Oil extraction from microalga Nannochloropsis sp. with isopropyl alcohol

An efficient process for fractioning microalgae oil and non-lipid biomass was developed. Isopropyl alcohol (IPA) was used to extract oil from Nannochloropsis sp. at 80?°C, leaving the majority of non-lipid biomass in the solid fraction. The effectiveness of extraction with or without a dewatering pretreatment (DW) was compared. Effects of dewatering time and solvent ratio, IPA concentration, IPA refluxing time, and sonication pretreatment on the oil and biomass yields were studied. The dewatering conditions with a high water-to-alcohol ratio (W/A?=?2:1) and mild mixing (1?min gentle shaking) had 14?% less oil loss in the DW fraction than that with a low water-to-alcohol ratio (W/A?=?1:1) and vigorous mixing (30?min and 300?rpm mixing). Sonication resulted in 14–26?% more oil loss in the DW fraction when compared to intact cell treatment. Without dewatering, 85?% of the total oil from intact cells was extracted by a single extraction using 70?% (wt) IPA aqueous solution. The 88 and 95?% IPA treatments extracted similar percentages of oil to that of the 70?% IPA, but used two- and fivefold more solvent. The amount of oil extracted from broken cells increased with increasing IPA concentrations. An effective extraction can be completed in 30?min. On a 100-g (wet matter) scale, the 70?% IPA achieved 92?% oil yield and 93?% non-lipid biomass yield.     

Lipid Estimation of Surfactant-Extracted Microalgae Oil Using Nile Red

Nile red staining has been used as a lipid quantification technique in many microalgae growth and oil accumulation studies. However, its application in lysed microalgae cells is limited. Therefore, this study focused on lysed microalgae cells and utilized the Nile red staining technique to evaluate oil content and extraction. This study aims to provide a rapid and high-throughput alternative method particularly in the microalgae extraction screening process. Potential interferences such as chlorophyll, β-carotene, soluble protein, and phospholipids were evaluated. The hydrophobic Nile red dye was found to quench in water, therefore the fluorometric measurement has to be completed immediately or within 5 min of dye addition. The fluorescence intensity was also found to be Nile red concentration dependent. The optimum Nile red concentration of 656 ppb was used throughout the study. In microalgae samples containing chlorophyll and carotenoids (such as Nannochloropsis sp.), Nile red fluorescence intensity was significantly reduced in comparison to non-chlorophyll microalgae (Schizochytrium limacinum). Soluble proteins from defatted microalgae did not fluoresce significantly relative to lipids, therefore did not interfere with the method to a high degree. Comparing the optimized Nile red staining method with the gravimetric lipid quantification method, a good linear correlation was found in all three materials tested (soybean oil, Nannochloropsis sp., and Schizochytrium limacinum).     

Isopropyl Alcohol Extraction of De‐hulled Yellow Mustard Flour

Vegetable oils are typically extracted with hexane; however, health and environmental concerns over its use have prompted the search for alternative solvents. Mustard oil was extracted with isopropyl alcohol (IPA) to produce an IPA‐oil miscella suitable for industrial applications. Single‐stage extraction resulted in 87.6 % oil yield at a 10:1 (v/w) IPA/flour ratio. Multiple‐stage extraction resulted in higher extraction efficiency with lower IPA use. Four‐stage cross‐current extraction at an IPA/flour ratio of 2:1 (v/w) per stage resulted in 93.7 % oil yield. At 45 °C, a 91.5 % oil yield was achieved with three‐stage extraction using a 2:1 (v/w) IPA/flour ratio. Any changes to the pH of the mixture resulted in reduced oil yield. Water also reduced the extraction efficiency. The azeotropic IPA solution containing 13 % water extracted ~40 % less oil than did dry IPA in both single and multiple‐stage extractions. Some polar compounds were also extracted, including sugars; however, protein extraction was negligible. The protein left in the extracted meal was not degraded or lost during the extraction. The results suggest that IPA is an excellent solvent for mustard oil, but water content exceeding 5 % in the solvent adversely affects the oil extraction and reuse of the IPA.     

