响应曲面法优化超临界CO2萃取猕猴桃籽油条件

以猕猴桃籽为试验原料,在单因素试验的基础上,采用响应曲面分析法建立了超临界CO2萃取猕猴桃籽油萃取率的二次多元回归方程,探讨了压力、温度、CO2流量等关键因素对萃取率的作用规律。结果表明,萃取压力、温度、CO2流量对萃取率影响显著,萃取压力和温度交互效应影响显著。根据萃取率回归方程对猕猴桃籽油的超临界萃取工艺参数进行了优选,最优工艺参数为:压力31.7 MPa,温度40.2℃,CO2流量27.4 kg/h,该条件下萃取率高达32.57%,与试验值31.24%仅有4.5%的误差,证实了该方程的预测值与试验值之间具有较好的拟合度。超临界CO2萃取的猕猴桃籽油与己烷提取的油脂在脂肪酸组成上没有显著差别。     

Optimization of Supercritical CO2 Extraction of Fish Oil from Viscera of African Catfish (Clarias gariepinus)

Fish oil was extracted from the viscera of African Catfish using supercritical carbon dioxide (SC-CO₂). A Central Composite Design of Response Surface methodology (RSM) was employed to optimize the SC-CO₂ extraction parameters. The oil yield (Y) as response variable was executed against the four independent variables, namely pressure, temperature, flow rate and soaking time. The oil yield varied with the linear, quadratic and interaction of pressure, temperature, flow rate and soaking time. Optimum points were observed within the variables of temperature from 35 °C to 80 °C, pressure from 10 MPa to 40 MPa, flow rate from 1 mL/min to 3 mL/min and soaking time from 1 h to 4 h. However, the extraction parameters were found to be optimized at temperature 57.5 °C, pressure 40 MPa, flow rate 2.0 mL/min and soaking time 2.5 h. At this optimized condition, the highest oil yields were found to be 67.0% (g oil/100 g sample on dry basis) in the viscera of catfish which was reasonable to the yields of 78.0% extracted using the Soxhlet method.     

超临界二氧化碳萃取葡萄籽油工艺优化

为了回收利用葡萄酒酿造过程产生的副产品中的有效成分,本文利用超临界CO₂萃取技术从葡萄籽中提取含有不饱和脂肪酸的葡萄籽油,意在考量超临界CO₂技术在萃取葡萄籽油方面的作用。设计单因素实验,研究了萃取压力、萃取温度、CO₂流量以及停留时间对葡萄籽油萃取率的影响。单因素实验结果表明萃取压力对萃取结果的影响最为显著。萃取温度和CO₂流量对萃取率的影响都存在最佳值,当温度和流量超过最佳值,萃取率开始降低。在单因素实验的基础上进行响应面实验,采用中心复合设计进行实验方案设计以优化萃取葡萄籽油工艺。对响应面实验结果进行方差分析,建立多元回归模型,模型P值<0.0001,预测超临界CO₂萃取葡萄籽油的最佳萃取条件为：萃取压力28MPa、萃取温度321 K、CO₂流量15.5L/h,停留时间155min,萃取率达到14.12%。     

Influence of operation variables on quality parameters of olive husk oil extracted with CO<Subscript>2</Subscript>: Three-step sequential extraction

Supercritical CO₂ extraction is a viable alternative process for the extraction of high-quality oil from olive husk (also known as olive pomace), a residue obtained in the production of olive oil. We analyzed the effect of pressure (100–300 bar), temperature (40–60°C), solvent flow (1–1.5 L/min), and particle size (0.30–0.55 mm) on four important quality parameters of the oil extracted with CO₂: tocopherol concentration, extinction coefficients at 232 and 270 nm, and saponification value. Response surface methodology was used to obtain mathematical expressions related to the operating variables and parameters studied. Results from these experiments were also used to design a three-step sequential CO₂ extraction procedure to obtain a higher-quality extract. The optimal operational sequence consisted of a first extraction step at 75 bar for 1 h using 1% (vol/vol) ethanol modifier, followed by a second extraction stage at 350 bar for 2.5 h without ethanol and a third step, also at 350 bar, for 2.5 h but using ethanol. These extraction conditions obtained an intermediate fraction of oil with 64% yield and all normal parameters according to European Commission food legislation. This fraction is suitable without any further refining. On the contrary, the oils obtained by hexane extraction and by conventional supercritical CO₂ extraction at optimal conditions are suitable for human consumption after further refining. This last finding may result in improved economics of the sequential CO₂ extraction process compared to the conventional extraction method with hexane.     

