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.     

Ethanol-Assisted Aqueous Enzymatic Extraction of Peony Seed Oil

An ethanol-assisted aqueous enzymatic extraction was performed for peony seed oil (content of 30%). This method included cooking pretreatment, pectinase hydrolysis, and aqueous ethanol extraction, and the corresponding variables in each step were investigated. The changes in viscosity and dextrose equivalent values of the reaction medium as a function of changing enzymatic hydrolysis time were compared to the oil yield. The microstructures of peony seeds were analyzed using confocal laser scanning microscopy to understand the process of oil release as a result of cooking and grinding. The highest oil yield of 92.06% was obtained when peony seeds were cooked in deionized water with a solid–liquid ratio of 1:5 (w/v) at 110°C for 1 hour, ground to 31.29 μm particle size, treated with 0.15% (w/w) pectinase (temperature 50°C, pH 4.5, time 1 hour), and then extracted with 30% (v/v) aqueous ethanol (temperature 60°C, pH 9.0, time 1 hour). After processing with pectinase followed by ethanol extraction, the residual oil content in water and sediment phase decreased to 5% and 3%, respectively. The quality of the oil obtained by ethanol-assisted aqueous enzymatic extraction was good, complying with the Chinese standard.     

水酶法提取大豆油

The procedure of enzymatic aqueous extraction of soybean oil was assessed when two-step controlled enzymatic hydrolysis was applied. With aqueous extraction of soybean oil-containing protein, the highest yield of oil was 96.1% at the optimized conditions studied. Soybean oil-containing protein was hydrolyzed and resulted in releasing part of oil. The separated protein that contained 40% oil was enriched due to its adsorption capacity of released oil, the average oil extraction yeild reached 93.5%. Then the high oil content protein was hydrolyzed again to release oil by enzyme, the oil extraction yeild was 80.4%. As a result, high quality of soybean oil was obtained and the content of total oil vield was 74.4%.     

Optimization of the Aqueous Enzymatic Extraction of Oil from Iranian Wild Almond

The seeds of wild almond, Amygdalus scoparia, contain a relatively high quantity of oil. In the current study, aqueous enzymatic extraction of the oil from Iranian wild almond was investigated using a protease and a cellulase to assist the extraction process. The effects of temperature, incubation time and pH on the oil recovery were evaluated using Box?Behnken design from response surface methodology (RSM). A 77.3 % recovery was predicted for oil using aqueous enzymatic extraction procedure at the optimized conditions of RSM (pH 5.76; 50 °C/5 h) when both enzymes were used at 1.0 % level (v/w). In practice, when both enzymes were used, a maximum of 77.8 % oil recovery was achieved at pH 5; 50 °C/4 h. Fatty acid profile, refractive index and saponification value of the aqueous enzymatic extracted oil in the current study were similar to those of the oil extracted with hexane. However, acid value, unsaponifiable matter and p‐anisidine value were higher when compared to those with hexane extracted oil. Peroxide value of the aqueous enzymatic oil was lower than that of oil extracted by hexane. Aqueous enzymatic extraction can be suggested as an environmentally‐friendly method to obtain oil from wild almond.     

Optimization of the Aqueous Enzymatic Extraction of Rapeseed Oil and Protein Hydrolysates

An aqueous enzymatic extraction method was developed to obtain free oil and protein hydrolysates from dehulled rapeseeds. The rapeseed slurry was treated by the chosen combination of pectinase, cellulase, and β-glucanase (4:1:1, v/v/v) at concentration of 2.5% (v/w) for 4 h. This was followed by sequential treatments consisting of alkaline extraction and an alkaline protease (Alcalase 2.4L) hydrolysis to both produce a protein hydrolysate product and demulsify the oil. Response surface methodology (RSM) was used to study and optimize the effects of the pH of the alkaline extraction (9.0, 10.0 and 11.0), the concentration of the Alcalase 2.4L (0.5, 1.0 and 1.5%, v/w), and the duration of the hydrolysis (60, 120, and 180 min). Increasing the concentration of Alcalase 2.4L and the duration of the hydrolysis time significantly increased the yields of free oil and protein hydrolysates and the degree of protein hydrolysis (DH), while the alkaline extraction pH had a significant effect only on the yield of the protein hydrolysates. Following an alkaline extraction at pH 10 for 30 min, we defined a practical optimum protocol consisting of a concentration of 1.25–1.5% Alcalase 2.4L and a hydrolysis time between 150 and 180 min. Under these conditions, the yields of free oil and protein hydrolysates were 73–76% and 80–83%, respectively. The hydrolysates consisted of approximately 96% of peptides with a MW less than 1500, of which about 81% had a MW less than 600 Da.     