Production of Isopropyl and Methyl Esters from Yellow Mustard Oil/IPA Miscellas

Using an isopropyl alcohol (IPA):flour [volume:weight (ml:g)] ratio of 1.5:1 per stage of extraction resulted in an oil yield of 86.3%. The combined miscella (IPA + oil), which contained 90.6 wt% IPA, 9.8 wt% oil, and 2.1 wt% water, was used as a feedstock for biodiesel production by transesterification. Transesterification of the IPA/oil miscella dehydrated using adsorption on 4Å molecular sieves with 1.2 wt% (based on oil) potassium hydroxide for 2 h at 72 °C converted only 29% of the feed to esters. The addition of methanol (MeOH) resulted in an ester yield of 87%, consisting of 79% methyl ester and 7% isopropyl ester when starting with an IPA:oil:MeOH molar ratio of 146:1:30. By increasing the KOH catalyst to 3 wt%, the ester yield increased to 94%. To increase the ester yield, the miscella was pretreated with sulfuric acid. This resulted in a reduction of the IPA content, the removal of other impurities such as phospholipids, and reduction of the water mass fraction to less than 1%. When IPA was used as a cosolvent with methanol in the transesterification process, a very high ester conversion (>99%) was achieved. The biodiesel produced was compliant with ASTM standards, showing that IPA can be used as a solvent for oil extraction from yellow mustard flour.     

Destabilization of Yellow Mustard Emulsion Using Organic Solvents

An aqueous extraction process was developed consisting of aqueous contact with dehulled yellow mustard flour to recover protein followed by dissolution of the released emulsion in dimethylformamide (DMF) or isopropyl alcohol (IPA) to recover the released oil in the form of single-phase oil–solvent miscellae suitable for industrial applications. Only some 38 ± 3 % of the oil in the yellow mustard emulsion was extracted using DMF even at high weight ratios since DMF is widely miscible with water, preventing separation of the oil from the emulsion. A ternary phase diagram of DMF/oil/water was prepared and confirmed the limited solubility of the oil in DMF in the presence of water. The use of 31:1 IPA:oil weight ratio could effectively recover over 94 % of the oil in the emulsion; however, multiple-stage treatment of the emulsion was proven to be more efficient with lower volumes of IPA required to achieve high oil extraction yields. The results suggest that the optimal conditions for multiple-stage process were four stages using 2:1 IPA:oil weight ratio, with 96 ± 1 % oil recovery from the emulsion.     

Separating Oil from Aqueous Extraction Fractions of Soybean

Previous research has shown that enzyme-assisted aqueous extraction processing (EAEP) extracts 88–90% of the total soybean oil from extruded full-fat soy flakes into the aqueous media, which is distributed as cream (oil-in-water emulsion), skim, and free oil. In the present work, a simple separatory funnel procedure was effective in separating aqueous skim, cream and free oil fractions allowing mass balances and extraction and recovery efficiencies to be determined. The procedure was used to separate and compare liquid fractions extracted from full-fat soy flour and extruded full-fat soy flakes. EAEP extracted more oil from the extruded full-fat soy flakes, and yielded more free oil from the resulting cream compared to unextruded full-fat soy flour. Dry matter partitioning between fractions was similar for the two procedures. Mean oil droplet sizes in the cream and skim fractions were larger for EAEP of extruded flakes compared to non-enzymatic AEP of unextruded flour (45 vs. 20 μm for cream; 13 vs. 5 μm for skim) making the emulsions from EAEP of extruded flakes less stable. All major soy protein subunits were present in the cream fractions, as well as other fractions, from both processes. The cream could be broken using phospholipase treatments and 70–80% of total oil in the extruded full-fat flakes was recovered using EAEP and a phospholipase de-emulsification procedure.     

