Supercritical carbon dioxide extraction of oil and squalene from amaranthus grain

Supercritical carbon dioxide (SC CO(2)) was used for the extraction of oil and squalene from Amaranthus grain. Very small amounts of oil could be extracted by SC CO(2) from undisrupted grains, although SC CO(2) possesses higher diffusivity. Grinding increased the extraction rate and oil yield, and smaller particle size gave higher extraction rate. The oil yield and initial extraction rate increased linearly with the increasing SC CO(2) flow rate from 1 to 2 L/min. Increasing the flow rate of SC CO(2) above 2 L/min resulted in only a slight increase of oil yield and extraction rate. In the pressure range of 150-250 bar, extraction decreased with increasing temperature at a constant pressure, whereas at a pressure of 300 bar, the extraction yield increased with increasing temperature. Possible reasons for this are discussed. Effects of temperature and pressure on squalene yield were different from those on oil yield. A good oil yield (4.77 g of oil/100 g of grain) was obtained at 40 degrees C and 250 bar. The highest squalene yield (0.31 g of squalene/100 g of grain) and concentration (15.3% in extract) were obtained at 50 degrees C and 200 bar, although the oil yield under this condition was low (2.07 g of oil/100 g of grain). The moisture content within 0-10% had little influence on yields of oil and squalene at 40 degrees C and 250 bar. Finally, the oil yield and the squalene concentration in the extracts by SC CO(2) were compared to those by solvent extraction.     

Extraction of natural vitamin E from wheat germ by supercritical carbon dioxide

An efficient supercritical fluid extraction (SFE) process with carbon dioxide (SFE-CO(2)) was developed for the extraction of natural vitamin E (V(E)) from wheat germ. Both the pretreatment of extracted wheat germ and extraction conditions were optimized to ensure maximal V(E) yield. The extraction was undertaken at the extracting pressure of 4000-5000 psi, the extracting temperature of 40-45 degrees C, and the carbon dioxide flow rate of 2.0 mL/min for 90 min. An optimized pretreatment of wheat germ was usually necessary with a particle size of 30 mesh and a moisture content of 5.1%. A yield comparison of V(E) and its isomers extracted by supercritical CO(2) with those by conventional solvent extraction suggested that this SFE process was a practical process prospectively superior to conventional solvent extraction to prepare V(E) from wheat germ.     

牡丹籽油提取工艺与精炼工艺的优化

为高效利用牡丹籽油,以牡丹籽油的各项理化性质为指标,通过单因素试验分析不同浸提溶剂、浸提时间、料液比、浸提温度和粉碎粒度等因素对牡丹籽油提取率的影响,在此基础上利用响应面分析方法对牡丹籽油的提取工艺进行优化;同时对牡丹籽油进行精炼,测定牡丹籽精炼油的各项理化指标并进行主成分分析,以确定牡丹籽油的最佳精炼工艺。结果表明,牡丹籽油提取的最佳工艺条件为:有机溶剂石油醚、浸提温度57℃、浸提时间5 h、料液比1∶11、粉碎粒度40目。在精制过程中分别加入4%沸水、8%碱液和2%活性白土,得到的精炼油磷脂含量、过氧化值、碘值及酸值分别为8.37 mg·100g^-1、2.48 meq·kg^-1、160.85 g·100 g^-1、0.37 mg NaOH·g^-1,牡丹籽油过活性碳柱后其精炼得率达21.37%。本研究结果为牡丹籽油的工业化生产提供了更优的工艺路线。     

Supercritical carbon dioxide extraction and fractionation of fennel oil

Ground fennel seeds were extracted with supercritical carbon dioxide. Small-scale subsequent extractions of the same sample showed that the composition of volatile compounds was changed with the extension of extraction time and only principal volatile components (limonene, fenchone, methylchavicol, and anethole) were present in the last-extracted sample. Fennel oil was successfully fractionated into the essential oil rich and fatty oil rich products in pilot-scale apparatus using two separators in series. Designed experiments were carried out to map the effects of pressure and temperature in the first separator on the yields and compositions of the products. The minimum level of the total undesired components in both essential oil rich and fatty oil rich products appeared at a pressure of 80-84 bar and a temperature of 31-35 degrees C in the first separator. Supercritical CO(2) extraction of fennel seeds resulted in higher yield (10.0%) than steam distillation (3.0%), almost the same yield as hexane extraction (10.6%), and lower yield than alcohol extraction (15.4%). Analysis of the volatile compounds revealed the significant difference of the composition in distilled oil and oleoresins prepared by CO(2) and solvent extractions. Sensory evaluation showed that the CO(2) extraction product and distilled oil were more intense in odor and taste than alcohol and hexane extracts.     