Two-Stage Countercurrent Enzyme-Assisted Aqueous Extraction Processing of Oil and Protein from Soybeans

Enzyme-assisted aqueous extraction processing (EAEP) is an increasingly viable alternative to hexane extraction of soybean oil. Although considered an environmentally friendly technology where edible oil and protein can be simultaneously recovered, this process employs much water and produces a significant amount of protein-rich aqueous effluent (skim). In standard EAEP, highest oil, protein and solids yields are achieved with a single extraction stage using 1:10 solids-to-liquid ratio (extruded flakes/water), 0.5% protease (wt/g extruded flakes), pH 9.0, and 50 °C for 1 h. To reduce the amount of water used, two-stage countercurrent EAEP was evaluated for extracting oil, protein and solids from soybeans using a solids-to-liquid ratio of 1:5–1:6 (extruded flakes/water). Two-stage countercurrent EAEP achieved higher oil, protein and solids extraction yields than using standard EAEP with only one-half the usual amount of water. Oil, protein and solids yields up to 98 and 96%, 92 and 87%, and 80 and 77% were obtained when using two-stage countercurrent EAEP (1:5–1:6) and standard single-stage EAEP (1:10), respectively. Recycling the second skim obtained in two-stage countercurrent EAEP enabled reuse of the enzyme, with or without inactivation, in the first extraction stage producing protein with different degrees of hydrolysis and the same extraction efficiency. Slightly higher oil, protein and solids extraction yields were obtained using unheated skim compared to heated skim. These advances make the two-stage countercurrent EAEP attractive as the front-end of a soybean biorefinery.     

Fatty and Resinic Acids Extraction from Crude Tall Oil

Abstract

The separation of fatty and resinic acidic fractions from crude tall-oil soap solutions with n-heptane by the technique of dissociation extraction is discussed. The theory of the overall process is supported by a systematic study developed to cover the high selectivity demonstrated in the differential solubility and the aptness between fatty and diterpenic acids to both liquids phases. To study the main factors affecting those liquid-liquid extraction systems and the amphiphilic behavior of such molecules involved, sodium salts aqueous solutions of crude tall oil and synthetic mixtures as molecular acidic models were used.     

Extraction and Demulsification of Oil From Wheat Germ,Barley Germ,and Rice Bran Using an Aqueous Enzymatic Method

An aqueous enzymatic method was developed to extract oil from wheat germ. Wheat germ pretreatment, effect of various industrial enzymes, pH, wheat germ to water ratio, reaction time and effect of various methods of demulsification, were investigated. Pretreatment at 180 °C in a conventional oven for 4 min reduced the moisture 12.8–2.2 % and significantly increased the oil yield. Adding a combination of protease (Fermgen) and cellulase (Spezyme CP) resulted in a 72 % yield of emulsified oil from wheat germ (both commercial and laboratory milled wheat germ). Using the same oil extraction conditions optimized for wheat germ, yields of 51 and 39 % emulsified oil were obtained from barley germ (laboratory milled), and rice bran, respectively. Three physical demulsification methods (heating, freeze-thawing, and pH adjustment) and enzymatic methods (Protex 6L, Protex 7L, Alcalase, Fermgen, Lysomax and G-zyme 999) were compared. After demulsification with Protex 6L, free oil yields of 63.8 and 59.5 % were obtained with commercial wheat germ and with laboratory milled wheat germ, respectively. Using the same demulsification conditions optimized for wheat germ, yields of 45.7 % emulsified oil and 35 % free oil were obtained for barley germ and rice bran, respectively.     