Recovery and Recycling of Isopropyl Alcohol Used in Biodiesel Production From Yellow Mustard Oil

The recovery of solvents used during biodiesel synthesis is an important factor in the economic feasibility and sustainability of the entire process. In this study, we looked at the use of isopropyl alcohol (IPA) for oil extraction and biodiesel production, as well as its potential for recovery and recycling. We found that multistage extraction improved oil recovery, with up to 86% oil yield using four stages of extraction at an IPA:mustard flour (volume:weight) ratio of 1.5:1 at room temperature. Using acid–base‐catalyzed transesterification, 99% of the mustard oil was converted to biodiesel. At the end of this process, IPA was recovered from the azeotrope by salting out using potassium carbonate or sodium carbonate. The solubility behavior of the components was evaluated by means of ternary‐phase diagrams of IPA/water/sodium carbonate and IPA/water/potassium carbonate, which determined their liquid–liquid–solid equilibrium constants at ambient pressure and at room temperature. Using 20% (w:w) potassium carbonate, 95% of the IPA was recovered at 99% purity from a starting mixture of IPA containing 13% water. Azeotropic distillation of the IPA–water azeotrope with 10% potassium carbonate resulted in the recovery of 99% of the IPA at 94% purity. These results suggest that IPA is not only a suitable solvent for mustard‐oil extraction but also for salt‐enhanced azeotropic distillation resulting in near‐complete recovery from aqueous solutions.     

Rapid equilibrium extraction of rice bran oil at ambient temperature

Rapid equilibrium extraction of soybean flour has been effective in obtaining an oil with reduced phospholipid content. This technique was examined to obtain a low phospholipid and low free fatty acid rice bran oil (RBO). The amount of RBO extracted with hexane from 1 g of rice bran at 22°C was measured over a 10-min period. The amount of oil extracted from variable amounts of bran with a fixed volume of solvent was also studied. Ninety percent of the oil was extracted in one minute, with 93% of the total RBO being extracted after ten minutes. This compares with the 98% yield obtained from soy flour, but increasing the amount of bran used did not reduce the extraction rate. This extraction method produced a good quality RBO with low phospholipid, low free fatty acid and low peroxide values.     

Response Surface Methodology to Supercritical Carbon Dioxide Extraction of Essential Oil from Amormum krevanh Pierre

Abstract

Response surface methodology was employed to investigate the effects of operating conditions and predict the optimal conditions for supercritical carbon dioxide extraction of essential oil from Amomum krevanh Pierre. The factors investigated were operating temperature (33–67°C), the operating pressure (91–259 bar), and the extraction time (20–70 min). The main effect of the operating pressure and the interaction effect between the operating temperature and the extraction time were found to be significant factors. From the response surface model, an optimal condition for essential oil content within the range of experimental study was found to be at 33°C, 175 bar, and 70 min, which gave the oil yield of 17.3 mg/g dry wt. The essential oil yield obtained at all conditions were higher than that obtained by organic solvent extraction (9.74 mg/g dry wt.) while the composition of the extract was similar, which were 1,8-cineole (70.87%), β-pinene (8.89%), and limonene (4.81%).     

Cooking and Sun Drying Effects on Properties of Allanblackia stanerana Kernels’ Oil

Previous studies have evaluated the nutritive potential of Allanblackia oils. Oil extraction from Allanblackia is done after a pretreatment of the kernels which has an influence on oil quality. In Cameroon, the pretreatment consists of cooking, followed by drying of the almonds in the sun. The oil is either edible or used as a body cream. Because of these important applications, it is necessary to determine treatment conditions that maximize extraction yields and preserve its quality. This study was aimed at finding the mathematical models that simulate the best pre-treatment conditions. The use of multiple linear regression analysis allowed developing satisfactory models and surface response plots that predict the evolution of the extraction rate as well as the quality of the extracted oil, depending on cooking and sun drying times. The coefficients of correlation obtained were 72.03 % for water content; 53.06 % for extraction yield; 71.06 % for acid; 76.48 and 83.29 % for iodine and refractive values respectively, indicating a suitable model of the experiment according to the studied variables. The response surface curves were superimposed to obtain a single optimal range that satisfies all response factors. The average cooking time of 12.5 min and the mean residence time of 8.5 days drying gave the following optimal values for the different response factors studied: moisture content 21.60 %; oil yield 70.69 %; refractive index 1.4546; iodine value 34.72; and acid value 0.38 mg KOH/g oil. The conditions to obtain a maximum extraction yield and low acidity were those that gave a residual water content of about 10–15 %. The quality indicators measured in this work generally remained within the threshold.     