Influence of operating variables on yield and quality parameters of olive husk oil extracted with supercritical carbon dioxide

Supercritical fluid extraction is a viable alternative process for extracting oil from olive husk, a residue obtained in the olive oil production. We analyzed the effects of pressure (P) (100–300 bar), temperature (T) (40–60°C), solvent flow (1–1.5 L/min), and particle size (D) (0.30–0.55 mm) on extraction yield, and three oil-quality parameters: acidity (OA), PV, and phosphorus content (PC). A response surface methodology based on the statistical analysis of the experimental data permitted us to obtain mathematical expressions relating the operational variables and parameters studied. At the best extraction condition of the experimental range analyzed (P=300 bar, T=60°C, D=0.30 mm, and solvent flow=1.25 L/min at standard conditions), the oil yield was 80% (w/w) with respect to hexane extraction, whereas the quality parameters OA, PV, and PC were 14% (w/w), 8 meq/kg, and 2.3·10⁻³% (w/w), respectively. These results were compared to those obtained by hexane Soxhlet extraction. The quality of the supercritical extract was superior, requiring only simple refining. This advantage may result in improved economics of the supercritical process in relation to the conventional extraction with hexane.     

Fatty Acid Composition and Antioxidant Activity of Tea (Camellia sinensis L.) Seed Oil Extracted by Optimized Supercritical Carbon Dioxide

Seeds are another product in addition to leaves (raw materials for teas) of tea (Camellia sinensis L.) plant. The great increase of tea consumption in recent years raises the challenge of finding commercial applications for tea seeds. In the present study, supercritical carbon dioxide (SC-CO(2)) extraction edible oil from tea seed was carried out, response surface methodology (RSM) was used to optimize processing parameters including time (20-90 min), temperature (35-45 °C) and pressure (50-90 MPa). The fatty acid composition and antioxidant activity of the extracted oil was also investigated. The highest yield of oil (29.2 ± 0.6%) was obtained under optimal SC-CO(2) extraction conditions (45 °C, 89.7 min and 32 MPa, respectively), which was significantly higher (p < 0.05) than that (25.3 ± 1.0%) given by Soxhlet extraction. Meanwhile, tea seed oil extracted by SC-CO(2) contained approximately 80% unsaturated fatty acids and showed a much stronger scavenging ability on the DPPH radical than that extracted by Soxhlet. SC-CO(2) is a promising alternative for efficient extraction of edible oil from tea seed. Moreover, tea seed oil extracted by SC-CO(2) is highly edible and has good antioxidant activity, and therefore may play a potential role as a health-promoting food resource in human diets.     

Supercritical extraction of evening primrose oil: Experimental optimization via response surface methodology

Supercritical carbon dioxide (CO₂) effective extraction parameters (pressure, temperature, static extraction time, and dynamic extraction time) of oil recovery from evening primrose seeds were optimized via response surface methodology (RSM). The results of this study indicated that the linear terms of static and dynamic time and the quadratics of temperature and pressure, as well as the interactions of temperature and static time, pressure and temperature had a significant effect on the oil recovery. The optimum extraction conditions of 14.2 MPa, 47.3°C, 30 min (static extraction time) and 150 min (dynamic extraction time) were obtained. Applying the optimum conditions, a mean experimental recovery of 92.98% (triplicate experiment) was achieved, which is well compatible with the RSM‐predicted value (93.61%). The fatty acid composition of extracted evening primrose oil using supercritical CO₂ was compared with that obtained by Soxhlet method in which minor difference was observed. © 2011 American Institute of Chemical Engineers AIChE J, 2011     