超临界CO2萃取小麦胚芽油的试验研究

测定并分析了小麦胚芽的粒度、含水量、萃取温度、压力和CO₂流量对小麦胚芽油的超临界CO₂萃取率及产物品质(包括脂肪酸构成、VE含量、酸价和色泽)的影响。     

Fractionation of flax shives by water and aqueous ammonia treatment in a pressurized low-polarity water extractor

Fractionation of flax shives into cellulose, hemicellulose, and lignin with a two-stage extraction process using water and aqueous ammonia was carried out in a pressurized low-polarity water extractor operated at different temperatures, flow rates, and ammonia concentrations. During the first stage with water, 84% of hemicellulose and 32% of lignin were removed at 190 degrees C at a flow rate of 1.5 mL/min for 30 min. During the second stage with aqueous ammonia, more than 77% of the lignin was removed, and hemicellulose removal reached 95% at 200 degrees C at a flow rate of 0.5 mL/min and with a solvent/feed ratio of 40 mL/g. The temperature and flow rate had a significant effect on lignin removal. The impact of additives (anthraquinone and hydrogen peroxide) and modifications (overnight soaking, reduced particle size, and elevated temperature) on lignin extraction was also studied. The combination of higher temperatures and reduced particle sizes resulted in enhanced lignin extraction. The extraction profiles of free phenolics (vanillin, acetovanillone, and vanillic acid) during the two-stage processing were monitored and compared with those of lignin.     

Analysis of free and esterified ergosterol in tomato products

A new extraction and chromatographic procedure to quantify free and esterified ergosterol in tomato products was devised. The extraction solution was composed of a dichloromethane/methanol mixture in a 2:1 (v/v) ratio. This extraction solvent allowed for higher ergosterol recovery from tomato products (an average of 25% more) compared to hexane, which is frequently employed for ergosterol extraction. Both free and esterified ergosterol were determined by HPLC reverse-phase chromatography employing a Nova-Pak C-18 column (300 x 3.9 mm), filled with 4 mm average particle size and a guard column of the same material. The elution was performed at a flow rate of 1 mL. min(-1) with a linear gradient of solvent A (methanol/water, 80:20, v/v) and solvent B (dichloromethane). The gradient, starting at sample injection, was from 0 to 50% B for 20 min for the free ergosterol analysis and additional 15 min at 50% B to analyze the ergosterol esters. This technique has proven to be more sensitive for ergosterol determination than other reported chromatographic procedures. Moreover, ergosterol esters, extracted from various fungal sources, separated well and were easily quantified.     

Extraction of grape seed oil using compressed carbon dioxide and propane: extraction yields and characterization of free glycerol compounds

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

Supercritical carbon dioxide extraction and characterization of Laurus nobilis essential oil

Supercritical carbon dioxide extraction allowed essential oil of Laurus nobilis to be obtained. Extraction conditions were as follows: pressure, 90 bar; temperature, 50 degrees C; and carbon dioxide flow, Phi = 1.0 kg/h. Waxes were entrapped in the first separator set at 90 bar and -10 degrees C. The oil was recovered in the second separator working at 15 bar and 10 degrees C. The main components were 1,8-cineole (22.8%), linalool (12.5%), alpha-terpinyl acetate (11.4%), and methyleugenol (8.1%). Comparison with the hydrodistilled oil did not reveal any significant difference. Collection of samples at different extraction times during supercritical extraction allowed the change of the oil composition to be monitored. Lighter compounds such as hydrocarbon and oxygenated monoterpenes were extracted in shorter times than the heavier hydrocarbon and oxygenated sesquiterpenes.     

Comparative analysis of the oil and supercritical CO2 extract of Elettaria cardamomum (L.) Maton

The volatile oil of Elettaria cardamomum (L.) Maton seeds was obtained by supercritical CO(2) extraction (SC-CO(2)). The effect of the extraction conditions on the yield and composition of the resulting cardamom volatile oil was examined by testing two pressure values, 9.0 and 11.0 MPa; two temperatures, 40 and 50 degrees C; two flow rate values, 0.6 and 1.2 kg/h; and two particles size values, 250-425 and >850 microm. The extraction conditions that gave the highest yield, Y (grams of extract per gram of seeds), of 5.5%, were as follows: pressure, 9.0 MPa; temperature, 40 degrees C; carbon dioxide flow, phi = 1.2 kg/h; and particles sizes in the range of 250-425 microm. Waxes, recovered as traces, were entrapped in the first separator set at 9.0 MPa and -10 degrees C. The oil was recovered in the second separator working at 1.5 MPa and 10 degrees C. The main components were as follows: alpha-terpinyl acetate, 42.3%; 1,8-cineole, 21.4%; linalyl acetate, 8.2%; limonene, 5.6%; and linalool, 5.4%. A comparison with the hydrodistilled oil, obtained at a yield of 5.0%, did not reveal any consistent difference. In contrast, the extract obtained using hexane, Y = 7.6%, showed strong composition differences. Indeed, the volatile fraction of the extract was made up mainly of the following: limonene, 36.4%; 1,8-cineole, 23.5%; terpinolene, 8.6%; and myrcene, 6.6%.     