Effect of moisture and temperature on the phosphorus content of crude soybean oil extracted from fine flour

Analysis of total oil content in soybeans is usually done by extracting flours, whereas commercial extraction for recovery of oil is done by extracting flakes. It has recently become apparent that phosphorus content of crude soybean oil extracted from flours can vary depending on extraction temperature and flour moisture. In this study, flour moistures below 6% yielded crude oil with low phosphorus (15 ppm), but phosphorus in the oil increased rapidly to 260 ppm at 9% moisture. When temperature of the extraction was increased from 25 to 60°C, the phosphorus in extracted oil also increased for moisture contents of 6.6% and 8.3%, but not for moisture contents of 5% and 3%. In addition to the effects of extraction temperature, it was found that preheating whole soybeans at various temperatures affected phosphorus in oil from extracted flour. Preheating at 130°C caused high phosphorus content regardless of how dry the flour was, whereas preheating at 100°C or below caused phosphorus content that increased with increased moisture. The response of phosphorus content in crude oil to temperature and moisture may be useful in improving the quality of commercially extracted soy oil.     

Effect of UV Processing Treatments on Soy Oil Conjugated Linoleic Acid Yields and Tocopherols Stability

Photoirradiation has been used to synthesize 20 % conjugated linoleic acid (CLA) in soy oil with an iodine catalyst. CLA yields are affected by ultraviolet (UV) irradiation time, Magnesol^® adsorbent treatment, iodine concentration and mixed tocopherols. However, these factors in combination had not been studied. Therefore, the objectives of this study were to determine the effect of (1) a combination of photoirradiation time, Magnesol^® adsorbent treatment and added mixed soy tocopherols on CLA yields and the oxidative stability of CLA-rich soy oil, (2) UV light on mixed tocopherol stability, as tocopherols enhance CLA yields during photoirradiation. Soy oil was initially treated with 5 % Magnesol^®. Iodine at 0 and 0.35 % was mixed with Magnesol^®-treated soy oil and irradiated for 12 and 6 h. The irradiated oil was again treated with Magnesol^®, mixed with 0, 0.35 or 0.175 % iodine; 1400 MT and irradiated for 12 or 6 more hours. CLA content in soy oil was determined by conventional gas chromatography-flame ionization detector. The oxidative stability of the oil was determined by measuring peroxide value (PV). The tocopherols stability was determined by high performance liquid chromatography. The results showed that increasing photoirradiation time increased CLA yields and lowered PV. Magnesol^® adsorption produced highest CLA yield for all treatments by removing peroxides in RBD soy oil. The γ-tocopherols exhibited highest stability during UV irradiation. The order of tocopherol degradation was α-tocopherol > δ-tocopherol > γ-tocopherols.     

Application of a Ternary Phase Diagram to the Phase Separation of Oil-in-Water Emulsions Using Isopropyl Alcohol

The oil-in-water emulsion formed during an aqueous extraction of yellow mustard seed flour was destabilized using isopropyl alcohol (IPA) in a four stage extraction process, with concurrent recovery of oil and water in separate phases. The emulsion was extracted using two different approaches: phase separation extraction (PSE) that used fresh IPA as the extraction solvent at each stage, and phase separation extraction with recycle (PSER) that reused the extracted water-rich phase, containing IPA, as the extraction solvent. Extraction processes by both approaches were modeled by the ternary liquid phase diagram of IPA, canola oil and water to characterize the extraction progress. PSER resulted in improved oil–water separation and IPA usage efficiency than PSE, but achieved only 84.0?% oil recovery, compared to 92.3?% by PSE. The ternary diagram of IPA, canola oil and water offered good approximation of the oil and water separation behavior of PSE and PSER by closely predicting the compositions of the separated phases; however, the weight ratio of the separated phases were not as closely predicted.     