超临界二氧化碳流体萃取油茶籽油及其GC／MS分析

采用环境友好的超临界二氧化碳流体萃取技术制备油茶籽油,考察了压力、时间、温度和二氧化碳流量等因素对茶籽油萃取率的影响,得到优化的工艺参数：当萃取压力30MPa、萃取温度35℃、CO2流量30L／h、萃取时间为3h时茶籽油萃取率可高达44．4％。根据中华人民共和国国家标准进行检测的结果表明：超临界二氧化碳流体萃取出的茶籽油,无需进一步精制即可达到国家食用植物油卫生标准GB／T2716—2005,而除含皂量、水分及挥发物外的指标均达到国家一级茶油标准GB11765—2003;GC／MS分析结果表明油茶籽油富含73．6％不饱和脂肪酸。实验结果表明：超临界二氧化碳流体技术萃取茶籽油具有操作简便、萃取率高、无溶剂残留、绿色环保等优点,萃取出的茶籽油具有较高的品质和良好的应用前景。     

Fatty acid composition,cytotoxicity and anti-inflammatory evaluation of melon (Cucumis melo L. Inodorus) seed oil extracted by supercritical carbon dioxide

ABSTRACT

Melon seed oil has been extracted by Soxhlet (hexane) and by supercritical CO₂ operating to various pressures and temperatures. Linoleic acid (67.06–68.22%) was the most abundant followed by oleic acid (21.63–22.45%), palmitic acid (5.57–6.23%) and stearic acid (2.98–3.67%). The highest inhibition of inflammation was 18.8% at 50 µg/mL for hexane and SC-CO₂ extracts obtained under 55 MPa and 70°C. The largest inhibition of IGROV and OVAR tumor cell lines were 29.9% and 21.6%, respectively, at 50 µg/mL for the ethanol extract. These results of biological activities indicate that melon seed oils can be dedicated to nutrition.     

超临界CO_2流体萃取植物油的实验研究

建立了一套超临界流体萃取实验装置,就大豆和花生两种植物油超临界流体萃取进行了较为详细的实验研究.在探讨了压力、温度、颗粒度、空隙率以及时间等对萃取率的影响之后,获得了指导实际生产的最佳工艺参数条件.     

超临界二氧化碳萃取葡萄籽油的研究

葡萄籽油中富含亚油酸和其它不饱和脂肪酸,具有较高的食用和药用价值。传统的葡萄籽油提取方法存在着收率低和溶剂残留的问题。今基于对酿酒过程中废弃葡萄籽的开发利用,探讨了采用绿色洁净分离技术——超临界流体萃取技术从废弃葡萄籽中萃取葡萄籽油的可行性,重点考察了萃取温度、萃取压力、CO2用量及不同原料对葡萄籽油产率的影响。研究表明萃取压力对产率的影响较温度显著,实验确定适宜工艺条件为萃取温度55C,萃取压力30MPa。此条件下以张裕酒厂提供的籽为原料所得产率为9.71%,同时气相色谱分析表明,葡萄籽油产品中含有72.05%的亚油酸。另外,分别以三种不同来源的葡萄籽为原料进行实验,研究显示,葡萄籽油产率随原料不同而存在一定差异,产率较高者可达13.51%。     

Development of green extraction process to produce antioxidant-rich extracts from purple coneflower

The present study was conducted to develop subcritical water extraction (SWE) of Echinacea purpurea flowers. The influence of temperature and extraction time on quality of extracts considering total phenols content, total flavonoids content, antioxidant capacity and extraction yield, was determined. Optimized extraction parameters for maximised investigated responses were as follows: 147.56 °C and 8.43 min. The experimental values agreed with the values predicted, thus indicating the adequacy of central composite experimental design for modelling the SWE of bioactive compounds from E. purpurea. Results of the study also highlighted the potential application of E. purpurea subcritical water extracts as a source of valuable bioactive compounds.     

