Method Development for Purification of γ-oryzanol from Hydrolyzed Rice Bran Acid Oil by Semi-preparative Chromatography.

The objective of this study was to develop a method for isolation and purification of γ-oryzanol from hydrolyzed rice bran acid oil (RBAO) using semi-preparative chromatography by first applying silica coated-thin layer chromatography (TLC) to determine the suitable mobile phase. Subsequently, column chromatography was carried out to determine the effects of purification conditions such as the amount of and particle sizes of the sample silica gel, and elution modes, on the percentage of γ-oryzanol yield and recovery. The results from the TLC suggested that 75:25 (v/v) hexane to ethyl acetate mixture was a suitable mobile phase. The semi-chromatographic results indicated that the column containing 10 g of 25-40 µm silica gel with isocratic elution gave the highest yield (84%) of purified γ-oryzanol (> 95% purity). Further application of a step-gradient elution with 85:15 (v/v), followed by 75:25 (v/v) hexane to ethyl acetate mixture increased chromatographic resolution (Rs), resulting in enhanced separation efficiency, which in turn led to a higher yield of purified γ-oryzanol of 90%.

Release Mechanisms and Kinetic Models of Gypsum-Sulfur-Zeolite-Coated Urea Sealed with Microcrystalline Wax for Regulated Dissolution.

In this study, a mineral-based coated urea was fabricated in a rotary pan coater using a mixture of gypsum/sulfur/zeolite (G25S25Z50) as an effective and low-cost coating material. The effects of different coating compositions on the dissolution rate of urea and the crushing strength and morphology of the coated urea were investigated. A 25:25:50 (wt %) mixture of gypsum/sulfur/zeolite (G25S25Z50) increased the coating effectiveness to 34.1% with the highest crushing strength (31.06 N). The effectiveness of coated urea was further improved to 46.6% with the addition of a microcrystalline wax (3%) as a sealant. Furthermore, the release mechanisms of various urea fertilizers were determined by fitting the release profiles with six mathematical models, namely, the zeroth-order, first-order, second-order, Higuchi, Ritger & Peppas, and Kopcha models. The results showed that the release mechanism of the uncoated urea and all other coated urea followed the Ritger & Peppas model, suggesting the diffusional release from nonswellable delivery systems. In addition, due to the increased mass-transfer resistance, the kinetic constant was decreased from 0.2233 for uncoated urea to 0.1338 for G25S25Z50-coated urea and was further decreased to 0.0985 when 3% Witcovar 146 sealant was applied.

Synergizing Sulfonated Hydrothermal Carbon and Microwave Irradiation for Intensified Esterification Reaction.

The synergy of sulfonated hydrothermal carbon and microwave (MW) irradiation was applied for the esterification of oleic acid with methanol (MeOH) to produce biodiesel. The effects of temperature, reaction time, ratio of oleic acid to methanol, and catalyst loading were investigated at a fixed MW power of 400 W. The addition of hexane, serving as a co-solvent and separator, was also investigated. The optimum conditions for the proposed process were oleic acid-to-methanol molar ratio of 1:5 and hexane-to-methanol ratio of 0.5 (v/v) in the presence of a 5 wt % catalyst, at 100 °C for 60 min, obtaining a 97% yield of oleic acid methyl ester. The addition of slight amounts of hexane resulted into an eightfold reduction in the amount of MeOH needed to obtain a yield above 90%, which normally required a MeOH-to-oil ratio of 40:1. This proposed novel approach could provide a more cost-effective method for the esterification of oil to produce biodiesel, that is, reactive separation utilizing carbon-based catalysts under MW irradiation.

Hydrothermal production and characterization of protein and amino acids from silk waste.