Downstream Processes for Aqueous Enzymatic Extraction of Rapeseed Oil and Protein Hydrolysates

Downstream processes following aqueous enzymatic extraction (AEE) of rapeseed oil and protein hydrolysates were developed to enhance the oil and protein yields as well as to purify the protein hydrolysates. The wet precipitate (meal residue) from the AEE was washed with twofold water at 60 °C, pH 11 for 1 h. Emulsions from the AEE and the washing step were pooled and submitted to a stepwise demulsification procedure consisting of storage-centrifugation and freezing–thawing followed by centrifugation. Aqueous phases were pooled and adsorbed onto macroporous adsorption resins (MAR) to remove salts and sugars. Following extensive rinsing with deionized water (pH 4), desorption was achieved by washing with 85% ethanol (v/v) to obtain crude rapeseed peptides (CRPs). In a separate experiment, stepwise desorption was carried out with 25, 55, and 85% ethanol to separate the bitter peptides from the other peptides. Using a combination of the AEE process, washing and demulsification steps, the yields of the total free oil and protein hydrolysates were 88–90% and 94–97%, respectively. The protein recovery was 66.7% and the protein content was enriched from 47.04 to 73.51% in the CRPs. No glucosinolates and phytic acid were detected in the CRPs. From the stepwise desorption, a non-bitter fraction RP25 (containing 64–66% of total desorbed protein) had a bland color and significantly higher protein content (81.04%) and hence was the more desirable product.     

水酶法提取肉桂油的工艺研究

探索了肉桂油的水酶法提油工艺.研究了不同酶系以及酶解条件对肉桂油得率的影响.结果表明,果胶酶的作用效果好;酶解条件中,加酶量、酶解时间都对肉桂油得率有显著的影响,通过单因素分析及正交试验的结果,得出在固液比1∶6、酶解pH=3.5、酶解温度40℃、加酶量1.5％、酶解时间2h条件下,肉桂油得率能达到1.72％.经检测得到处理得到的肉桂油中桂皮醛含量达到83.6％.     

Unexploited Thapsia garganica,Orlaya maritima,and Retama raetam Seeds: Potential Sources of Unsaturated Fatty Acid and Natural Antioxidants

Total lipid contents, fatty acid compositions, phenolic profiles and antioxidants activities of seeds from Thapsia garganica, Orlaya maritima, and Retama raetam were investigated. The oil values were more than 26 %, except seeds of R. raetam (ca. 3 %). Unsaturated fatty acids accounted for the majority of the fatty acids (more than 75 %). Oleic and linoleic acid were the predominant fatty acids. Total phenolic compounds (24–104 mg GAE g^?1 DR), total flavonoids (4–102 mg QE g^?1g DR), total tannins (28–85 mg GAE g^?1 DR) and condensed tannins (0.62–131 mg CE g^?1 DR) were also determined. The antioxidant activities using different assays were evaluated. The predominant detected classes were the phenolic acids (42–85 %) and the flavonoids (11–48 %). The major phenolic acids were caffeic, trans‐4‐hydroxy‐3‐methoxycinnamic, p‐coumaric, and gallic acid. The predominant flavonoids were quercetin, luteolin, naringin, apigenin, and kaempferol. This study brings attention to the medicinal importance of these species as a source of oil and antioxidant molecules.     

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.     

Physico-Chemical Characteristics of Citrus Seeds and Seed Oils from Pakistan

The physico-chemical characteristics of the seeds and seed oils of four citrus species, Mitha (Citrus limetta), Grapefruit (Citrus paradisi), Mussami (Citrus sinensis), and Kinnow (Citrus reticulata) were investigated. The hexane-extracted oil content of citrus seeds ranged from 27.0 to 36.5%. The protein, fiber and ash contents were found to be 3.9–9.6%, 5.0–8.5%, and 4.6–5.6%, respectively. The extracted oils exhibited an iodine value of 99.9–110.0; refractive index (40 °C), 1.4639–1.4670; density (24 °C), 0.920–0.941 mg/mL; saponification value, 180.9–198.9; unsaponifiable matter, 0.3–0.5%; acid value (mg KOH/g of oil), 0.5–2.2 and color (1-in. cell) 1.4–3.0R + 15.0–30.0Y. The oils revealed a good oxidative stability as indicated by the determinations of specific extinctions at 232 and 270 nm (2.3–4.4 and 0.6–0.9, respectively), p-anisidine value (2.2–3.2) and peroxide value (1.6–2.4 mequiv/kg of oil). The citrus seed oils mainly consisted of linoleic acid (36.1–39.8%). Other prominent fatty acids were palmitic acid (25.8–32.2%), oleic acid (21.9–24.1%), linolenic acid (3.4–4.4%), and stearic acid (2.8–4.4%). The contents of tocopherols (α, γ, and δ) in the oil were 26.4–557.8, 27.7–84.1, and 9.1–20.0 mg/kg, respectively. The results of the present study demonstrated that the seeds of citrus species investigated are a potential source of valuable oil which might be utilized for edible and other industrial applications.     