Supercritical Carbon Dioxide Extraction of the Oak Silkworm (Antheraea pernyi) Pupal Oil: Process Optimization and Composition Determination

Supercritical carbon dioxide (SC-CO(2)) extraction of oil from oak silkworm pupae was performed in the present research. Response surface methodology (RSM) was applied to optimize the parameters of SC-CO(2) extraction, including extraction pressure, temperature, time and CO(2) flow rate on the yield of oak silkworm pupal oil (OSPO). The optimal extraction condition for oil yield within the experimental range of the variables researched was at 28.03 MPa, 1.83 h, 35.31 °C and 20.26 L/h as flow rate of CO(2). Under this condition, the oil yield was predicted to be 26.18%. The oak silkworm pupal oil contains eight fatty acids, and is rich in unsaturated fatty acids and α-linolenic acid (ALA), accounting for 77.29% and 34.27% in the total oil respectively.     

超临界流体萃取沙棘油实验研究

建立了一套萃取实验装置 ,对超临界CO2 流体萃取沙棘油进行了实验研究。压力 15— 30MPa,温度 30— 5 0℃。分别考察了萃取压力、萃取温度、颗粒度、物料填充量以及萃取时间等条件对萃取率的影响 ,并就工艺参数对萃取率的影响机理和原因进行了分析与讨论。结果表明 :当压力为 2 5MPa、温度为 40℃时可获得较高的萃取率。流量为 0 .2m3 /h时 ,萃取时间为 4— 5h。化学成分分析结果证明 :沙棘油中饱和脂肪酸含量占 12 .3%,不饱和脂肪酸含量占 87.7%。     

超声强化密相CO2萃取葵花籽油的研究

进行了超声强化密相CO2萃取葵花籽油的研究,探讨了萃取温度、压力、时间、CO2流速以及超声功率密度和频率对葵花籽油萃取率的影响.结果表明,附加20 kHz、100 W·L-1的超声波后,萃取压力、时间和CO2流速分别降低了5 MPa、0.5 h和0.5 L·h-1.超声对萃取的影响主要是由于超声的机械波动效应.采用了响应曲面法对超声强化萃取条件进行了优化,并得到优化后的萃取条件为:萃取温度28.3℃、压力28 MPa、时间178 min、CO2流速3.0 L·h-1、超声功率密度为100 W·L-1、超声频率为20 kHz.在优化条件下,UDCE与DCE相比能够提高19%的萃取率.     

碱蓬籽油脂的超临界CO_2提取工艺优化

碱蓬籽中油脂含量丰富,尤以不饱和脂肪酸甘油酯-亚油酸酯居多,使用超临界CO2提取碱蓬籽油,确定最佳的提取条件。以亚油酸酯得率为指标,考察了提取温度、提取压力、提取时间、夹带剂流量对实验的影响,在单因素的基础上,采用响应面法对工艺进行优化,得到的最佳提取条件为:提取温度46℃,提取压力23.5MPa,提取时间137min,夹带剂流量0.04m L·min-1,在此条件下亚油酸酯得率为15.29%。优化的提取工艺可行,对工业化生产有一定的指导意义。     

响应面优化淫羊藿抗氧化多酚超声提取工艺

以总多酚得率和DPPH自由基清除率为指标,采用响应面设计法优化淫羊藿抗氧化活性多酚超声提取工艺。结果表明以多酚得率为指标时,最佳工艺条件为：57％乙醇,料液比28 mL／g,在50℃下超声提取25 min,总多酚得率为34．58 mg／g;以DPPH自由基清除率为指标时,最佳工艺条件为：58％乙醇,料液比30 mL／g,在50℃下超声提取22 min, DPPH自由基清除率为88．4％。     

超临界二氧化碳萃取在石油工业中的应用

近年来,超临界二氧化碳萃取技术作为分析化学中一种新兴技术,迅速显示了其特有的效果和广泛的运用前景。文章介绍了超临界二氧化碳萃取的原理和特性,重点阐述其在油气开采和石油炼制研究领域的进展状况,并指出了该技术的发展方向。