Non-catalytic hydrothermal decomposition of sericin and fibroin from silk waste into useful protein and amino acids was examined in a closed batch reactor at various temperatures, reaction times, and silk to water ratios to examine their effects on protein and amino acid yields. For the decomposition of sericin, the highest protein yield was found to be 0.466 mg protein/mg raw silk, obtained after 10 min hydrothermal reaction of silk waste at 1:100 silk to water ratio at 120 degrees C. The highest amino acid yield was found to be 0.203 mg amino acids/mg raw silk, obtained after 60 min of hydrothermal reaction of silk waste at 1:20 silk to water ratio at 160 degrees C. For the hydrothermal decomposition of fibroin, the highest protein yield was 0.455 mg protein/mg silk fibroin (1:100, 220 degrees C, 10 min) and that of amino acids was 0.755 mg amino acids/mg silk fibroin (1:50, 220 degrees C, 60 min). The rate of silk fibroin decomposition could be described by surface reaction kinetics. The soluble reaction products were freeze-dried to obtain sericin and fibroin particles, whose conformation and crystal structure of the particles were shown to differ from the original silk materials, particularly in the case of fibroin, in which the change from beta-sheet conformation to alpha-helix/random coil was observed.

Supercritical carbon dioxide extraction of astaxanthin from Haematococcus pluvialis with vegetable oils as co-solvent.

Soybean oil and olive oil were investigated as continuous co-solvents for supercritical carbon dioxide (SC-CO(2)) extraction of astaxanthin from Haematococcus pluvialis. Without co-solvents, only 25.40+/-0.79% efficiency was achieved with SC-CO(2) extraction at 70 degrees C and 40 MPa at a continuous flow rate of 3 mL min(-1) for 5h. In the presence of soybean oil or olive oil as a co-solvent, the extraction efficiency was enhanced, with the most appropriate level of soybean oil in the solvent mixture being 10% by volume. At this concentration and the above extraction conditions, the highest extraction efficiency of 36.36+/-0.79% was obtained for soybean oil, a 30% increase in extraction efficiency compared with SC-CO(2) extraction without soybean oil, whereas the 10% olive oil increased the extraction efficiency further to 51.03+/-1.08%, which was comparable to that obtained using ethanol as co-solvent.

Value-added subcritical water hydrolysate from rice bran and soybean meal.

New value-added product was derived from agricultural by-products: rice bran and soybean meal by means of subcritical water (SW) hydrolysis. The effect of temperature (200-220 degrees C), reaction time (10-30 min), raw material-to-water weight ratio (1:5 and 2:5), was determined on the yields of protein, total amino acids, and reducing sugars in the soluble products. The suitable hydrolysis time was 30 min and the proper weight ratio of the raw material-to-water was 1:5. The reaction temperature suitable for the production of protein and amino acids was 220 degrees C for raw and deoiled rice bran, 210 degrees C for raw soybean meal, and 200 degrees C for deoiled soybean meal. The products were also found to have antioxidant activity as tested by ABTS(.)(+) scavenging assay. In addition, sensory evaluation of milk added with the hydrolysis product of deoiled rice bran indicated the potential use of the product as a nutritious drink.

Response surface methodology to supercritical carbon dioxide extraction of astaxanthin from Haematococcus pluvialis.

Experimental design was used to investigate the effect of operating temperature (40-80 degrees C), operating pressure (30-50 MPa), and extraction time (1-4h) of supercritical carbon dioxide (SC-CO2) extraction on astaxanthin yields and the extract antioxidant activity (IC50). The ranges of the factors investigated were 40-80 degrees C for the operating temperature (X1), 30-50 MPa for the operating pressure (X2), and 1-4h for the extraction time (X3). The statistical analysis of the experiment indicated that pressure, extraction time, and the interaction between temperature and pressure (X1X2) had significant effect on astaxanthin yields. The central composite design showed that polynomial regression models were in good agreement with the experimental results with the coefficients of determination of 0.924 and 0.846 for astaxanthin yield and antioxidant activity, respectively. The optimal condition for astaxanthin yield within the experimental range of the variables studied was at 70 degrees C, 50 MPa, and 4h. At this condition, the predicted amount of astaxanthin extracted was 23.04 mg/g (2.3 wt% or 83.78% recovery). For the effect of experimental extraction conditions on antioxidant activity, IC50 was used as an index, which is the concentration that gives a 50% reduction in the absorbance of the ABTS free radical. The analysis of the results showed that the interaction between the operating temperature and operating pressure (X1X2) was the only significant factor affecting the extract antioxidant activity. The statistical model gave the minimum point for antioxidant activity at 67 degrees C, 40.3 MPa, and 1.86 h of extraction, at which the value for 1/IC50 was 0.39 l/mg (or IC50 was 2.57 mg/l).