Extraction of peanut skin oil by modified supercritical carbon dioxide: Empirical modelling and optimization

ABSTRACT

Peanut skin is a waste by-product from peanut industries. It is rich in antioxidants and bioactive compounds. Therefore, the objective of this study was to empirically model and optimize supercritical CO₂ extraction of oil from peanut skin. The extraction conditions were pressure (100, 200 and 300 bar), temperature (313, 328 and 343 K) and rate of modifier ethanol (0.075, 0.15 and 0.225 mL/min). The extraction process was subsequently examined using modified Brunner and Esquivel models. The optimum conditions for extraction peanut skin oil were 279 bar, 70°C and rate of modifier of 7.5% with a maximum yield of peanut skin oil of 0.83 g and initial slope of 0.568 g/min.     

Optimization of Ethanol-Ultrasound-Assisted Destabilization of a Cream Recovered from Enzymatic Extraction of Soybean Oil

A novel method using ethanol and ultrasound to extract oil from cream obtained from enzyme-assisted aqueous extraction of soybean oil was developed. To evaluate the relationships between operating variables and free oil yield and to maximize the free oil yield, response surface methodology was introduced in this work. The developed regression model was fitted with R ² = 0.9591. Optimized variables were: ethanol concentration of 73 %, ethanol addition volume of 0.55 L/kg, ultrasound power of 427 W, ultrasound time of 47 s, and ultrasound temperature of 53 °C. The free oil yield from the cream under the above conditions was 92.6 ± 3.4 %. Scanning electron microscopy (SEM) was used to evaluate the effect of ultrasonic treatment on ethanol-treated cream, and the SEM images clearly showed that the ultrasound treatment affected dispersing and fracturing of the microstructure of ethanol-treated cream.     

Effect of equilibrium oil extraction on the chemical composition and sensory quality of soy flour and concentrates

Previous studies have shown that ambient-temperature equilibrium, hexane extraction of soy flour yielded the same amount of oil as was extracted from soy flakes by conventional high-temperature processing. The oil obtained at ambient temperatures contained less phospholipid than commercial crude oils obtained by traditional processing. In this study, chemical composition, flavor and odor of soy flour obtained after oil extraction by the equilibrium procedure were evaluated before and after toasting. Results were compared with those obtained for commercial untoasted food-grade soy flakes. Chemical and sensory analyses were performed on soy protein concentrates (SPC) prepared from defatted flour, defatted toasted flour and commercial defatted white food-grade flakes. SPC were made by acid and ethanol-extraction methods. Ethanol extraction of soy flour produced SPC with similar protein, lipid and sensory qualities to those obtained from commercial flakes. Acid extraction produced SPC with more lipid than was obtained by ethanol extraction. Toasted soy flour and flakes had similar sensory properties, as did the SPC prepared from them.     

Enzymatic Demulsification of the Oil-Rich Emulsion Obtained by Aqueous Extraction of Peanut Seeds

This study details the enzymatic destabilization of the emulsion formed during aqueous extraction of peanut seeds and the quality of the resulting oil. The emulsion was exposed to enzymatic treatment and pH adjustment. The experimental results suggest that the alkaline endopeptidase Mifong^®2709 was the most effective demulsifier, while Phospholipase A2 and pH adjustment had little effect on emulsion stability. The demulsifying conditions of Mifong^®2709 were optimized by response surface methodology (RSM). The optimal conditions which produced a free oil yield of ~94 % were: 1:1 water-to-emulsion ratio, enzyme concentration of 1,600 IU/g of emulsion and 70 min hydrolysis time at 50 °C. We found that these conditions resulted in a positive relationship (R ² = 0.9671) between free oil yield and the degree of protein hydrolysis. Increased protease treatment produced a smaller number of oil droplets, but the size of these droplets increased significantly. When compared to demulsified oil products obtained by using thermal treatment, the oil obtained by Mifong^®2709 exhibited lower acid and peroxide values, contained more tocopherols and had a longer induction time as determined in the Rancimat test. The high yield and quality of peanut oil obtained by enzymatic treatment makes enzyme demulsification a promising approach to recovering free oil in aqueous extractions of peanuts.     