Development of a rapid method for the sequential extraction and subsequent quantification of fatty acids and sugars from avocado mesocarp tissue

Methods devised for oil extraction from avocado (Persea americana Mill.) mesocarp (e.g., Soxhlet) are usually lengthy and require operation at high temperature. Moreover, methods for extracting sugars from avocado tissue (e.g., 80% ethanol, v/v) do not allow for lipids to be easily measured from the same sample. This study describes a new simple method that enabled sequential extraction and subsequent quantification of both fatty acids and sugars from the same avocado mesocarp tissue sample. Freeze-dried mesocarp samples of avocado cv. Hass fruit of different ripening stages were extracted by homogenization with hexane and the oil extracts quantified for fatty acid composition by GC. The resulting filter residues were readily usable for sugar extraction with methanol (62.5%, v/v). For comparison, oil was also extracted using the standard Soxhlet technique and the resulting thimble residue extracted for sugars as before. An additional experiment was carried out whereby filter residues were also extracted using ethanol. Average oil yield using the Soxhlet technique was significantly (P < 0.05) higher than that obtained by homogenization with hexane, although the difference remained very slight, and fatty acid profiles of the oil extracts following both methods were very similar. Oil recovery improved with increasing ripeness of the fruit with minor differences observed in the fatty acid composition during postharvest ripening. After lipid removal, methanolic extraction was superior in recovering sucrose and perseitol as compared to 80% ethanol (v/v), whereas mannoheptulose recovery was not affected by solvent used. The method presented has the benefits of shorter extraction time, lower extraction temperature, and reduced amount of solvent and can be used for sequential extraction of fatty acids and sugars from the same sample.     

杜仲叶绿原酸的微波提取及高速逆流色谱分离纯化

以杜仲叶为原料,正交试验优化了微波辅助提取绿原酸的工艺条件。应用高速逆流色谱（HSCCC）分离制备高纯度杜仲叶绿原酸,通过质谱技术与核磁共振技术进行结构鉴定。结果表明,杜仲叶最佳提取工艺条件为微波辅助50%的丙酮水溶液浸提,料液比1∶30,提取时间25min,提取功率400W,绿原酸的提取率达2.28%;高速逆流色谱法...     

亚临界丙烷萃取米糠油及其微量活性组分动力学模型

为了揭示亚临界流体萃取米糠油及其微量活性组分的动力学规律,该文以亚临界丙烷为萃取介质,研究了米糠油、γ-谷维素及α-生育酚等活性组分在不同萃取温度和时间的萃取率,并基于 Baümler 模型对目标物的萃取率进行模型拟合,建立相应的动力学模型并验证。结果表明,亚临界萃取过程中目标物的相对萃取率随时间增长递增,且在初始阶段（洗涤过程）的增长速率快于第二阶段（扩散过程）的增长速率;同时,升高萃取温度可同时提高目标产物的扩散系数和相对萃取率;基于Baümler模型可较好拟合亚临界丙烷萃取米糠油、γ-谷维素和α-生育酚的动力学过程（R2>0.95）,所得动力学模型具有较好的预测准确性。由Arrhenius方程可计算出米糠油、α-生育酚和γ-谷维素的亚临界萃取反应活化能,其中米糠油的活化能最低（5.23 kJ/mol）,α-生育酚次之（7.05 kJ/mol）,γ-谷维素最高（9.11 kJ/mol）,表明γ-谷维素最难萃取且对温度依赖程度最高;根据拟合所得动力学模型,对米糠油提取率进行预测,结果表明,该模型对米糠油萃取率的预测准确率达95.8%,而对γ-谷维素和α-生育酚萃取率的预测准确度稍低,分别达94.7%和94.4%,对三者均具有很好的预测准确性。总之,基于 Baümler 模型可以较好地建立米糠油及其有益伴随物的亚临界萃取动力学模型,从而较为准确的预测米糠油及其微量活性组分的萃取率,对米糠油的亚临界萃取工艺具有一定的理论指导意义。     

