced by Penicillium Species Isolated from Seeds of Picea glehnii

We screened the microorganisms that are present on the surface of Picea glehnii seeds and produced antifungal compounds against Pythium vexans, a fungus that causes damping-off. Four isolates of Penicillium species that produced patulin, citrinin, palitantin, and arthrographol, respectively, were identified from 149 different microorganisms screened. This study is the first step in an examination of the ecological interaction between host conifers and fungi located on the surface of their seeds.     

Purification of γ-linolenic acid from borage oil by a two-step enzymatic method

γ-Linolenic acid (GLA) was purified from borage oil by a two-step enzymatic method. The first step involved hydrolysis of borage oil (GLA content, 22.2 wt%) with lipase, Pseudomonas sp. enzyme (LIPOSAM). A mixture of 3 g borage oil, 2 g water, and 5000 units (U) LIPOSAM was incubated at 35°C with stirring at 500 rpm. The reaction was 91.5% complete after 24 h. The resulting free fatty acids (FFA) were extracted from the reaction mixture with n-hexane (GLA content, 22.5 wt%; recovery of GLA, 92.7%). The second step involved selective esterification of borage-FFA with lauryl alcohol by using Rhizopus delemar lipase. A mixture containing 4 g borage-FFA/lauryl alcohol (1:2, mol/mol), 1 g water, and 1000 U lipase was incubated at 30°C for 20 h with stirring at 500 rpm. Under these conditions, 74.4% of borage-FFA was esterified, and the GLA content in the FFA fraction was enriched from 22.5 to 70.2 wt% with a recovery of 75.1% of the initial content. To further elevate the GLA content, unesterified fatty acids were extracted, and esterified again in the same manner. By this repeated esterification, GLA was purified to 93.7 wt% with a recovery of 67.5% of its initial content.     

Production and structural features of a water-soluble polysaccharide from a mutant strain of Agrobacterium sp.

We have developed a mutant strain derived from Agrobacterium sp. ATCC 31750, which produces a water-soluble polysaccharide having potential utility to the food, feed, pharmaceutical and cosmetic industries. A high concentration of product (15 g/L) is obtained by 48 h cultivation of the mutant strain under optimized fermentation conditions. The water-soluble polysaccharide obtained from cultures of the mutant strain beta82 has Glc:Man:Gal in approximate molar ratios of 5.8:6.7:1.0. The molecular weight of the polysaccharide was determined to be approximately 1000 kDa by HPSEC analysis. Linkage analysis contained 3-Glcp, 3-Manp, terminal Glcp and terminal Manp, as well as a small proportion of 3- and 3,4-Galp, and 4,6-Manp residues. Based on analyses using FT-IR and ¹³C NMR spectrometers, most glycosidic bonds joining these sugar residues are of the α-type, and acetyl groups are apparently attached to the polymer chain at random.     

Biosorption of Pb(II) ions from aqueous solution by pine bark (Pinus brutia Ten.)

The biosorption potential of pine (Pinus brutia Ten.) bark in a batch system for the removal of Pb(II) ions from aqueous solutions was investigated. The biosorption characteristics of Pb(II) ions on the pine bark was investigated with respect to well-established effective parameters including the effects of solution pH, initial Pb(II) concentration, mass of bark, temperature, and interfering ions present, reusability, and desorption. Initial solution pH and contact time were optimized to 4.0 and 4 h, respectively. The Langmuir and Freundlich equilibrium adsorption models were studied and observed to fit well. The maximum adsorption capacity of the bark for Pb(II) was found to be 76.8 mg g⁻¹ by Langmuir isotherms (mass of bark: 1.0 g L⁻¹). The kinetic data fitted the pseudo-second-order model with correlation coefficient greater than 0.99. The thermodynamic parameters Gibbs free energy (ΔG°), enthalpy (ΔH°), and entropy (ΔS°) changes were also calculated, and the values indicated that the biosorption process was spontaneous. Reutilization of the biosorbent was feasible with a 90.7% desorption efficiency using 0.5 M HCl. It was concluded that pine bark can be used as an effective, low cost, and environmentally friendly biosorbent for the removal of Pb(II) ions from aqueous solution.     

Purification and identification of a novel cutinase from Coprinopsis cinerea by adsorptive bubble separation

A novel extracellular esterase was separated from culture supernatants of the basidiomycete Coprinopsis cinerea by means of foam fractionation. The parameters pH value, gas flow rate, addition of detergents, and the column design were varied to optimise the transport of the active enzyme into the foam phase. On the 70-mL scale, a recovery of activity of 79% with an enrichment factor of 10.5 was obtained at pH 7 and 20 mL air min⁻¹ within 15 min. The enriched enzyme was characterized biochemically by semi-native SDS-PAGE and IEF electrophoresis with activity staining. Peptide sequencing was performed after tryptic digestion by electrospray tandem mass spectrometry. Homology searches revealed significant similarities to cutinases of various ascomycetes and to C. cinerea genome data recently annotated as cutinases.     

Microwave-assisted extraction of chlorogenic acid from flower buds of Lonicera japonica Thunb.

An efficient microwave-assisted extraction (MAE) technique has been developed to recover chlorogenic acid from flower buds of Lonicera japonica Thunb. The yield of chlorogenic acid rapidly reached 6.14% within 5 min under the optimal MAE conditions, i.e. 50% ethanol as extraction solvent, 1:10 (w/v) of the solid/liquid ratio and 60 °C of extraction temperature. The MAE showed obvious advantages in terms of short duration and high efficiency to recover chlorogenic acid from raw plant materials in comparison with conventional heat-reflux extraction. The mechanism of the enhanced extraction by microwave assistance was discussed by observing cell destruction of plant material after MAE treatment by scanning electron microscopy. The results showed that the plant materials were significantly destroyed due to the cell rupture after MAE treatment.     