Recycling of Aqueous Supernatants in Soybean Oleosome Isolation

Oleosome extractions from soybean flour typically generate significant quantities of aqueous sucrose- and sodium chloride-rich supernatant which could be recycled. To determine the feasibility of recycling the oleosome process aqueous supernatants, three extraction protocols were evaluated. The first extraction used the original extraction solution, 0.1 M fresh potassium acetate pH 4.6 containing 0.4 M sucrose and 0.5 M NaCl. The second protocol reused the aqueous supernatant obtained from the first extraction. The third protocol reused the aqueous supernatant obtained from the second protocol. Oleosome extraction yields were significantly higher in the first extraction with enzymes (Multifect^® Pectinase FE, Multifect^® GC, and Multifect^® CX B, 1% each, v/w) compared to the yield when the supernatant was reused with no additional enzymes (81.41 ± 2.24 vs. 73.09 ± 3.39%, respectively). Oil yields from oleosome fractions were not statistically different when extractions were made with 0 or 3% enzymes in the third protocol. Protein was the predominant constituent in the supernatant in addition to mineral and carbohydrate. Soybean storage protein profile from recycled supernatants obtained without adding enzyme were similar to a traditional soy protein water extract but with a decrease of intensity of the β-conglycinin bands. Addition of 3% enzymes in both recycling protocols resulted in the disappearance of the α′ and α subunits of the β-conglycinin due to a protease contaminant in Multifect^® Pectinase FE. Results from this work revealed essential information for a promising possibility of the future industrial application of this technology.     

Flaking and extrusion as mechanical treatments for enzyme-assisted aqueous extraction of oil from soybeans

Flaking and extruding dehulled soybeans were evaluated as a means of enhancing oil extraction efficiency during enzyme-assisted aqueous processing of soybeans. Cellulase, protease, and their combination were evaluated for effectiveness in achieving high oil extraction recovery from extruded flakes. Aqueous extraction of extruded full-fat soy flakes gave 68% recovery of the total available oil without using enzymes. A 0.5% wt/wt protease treatment after flaking and extruding dehulled soybeans increased oil extraction recovery to 88% of the total available oil. Flaking and extruding enhanced protease hydrolysis of proteins freeing more oil. Treating extruded flakes with cellulase, however, did not enhance oil extraction either alone or in combination with protease. Discrepancies in oil extraction recoveries were encountered when merely considering crude free fat because some oil became bound to denatured protein during extrusion and/or sample drying. Bound fat was unavailable for determination by using the hexane extraction method, but was accounted for by using the acid hydrolysis method for total oil determination. Oil extraction recovery from extruded soybean flakes was affected by oil determination methods, which was not the case for unextruded full-fat soy flour.     

Optimization of an Aqueous Extraction Process for Pomegranate Seed Oil

Response surface methodology employing a five-level, four-variable central composite rotatable design was applied to study the effects of extraction time, extraction temperature, pH and water/solid ratio on the extraction yield of pomegranate seed oil using an aqueous extraction approach. In addition, quality indices, fatty acid composition and antioxidant activity of the obtained oil were studied and compared with those of typical hexane-, cold press- and hot press-extracted oil. Aqueous extraction resulted in the maximum oil recovery of 19.3% (w/w), obtained under the following critical values: water/solid ratio (2.2:1.0, mL/g), pH 5.0, extraction temperature = 63 °C and extraction time = 375 min. This yield is lower than that obtained via hexane extraction (26.8%, w/w) and higher than the yields from cold press (7.0%, w/w) and hot press (8.6%, w/w) extraction. A comparison of the characteristics of the oils based on extraction method revealed that the unsaturated fatty acid content was highest for the oil obtained by aqueous extraction. In addition, higher levels of iodine and peroxide and lower levels of acid, p-anisidine and unsaponifiable matter were observed. The oil obtained with aqueous extraction also exhibited higher antioxidant activity than oils obtained by hexane or hot press extraction.