乙醇水溶液提取玉米胚芽油的工艺优化

为了解决水酶法提取玉米胚芽油生产成本高、提取时间长的缺点,该文采用乙醇水溶液作为提取剂提取玉米胚芽油。通过对粒径、料液比、温度、乙醇体积分数、p H值和时间等条件对油在油相、水相和渣相中分布的研究发现,物料粒径和乙醇体积分数对提高清油得率具有显著(P0.05)的影响,而提取时间对清油得率的影响最小(P0.05)。在单因素试验的基础上通过正交试验,得出乙醇水溶液提取玉米胚芽油的最佳工艺参数为:物料细粉4次(此时粒径为49.18μm)、料液比1∶7 g/m L、温度70℃、乙醇体积分数30%、p H值9.0、提取时间2 h。在该条件下,清油的得率为94.05%±0.32%,水相含油量为3.49%±0.77%,渣相含油量为2.55%±0.82%。分析乙醇水溶液提取的玉米胚芽毛油酸价、过氧化值和含水率等指标发现,该毛油的质量优于国标规定的玉米原油,并且和压榨一级成品油指标接近,只需要经过简单精炼就可以达到食用油要求。研究结果为乙醇水溶液工业化生产玉米胚芽油提供参考。     

Selected Factors Affecting Crude Oil Analysis of Distillers Dried Grains with Solubles (DDGS) as Compared with Milled Corn

With increasing production of distillers dried grains with solubles (DDGS), both fuel ethanol and animal feed industries are demanding standardized protocols for characterizing quality. AOCS Approved Procedure (Am 5‐04) was used for measuring crude oil content in milled corn and resulting DDGS. Selected factors, including sample type (milled corn, DDGS), sample origin (ethanol plant 1, 2, 3), sample particle size (original matrix, <0.71 mm, <0.50 mm mesh opening; the last two materials were obtained by grinding and sieving), solvent type (petroleum ether, hexane), extraction time (30, 60 min), and postextraction drying time (30, 60 min) were investigated by a complete factorial design. For milled corn, only sample origin and extraction time had significant effects (P < 0.05) on crude oil values measured, but for DDGS, besides those two factors, sample particle size, solvent type, and drying time also had significant effects. Among them, the particle size of DDGS had the most effect. On average, measured oil content in DDGS ranged from 11.11% (original matrix) to 12.12% (<0.71 mm) and to 12.55% (<0.50 mm). For measuring the crude oil content of DDGS, particle size reduction, 60 min of extraction, and 60 min of drying are recommended. Regardless of the underlining factors, the method was very repeatable (standard errors <0.05). The observed particle size effect on crude oil analysis of DDGS suggests the need for similar confirmations using other analytical methods.     

Supercritical fluid extraction of lycopene from tomato processing byproducts

Tomato seeds and skins acquired from the byproduct of a local tomato processing facility were studied for supercritical fluid extraction (SFE) of phytochemicals. The extracts were analyzed for lycopene, beta-carotene, alpha-carotene, alpha-tocopherol, gamma-tocopherol, and delta-tocopherol content using high-performance liquid chromatography-electrochemical detection and compared to a chemically extracted control. SFEs were carried out using CO(2) at seven temperatures (32-86 degrees C) and six pressures (13.78-48.26 MPa). The effect of CO(2) flow rate and volume also was investigated. The results indicated that the percentage of lycopene extracted increased with elevated temperature and pressure until a maximum recovery of 38.8% was reached at 86 degrees C and 34.47 MPa, after which the amount of lycopene extracted decreased. Conditions for the optimum extraction of lycopene from 3 g of raw material were determined to be 86 degrees C, 34.47 MPa, and 500 mL of CO(2) at a flow rate of 2.5 mL/min. These conditions resulted in the extraction of 61.0% of the lycopene (7.19 microg lycopene/g).     