Extraction of protein and amino acids from deoiled rice bran by subcritical water hydrolysis.

This study investigated the production of value-added protein and amino acids from deoiled rice bran by hydrolysis in subcritical water (SW) in the temperature range between 100 and 220 degrees C for 0-30 min. The results suggested that SW could effectively be used to hydrolyze deoiled rice bran to produce useful protein and amino acids. The amount of protein and amino acids produced are higher than those obtained by conventional alkali hydrolysis. The yields generally increased with increased temperature and hydrolysis time. However, thermal degradation of the product was observed when hydrolysis was carried out at higher temperature for extended period of time. The highest yield of protein and amino acids were 219 +/- 26 and 8.0 +/- 1.6 mg/g of dry bran, and were obtained at 200 degrees C at hydrolysis time of 30 min. Moreover, the product obtained at 200 degrees C after 30 min of hydrolysis exhibited high antioxidant activity and was shown to be suitable for use as culture medium for yeast growth.

Photoautotrophic high-density cultivation of vegetative cells of Haematococcus pluvialis in airlift bioreactor.

This work aimed to investigate the effects of the bioreactor configurations and their design variables on the cultivation of vegetative cells Haematococcus pluvialis to achieve sustainable high cell density. The addition of vitamin B to F1 growth medium could appreciably enhance the final cell density. Employing this medium, the cultivation in the airlift bioreactor was demonstrated to outperform the bubble column at the same operating conditions. Aeration was crucial for a proper growth of the alga in the airlift bioreactor, but it must be maintained at low level to minimize shear stress. The most appropriate aeration velocity (superficial velocity) was at the lower limit of the pump, i.e. 0.4 cm s(-1) and a smaller riser was shown to have positive influence on the cell growth. A 1% CO(2) supplement to the air supply considerably enhanced the growth rate of H. pluvialis and the most suitable light intensity for the growth was at 20 micromol photon m(-2) s(-1). The semi-continuous culture was successfully implemented with the optimal airlift bioreactor design and under optimal conditions the harvest could be performed every four days with the specific growth rate of 0.31 d(-1).

Ultrasound-assisted extraction of anthraquinones from roots of Morinda citrifolia.

This study investigated the use of ultrasound-assisted extraction (UAE) to improve the extraction efficiency of the classical solvent extraction techniques such as maceration and soxhlet extraction to extract anti-oxidant activity compounds, anthraquinones, from the root of Morinda citrifolia. The effects of different extraction conditions were determined, i.e., temperature of (25, 45, 60 degrees C), ultrasonic power, solvent types, and compositions of ethanol in ethanol-water mixtures. The results show that the yield increases with increasing extraction times and extraction temperatures. The percent recovery of anthraquinones using ultrasound was found to be highly dependent on the type of solvents (acetone > acetonitrile > methanol > ethanol). Furthermore, the use of ethanol-water solution as extraction solvent increased the yield of anthraquinones due to the relative polarity, the swelling effect of plant tissue matrix by water, and increased sound absorption. To achieve the same recovery as that achieved by UAE, soxhlet extraction and maceration required much longer time.

Hydrothermal decomposition of yeast cells for production of proteins and amino acids.

