Comparison of Constituents and Insecticidal Activities of Essential Oil from Artemisia lavandulaefolia by Steam Distillation and Supercritical-CO_2 Fluid Extraction

Essential oil was extracted from Artemisia lavandulaefolia DC.by steam distillation（SD） and supercritical-CO2 fluid extraction（SFE）,respectively.The constituents of the essentil oils extracted with those two methods were analyzed by gas chromatography-mass spectrometry（GC-MS） and insecticidal activities of the essential oils were evaluated,then the results were compared to assess their biological activity.Thirty-one compounds were identified in the essential oil extracted by SD,and its main components were eucalyptol,α,α,4-trimethyl-3-cyclohexene-1-methanol and so on.Twenty-two compounds were identified for the essential oil extracted by SFE,and its main components were cyclodecene,n-hexadecanoic acid and so on.Six chemical compositions were all contained in the essential oils extracted by the two methods,i.e.,eucalyptol,α,α,4-trimethyl-3-cyclohexene-1-methanol,caryophyllene,[3aS-（3aα,3bβ,4β,7α,7aS）]-octahydro-7-methyl-3-methylene-4-（1-methylethyl）-1H-cyclopenta[1,3]cyclopropa-[1,2]benzene,nerolidol and（-）-Spathulenol.The fumigation toxicity of the essential oil obtained by means of SD to the adults of Sitophilus zeamais is significantly higher than that of the essential oil by means of SFE.The contact toxicity of the essential oil obtained by means of SFE to the adults of S.zeamais is higher than that of the essential oil obtained by means of SD,but the difference is not significant.

Quality of Canola Oil Obtained by Conventional and Supercritical Fluid Extraction

Quality of canola oil obtained by the supercritical fluid extraction (SFE), using CO2 with ethanol as a co-solvent, was evaluated and compared to that of the conventionally-obtained oils using either n-hexane or chloroform methanol mixture. Physical characteristics, chemical properties, fatty acid composition and phenolic profile of oils were investigated. The SFE oil showed significantly lower melting point, peroxide value (PV) and higher free fatty acids (FFAs) and iodine value (IV) than the n-hexane-extracted one. There were no significant differences in the fatty acid composition of different oils. The SFE oil showed significantly higher phenolic content (35.91, 10.15, 3.16, 0.32 and47.48mg/g of sinapic acid, sinapine, sinapoyl glucose, canolol and total phenolics) as compared to 0.08, 0.70, 0.88, 0.45 and0.71mg/g, respectively in the n-hexane-extracted oil. These results indicate the superiority of SFE and advocate its use for the extraction of highly stable and functional canola oil for further health and nutraceutical uses. The present results have an industrial and technological relevance as SFE could be competitive with the traditional extraction techniques providing an environmental approach and enhancing the obtained oil quality and stability. After recovery of the initial installation costs, SFE could be more economic than conventional extraction. However, further economical studies are needed to validate this last conclusion.

Supercritical fluid extraction of essential oil from the fruits of Bupleurum chinense DC. and their characterization by GC/MS

Objective:Aim To analyze the chemical constituents of essential oil from the fruits of Bupleurum chinense DC.Methods:Essential oil from the fruits of Bupleurum chinense DC.was extracted by using supercritical fluid extraction (SFE),and the chemical constituents to be identified by GC/MS spectrum.Results:The yield of essential oil from the fruits of Bupleurum chinense DC.by SFE was 6.60%(V/W)and 73 components were identified in this oil.Conclusions:The essential oil from the fruits of Bupleurum chinense DC.was produced for the first time,and its yield was 3 times more than its root,the relative contents of linoleic acid,cetyl acetate,ethyl linoleate,(-)-caryophyllene oxide are 34.85%,16.63%,2.64%,1.81% apart in this essential oil.Phytol,cetyl acetate,ethyl linoleate,(-)-caryophyllene oxide were confirmed for the first time from the genus of Bupleurum.

A Comparative Study on Hemp(Cannabis sativa)Essential Oil Extraction Using Traditional and Advanced Techniques