Efficient and Response Surface Optimized Aqueous Enzymatic Extraction of Camellia oleifera (Tea Seed) Oil Facilitated by Concurrent Calcium Chloride Addition

This paper reports an efficient aqueous enzymatic extraction (AEE) method for Camellia oleifera seed oil with the aid of response surface analysis. A maximum oil recovery of ~93.5% was obtained when a 2‐step AEE process was performed using 0.80% cellulase (v/w) solution at pH 6.0 maintained at 50 °C for 1 h followed by a solution of 0.70% Alcalase® with pH 9.2 at 57 °C for 4.1 h. It was found that the addition of Ca²⁺ during the proteolysis stage improved the free oil yield from ~62.1 to ~86.6%. This was attributed to the removal of tea saponins, cross‐linkage of anionic polysaccharides, and destabilization of cream emulsion by Ca²⁺. This was verified by decreased tea saponin and polysaccharide levels in the cream emulsion and bulk solution as well as lowering of the emulsion fraction. It was determined that addition of CaCl₂ solution in continuous flow to the proteolysate is superior to one‐time or batch addition in inhibiting emulsion formation. The addition of CaCl₂ may provide a means of replacing the more laborious, time‐consuming demulsification process otherwise required.     

Enzyme-Assisted Aqueous Extraction of Oil and Protein from Soybeans and Cream De-emulsification

The effects of two commercial endoproteases (Protex 6L and Protex 7L, Genencor Division of Danisco, Rochester, NY, USA) on the oil and protein extraction yields from extruded soybean flakes during enzyme-assisted aqueous extraction processing (EAEP) were evaluated. Oil and protein were distributed in three fractions generated by the EAEP: cream + free oil, skim and insolubles. Protex 6L was more effective for extracting free oil, protein and total solids than Protex 7L. Oil and protein extraction yields of 96 and 85%, respectively, were obtained using 0.5% Protex 6L. Enzymatic and pH treatments were evaluated to de-emulsify the oil-rich cream. Cream de-emulsification generated three fractions: free oil, an intermediate residual cream layer and an oil-lean second skim. Total cream de-emulsification was obtained when using 2.5% Protex 6L and pH 4.5. The extrusion treatment was particularly important for reducing trypsin inhibitor activity (TIA) in the protein-rich skim fraction. TIA reductions of 69 and 45% were obtained for EAEP skim (the predominant protein fraction) from extruded flakes and ground flakes, respectively. Protex 6L gave higher degrees of protein hydrolysis (most of the polypeptides being between 1,000 and 10,000 Da) than Protex 7L. Raffinose was not detected in the skim, while stachyose was eliminated by α-galactosidase treatment.     

Characteristics of Oil and Skim in Enzyme-Assisted Aqueous Extraction of Soybeans

The economic viability of enzyme-assisted aqueous extraction processing (EAEP) of soybeans depends on properties and potential applications of all fractions (skim and insolubles as well as oil). EAEP oil contained lower free fatty acid, phosphorus, and tocopherol contents, similar unsaponifiable matter levels, and higher degrees of oxidation (peroxide and p-anisidine values) than hexane-extracted oil. The phospholipid profile of EAEP fractions was mainly composed of phosphatidic acid, followed by phosphatidylcholine, phosphatidylinositol, and phosphatidylethanolamine. Most of phospholipids were present in the skim, except for phosphatidic acid, which was the major phospholipid in the cream fraction. Skim and cream contained 55 and 3 % of the soluble carbohydrates in the original extruded flakes, respectively. Soluble carbohydrates of the skim were mainly composed of stachyose (5.8 ± 0.8 mg/mL) and sucrose (9.9 ± 0.8 mg/mL), which were hydrolyzed into glucose, galactose, and fructose after addition of α-galactosidase. Skim and cream peptides contained <20 kDa MW molecules. About 71 % of the skim peptides were <20 kDa MW, with 49 % being <1.35 kDa MW, 22 % being 17–1.35 kDa MW, and 29 % being 44–670 kDa MW. Skim protein and carbohydrate contents make this fraction suitable for replacing water in ethanol fermentations, thereby improving the fermentation rate/production and the nutritional quality of distiller’s dried grains with solubles.     