This study examines hydrothermal decomposition of Baker's yeast cells, used as a model for spent Brewer's yeast waste, into protein and amino acids. The reaction was carried out in a closed batch reactor at various temperatures between 100 and 250 degrees C. The reaction products were separated into water-soluble and solid residue. The results demonstrated that the amount of yeast residue decreased with increasing hydrolysis temperature. After 20 min reaction in water at 250 degrees C, 78% of yeast was decomposed. The highest amount of protein produced was also obtained at this condition and was found to be 0.16 mg/mg dry yeast. The highest amount of amino acids (0.063 mg/mg dry yeast) was found at the lowest temperature tested after 15 min. The hydrolysis product obtained at 200 degrees C was tested as a nutrient source for yeast growth. The growth of yeast cells in the culture medium containing 2 w/v% of this product was comparable to that of the cells grown in the medium containing commercial yeast extract at the same concentration. These results demonstrated the feasibility of using subcritical water to potentially decompose proteinaceous waste such as spent Brewer's yeast while recovering more useful products.

Application of rotary microfiltration in debittering process of spent brewer's yeast.

This study concerns the production of yeast extract from spent brewer's yeast using rotary microfiltration as a means to combine debittering and cell debris separation into a single step, without using a toxic alkali wash. The pH of yeast homogenate was found to affect protein yield and bitterness of the product. Rotary filtration of yeast homogenate at various pHs resulted in different percent protein transmissions. These were found to be 5.05%, 9.83%, and 30.83% for pH 5, 6, and 7.5, respectively. The bitterness concentration in the permeate was also found to be higher at higher pHs. Autolysis of the cell homogenate prior to filtration increased protein yield and decreased bitterness considerably. At pH 5.5, the protein transmission was increased to 60% and debittering efficiency was increased from 59% to 86%. The permeate flux and protein productivity could be further increased by increasing the rotational speed, but this resulted in a decrease in debittering efficiency. Thus, the rotational speed should be carefully selected to compromise between the yield and product quality. Furthermore, for the tested rotational speeds of 600 and 1000 rpm, the change in feed flow rate from 11 to 35 L h(-1) changes the flow behavior from turbulent vortex flow to laminar vortex flow, thus decreasing the flux and protein productivity.

Pressurized hot water extraction of anthraquinones from the roots of Morinda citrifolia.

This study examines pressurized hot water extraction of anthraquinones from dried roots of Morinda citrifolia (Noni). The effects of various operating conditions such as water temperature (110, 170, and 220 degrees C), and water flow rate (2, 4, and 6 mL min(-1)) on extraction yield and extraction rate were determined. At 220 degrees C, the extraction yield was the highest and was approximately 43.6 mg g(-1). Subcritical water extraction at 4 mL min(-1) or higher was found to be able to recover all the antraquinones present in the roots within 3 h of extraction, even at 170 degrees C. Pressure had no significant effect on the results for the range of temperatures studied. The flow rate of 6 mL min(-1) resulted in the highest extraction rate, but the extraction efficiency, as measured by the amount of anthraquinones extracted per unit volume of water was lower than that of 4 mL min(-1). Anthraquinones solubility in pressurized hot water was determined. The results indicate a presence of a mass transfer limitation in the extraction process from solid matrix.

Microwave pretreatment of defatted rice bran for enhanced recovery of total phenolic compounds extracted by subcritical water.

Enhanced recovery of total phenolics (TP) from defatted rice bran (DRB) subjected to prior microwave pretreatment was achieved by subcritical water extraction (SWE). The effects of microwave pretreatment temperature (60-100°C) and duration (0-30 min) were determined at raw material:water ratios (1:2 and 1:5) for SWE under fixed conditions. Optimal extraction was observed at 80°C (for 10 min, at a ratio of 1:2). With pretreatment carried out under these conditions, a shorter extraction time of 10 min was required for SWE at 200°C. Combining both optimized conditions, a TP yield of 190.4±3.3 mg/g of DRB was achieved, some 55% more than was found to be extractable from un-pretreated samples. The antioxidant activity of the extract was also greater, as indicated by a corresponding decrease in IC(50) from 38.8±0.4 to 27.7±0.5 µg/ml.