马铃薯茎叶挥发性成分的两种提取方法比较

应用水蒸气蒸馏-溶剂萃取法和微波辅助-溶剂萃取法提取了成熟期马铃薯茎叶挥发性成分。用乙醚为萃取溶剂的水蒸气蒸馏法提取时,以0.533%（m/m）得油率获得精油;以正己烷为溶剂的微波辅助萃取法的最适提取条件为：温度60℃,时间9 min,液料比10︰1（V/m）,在此条件下的得油率为0.528%（m/m）。用GC-MS分析检测出水蒸气蒸馏法获得的精油含有81个成分,解析鉴定出占精油相对含量79.386%的43种物质,醇类化合物（24.789%）为主要成分;微波法获得的精油检测出78个成分,解析鉴定出占总精油82.226%的36种成分,酯类化合物（44.482%）为主要成分。2种提取方法获得的精油成分有很大的差别。     

水酶法提取山核桃油脂工艺研究

为优化水酶法提取山核桃油脂工艺,以山核桃为原料,采用水酶法提取油脂,在单因素试验基础上,采用响应面法研究木瓜蛋白酶用量、酶解时间、pH值、酶解温度和料液比对山核桃油提取率的影响;采用气相色谱-质谱联用技术分析提取油脂的脂肪酸组成,并对比了压榨法、溶剂法和水酶法3种方式对油脂理化性质的影响。结果表明,水酶法提取山核桃油脂工艺的最佳条件为:木瓜蛋白酶量0.17%,酶解时间150 min,pH值6.34,酶解温度54.43℃、料液比1∶5,在此条件下山核桃中油脂提取率为81.32%。采用气相色谱-质谱联用技术对提取油脂的脂肪酸组成进行分析,共测出12种脂肪酸,棕榈酸、油酸、亚油酸、亚麻酸是4种主要脂肪酸,其中饱和脂肪酸(SFA)占7.61%,单不饱和脂肪酸(MUFA)占69.10%,多不饱和脂肪酸(PUFA)占23.29%。对比3种提油方式发现,水酶法是一种较为理想的油脂提取方法。本研究结果为水酶法提取山核桃油脂生产提供了理论依据。     

Antioxidant activity of extracts of black sesame seed (Sesamum indicum L.) by supercritical carbon dioxide extraction

Antioxidant activities of extracts derived from sesame seed by supercritical carbon dioxide (SC-CO(2)) extraction and by n-hexane were determined using alpha,alpha-diphenyl-beta-picylhydrazyl (DPPH) radical scavenging and linoleic acid system methods. The highest extracted yield was given at 35 degrees C, 40 MPa, and a CO(2) flow rate of 2.5 mL min(-1) by an orthogonal experiment. The yields of extracts increased with increasing pressure, and yields at 40 and 30 MPa were higher than that by solvent extraction at 46.50%. Results from the linoleic acid system showed that the antioxidant activity follows the order: extract at 35 degrees C, 20 MPa > BHT > extract at 55 degrees C, 40 MPa > extract at 55 degrees C, 30 MPa > Trolox > solvent extraction > alpha-tocopherol. The SC-CO(2) extracts exhibited significantly higher antioxidant activities comparable to that by n-hexane extraction. The extracts at 30 MPa presented the highest antioxidant activities assessed in the DPPH method. At 20 MPa, the EC(50) increased with temperature, which indicated that the antioxidant activity was decreased in a temperature-dependent manner. The significant differences of antioxidant activities were found between the extracts by SC-CO(2) extraction and n-hexane. However, no significant differences were exhibited among the extracts by SC-CO(2) extraction. The vitamin E concentrations were also significantly higher in SC-CO(2) extracts than in n-hexane extracts, and its concentrations in extracts corresponded with the antioxidant activity of extracts.     

Pressurized fluids for extraction of cedarwood oil from Juniperus virginianna

The extraction of cedarwood oil (CWO) using liquid carbon dioxide (LC-CO(2)) was investigated and compared to supercritical fluid extraction, including the effects of extraction pressure and length of extraction. The chemical composition of the extracts was monitored over the course of the extraction as well. The cumulative yields of CWO from cedarwood chips using 80 L of carbon dioxide varied very little treatment to treatment, with all temperature/pressure combinations yielding between 3.55 and 3.88% CWO, and the cumulative yields were statistically equivalent. The rate of extraction was highest under the supercritical extraction conditions (i.e., 100 degrees C and 6000 psi). Under the liquid CO(2) conditions (i.e., 25 degrees C), the extraction rates did not vary significantly with extraction pressure. However, there were differences in the chemical composition of the collected CWO. Extractions at 100 degrees C gave a much lower ratio of cedrol/cedrene than extractions at 25 degrees C. The highest ratio of cedrol/cedrene was obtained using 25 degrees C and 1500 psi. The use of subcritical water was also investigated for the extraction of CWO as well. Although some CWO was extracted using this method, the temperature/pressure combinations that gave the highest weight percentage yields also gave oils with an off odor while those combinations that gave a higher quality oil had very low yields. It appears that the high temperatures and acidic conditions cause a dehydration of the tertiary alcohol, cedrol, to its hydrocarbon analogue, cedrene, during CO(2) or pressurized water extractions of cedarwood.