葡萄籽中主要成分提取方法的研究

对葡萄籽中3种有经济价值的成分：葡萄籽油、蛋白质、原花青素的提取方法以及原花青素的定量分析方法做了简要介绍。通过比较不同方法,同时对一些影响因素进行分析,提出了对3种有效成分分步提取的思路,以期达到充分、全面利用葡萄籽这一经济资源。     

Extraction of Fatty Acids from Noncatalytically Cracked Triacylglycerides Using Aqueous Amines

It has been reported that a basic aqueous solution was effective in extracting short chain C₂–C₆ fatty acids from noncatalytically cracked triacylglyceride oils. However, the extraction efficiency was not optimal over the entire range (C₂–C₁₂) of acids present in the cracking reactor organic liquid product (OLP). Therefore, an additional study was performed to explore the efficiency of solvent extraction using aqueous amines for this application. Based on the screening of several amines, two tertiary amines, trimethyl amine (TMA), and dimethyl ethanolamine (DMEA), were selected and evaluated. The extraction conditions were optimized with respect to several factors: temperature, amine concentration, and the amine-to-OLPratio (amine/OLP). Under optimal conditions, both TMA and DMEA were effective in extracting a wide range of organic acids, with TMA removing 93% of total acids and DMEA removing 100% of total acids. The amine/OLP was found to be a significant factor, as was the concentration of the amine solution. Temperature was not found to be a significant factor over the range studied. These results provide a basis for the development of a scalable, continuous process to produce a variety of C₂–C₁₂ fatty acids from biological sources.     

Fatty Acids and Flavor Components in the Oil Extracted from Golden Melon Seeds

For complete utilization of raw materials and edible oil production, the oil from golden melon seeds (GSs) is extracted via the cold-pressing, hot-pressing, and ultrasound-assisted aqueous enzymatic extraction (AEE), and the fatty acid composition, and nutritional value of the extracted GS oils (GSOs) are analyzed. The volatile compounds present in the GSOs are determined using gas chromatography–mass spectrometry. The aroma profiles of different GSO samples are further distinguished by using an electronic nose. A total of 16 fatty acids are identified in the GSO samples, with atherogenic, thrombogenic, and nutritive value indices ranging from 0.142–0.151, 0.366–0.403, and 5.019–5.299, respectively. Moreover, 43 volatile compounds, including esters, hydrocarbons, alcohols, ketones, pyrazines, and aldehydes are identified. The cold-pressed GSO presents fresh and fruity flavors, while the hot-pressed GSO presents roasted, nutty, fatty, and fruity flavors, and the GSO obtained via AEE presents fatty and fruity flavors. The acid and peroxide contents of these oil samples are 0.69–079 mg g⁻¹ and 5.17–5.79 mmol kg⁻¹, respectively. The results indicate that the extraction method affects the fatty acid composition, flavor components, and physiochemical properties of the GSO. This study may help promote the development of edible GSO. Practical applications: With high demand for edible oils, it is of great significance to find natural edible oils from different sources. The oil in golden melon seeds is extracted by different methods. Their fatty acid composition and flavor components are analyzed. The GSO extracted via AEE method is rich in fatty acids composition. This work would guide the development of an edible GSO and increase the value of golden melon.     

Pretreatment Camellia Seeds by Protease and Application to Extraction of Camellia Oil

High-temperature pretreatment that is currently used in camellia oil extraction can have negative effects on the quality of camellia oil. In this study, the enzymatic pretreatment of camellia seeds is explored as an alternative to high-temperature pretreatment. The main conditions for enzymatic pretreatment of camellia seeds including enzyme, pH, temperature, time, and buffer solution are optimized using the response surface methodology. Under the optimal conditions of enzymatic pretreatment, the oil recovery is close to 75%. Moreover, residual oil recovery from camellia seeds subjected to 1398 neutral protease pretreatment (4 g per kg seeds) and high-temperature pretreatment are 5.62 ± 0.08% and 9.97 ± 0.18%, respectively. The enzymatic pretreatment is further applied to pre-pressing solvent extraction of camellia oil, the cake oil recovery from camellia seeds subjected to enzymatic pretreatment is higher than that from high-temperature pretreatment. These results show that enzymatic pretreatment of camellia seeds has potential for application in the oil industry. Practical Applications : This study suggests that enzymatic pretreatment can replace high-temperature pretreatment and improve oil recovery and oil quality. Ultimately, this method can be used to extract camellia oil.