Effect of some leaf essential oil phenotypes from coastal redwood on growth of its predominant endophytic fungus,Pleuroplaconema sp.

Experiments were performed to assess the effect of four foliar essential oil phenotypes from a coastal redwood (Sequoia sempervirens) population on isolates ofPleuroplaconema sp., its ubiquitous endophytic fungus. Isolates were exposed to essential oils extracted from their trees of origin and from other trees. The hypotheses tested were: (1) redwood leaf essential oils extracted from distinct trees would have a differential effect onPleuroplaconema sp. growth, and (2) growth of isolates from a particular tree would be differentially affected when exposed to essential oil phenotypes different from that of their tree of origin. The essential oil phenotypes were differentially inhibitory, but the pattern of inhibition did not support the second hypothesis.Pleuroplaconema sp. showed low average tolerance to all of the essential oils; two phenotypes reduced growth 70–80% and the other two 50–60% at the dose tested. The overall growth response of individual isolates to all treatments suggests that more than one fungus genotype per tree was represented in the experiment. The variability in tolerance of individual isolates to the essential oils was low for three phenotypes. The low tolerance ofPleuroplaconema sp. to redwood essential oils, in spite of its predominance and specialization in this conifer, is discussed considering: (1) the possible pathogenic ancestry of this fungus, and (2) that essential oil phenotypes may be important in controlling the activity ofPleuroplaconema sp. after it colonizes the leaf.     

Purification of docosahexaenoic acid by selective esterification of fatty acids from tuna oil with Rhizopus delemar lipase

To purify docosahexaenoic acid (DHA), we attempted the selective esterification of fatty acids originating from tuna oil with lipases. Tuna oil was hydrolyzed in NaOH-ethanol solution, and the resulting fatty acid mixture [DHA, 23.2%; named tuna-free fatty acid (FFA)] was used as a starting material. Rhizopus delemar which acted lightly on DHA, was a suitable catalyst for the selective esterification of tuna-FFA, and lauryl alcohol was the best substrate. The reaction proceeded most effectively when a mixture of 2.4 g lauryl alcohol/tuna-FFA (2:1, mol/mol), 0.6 g water, and 600 U Rhizopus lipase was incubated at 30°C for 20 h with stirring at 500 rpm. Under these conditions 72% of tuna-FFA was esterified, and 84% of DHA was recovered in the unesterified fatty acid fraction. The DHA content in the fatty acid fraction rose from 23 to 73% with this reaction. To further elevate the DHA content, the unesterified fatty acids were extracted, and then esterified again under the same conditions. By this repeated esterification, DHA was purified to 89% with a recovery of 71% of its initial content.     

Preparation of liposomes entrapping essential oil from Atractylodes macrocephala Koidz by modified RESS technique

A modified technique of rapid expansion of supercritical solutions (RESS) was applied to incorporate essential oil extracted from Atractylodes macrocephala Koidz into liposomes. In the modified RESS process, both the liposomal materials and the essential oil were dissolved in the mixture of supercritical carbon dioxide (SC-CO₂)/ethanol and then the solution was sprayed into an aqueous medium through a coaxial nozzle to form liposomes suspension. The encapsulation performance of liposomes could be controlled by changing expansion processing conditions such as pressure, temperature of SC-CO₂ and the amount of ethanol. The entrapment efficiency, drug loading and average particle size of liposomes were found to be 82.18%, 5.18% and 173 nm, respectively, under the optimum conditions of at a pressure of 30 MPa, a temperature of 338 K and a ethanol mole fraction in SC-CO₂ [(x(CH₃CH₂OH)] of 15%. The formed liposomes appeared as double-layered colloidal spheres with a uniform and narrow particle size distribution. The physicochemical properties of liposomes including entrapment efficiency, dissolution rate and stability were complied with the provisions of Chinese pharmacopoeia. All these results indicate that the modified RESS technique is an innovative way for self-assembly of liposomes incorporation of multi-components extracted from Chinese traditional medicines in the SC-CO₂.     

Antioxidant and Antimicrobial Activities of Echinacea (Echinacea purpurea L.) Extracts Obtained by Classical and Ultrasound Extraction

Antioxidant and antimicrobial activities of Echinacea purpurea L. (Asteraceae) extracts obtained by classical and ultrasound solvent extraction were compared. The dry aerial part of plant was extracted by 70% ethanol at a solid-to-liquid ratio of 1:10 (m/v) and 25°C. The extract obtained by classical solvent extraction contained 29% larger amounts of phenolic compounds and 20% higher content of flavonoids. 2,2-diphenyl-1-picril hydrazyl radical (DPPH) scavenging reached 93.6% and the values of EC50 were (34.16±0.65) μg·ml⁻¹ and (65.48±1.12) μg·ml⁻¹ for the extracts obtained by the classical and ultrasound extractions, respectively. The extracts, independent of the extraction technique applied, showed a considerable growth inhibition on Candida albicans and Saccharomyces cerevisiae, while no growth inhibition zones were observed for Aspergillus niger. The diameters of inhibition zone observed for all the microorganisms were larger for extracts obtained by classical extraction than those by ultrasound extraction.