A comparative study of Cannabis sativa(Hemp)essential constituents obtained by using Supercritical Fluid Extraction(SCFE),Steam Distillation(SD)and Hydrodistillation(HD)is presented here.The optimized extraction temperatures were 130,110and 50℃for hydrodistillation,steam distillation and supercritical fluid extraction respectively.The essential oil of C.sativa was analyzed by using Gas chromatography mass spectrometry(GC-MS).A total of 33,30and 31components have been identified in HD,SD and SCFE respectively.Yield of essential oil using SCFE(0.039%)was more than HD(0.025%)and SD(0.035%)extraction respectively.The main component of sesquiterpenes obtained by hydrodistillation at 130℃with their percentages included caryophyllene(40.58%),trans-α-bergamotene(5.41%),humulene(10.97%),cis-β-farnesene(8.53%)and monoterpenes includedα-pinene(2.13%),d-limonene(6.46%),p-cymol(0.65%)and cineole(2.58%)respectively.The main component of sesquiterpenes obtained by SD steam distillation at110℃including caryophyllene(38.60%)trans-α-bergamotene(4.22%),humulene(10.26%),cis-β-farnesene(6.67%)and monoterpenes includedα-pinene(3.21%),d-limonene(7.07%),p-cymol(2.59%)and cineole(3.88%)whereas the more percentages of major components were obtained by SCFE at 50℃included caryophyllene(44.31%),trans-α-bergamotene(6.79%),humulene(11.97%)cis-β-farnesene(9.71%)and monoterpenes includedα-pinene(0.45%),d-limonene(2.13%)p-cymol(0.19%)and cineole(1.38%)respectively.We found yield/efficiency,chemical composition,quality of the essential oils by supercritical fluid extraction superior in terms of modern,green,saving energy and a rapid approach as compared to traditional techniques.

Essential Oil from Inula britannica Extraction with SF-CO_2 and Its Antifungal Activity

The aim of this study was to determine the extraction technique of supercritical fluid carbon dioxide（SF-CO 2） for the essential oil from Inula britannica flowers and its antifungal activities against plant pathogenic fungi for its potential application as botanical fungicide.The effects of factors,including extraction temperature,extraction pressure,SF-CO 2 flow rate,flower powder size,and time on the essential oil yield were studied using the single factor experiment.An orthogonal experiment was conducted to determine the best operating conditions for the maximum extraction oil yield.Adopting the optimum conditions,the maximum yield reached 10.01% at 40°C temperature,30 MPa pressure,60 mesh flower powder size,20 L h-1SF-CO 2 flow rate,and 90 min extraction time.The antifungal activities of I.britannica essential oil using the SF-CO 2 against the most important plant pathogenic fungi were also examined through in vitro and in vivo tests.Sixteen plant pathogenic fungi were inhibited to varying degrees at 1 mg mL-1concentration of the essential oil.The mycelial growth of Gaeumannomyces graminis var.tritici was completely inhibited.The radial growths of Phytophthora capsici and Fusarium monilifome were also inhibited by 83.76 and 64.69%,respectively.In addition,the essential oil can inhibit the spore germination of Fusarium oxysporum f.sp.vasinfectum,Phytophthora capsici,Colletotrichum orbiculare,and Pyricularia grisea,and the corresponding inhibition rates were 98.26,96.54,87.89,and 87.35% respectively.The present study has demonstrated that the essential oil of I.britannica flowers extracted through the SF-CO 2 technique is one potential and promising antifungal agent that can be used as botanical fungicide to protect crops.

Comparative study on yields and quality parameters of argan oils extracted by conventional and green extraction techniques

Argan oil is most frequently sold as pure oil,which can be directly applied topically due to its cosmetological proprieties or ingested in order to provide several health benefits.It's also commonly mixed into a number of cosmetic products like shampoos,soaps and conditioners.In this study we aimed to improve the argan oil extraction yield and quality parameters by comparing the effects of different extraction technologies.Argan kernel oils were extracted using four methods:mechanical cold press,Soxhlet extraction with n-hexane,supercritical fluid extraction(SFE),and enzyme assisted extraction with three different enzyme solutions cellulase(cellulast),pectinase(Pectinex)and a mixture of carbohydrase enzymes(Viscozyme®).The quality parameters was evaluated by determining the acid,peroxide and iodine values aswell as the extinction coefficients K_(232) and K_(270) as measures of conjugated dienes and trienes,respectively.The results showed that the highest yield(66.37%±3.3%)was obtained by enzyme assisted extraction using the carbohydrases enzymes mixture(Viscozyme®),followed by Soxhlet extraction(59.5%±3.1%)and pectinase extraction(52.03%±3.55%).All argan oils samples obtained by the different methods showed a good oxidation stability,with acid,peroxide and iodine values lower than 0.8 mg/g,15 meq/kg and 110 g/100 g according to the official argan oil norm,respectively.The results of argan oils quality parameters demonstrated that the enzyme extracted argan oils showed low oxidation,with the following quality parameters:acid values(0.4-0.6 mg/g),iodine values(95-100 g/100 g),dienes(K_(232)<2),trienes(K_(270)<0.35),and peroxide values(<1.5 meq/kg).The results proved that the enzyme assisted extraction method can be applied to improve the argan oil yield without affecting the oil quality.The enzyme extraction method may be a great alternative to solvent and cold press extractions for this eco-friendly processing approach.

超临界萃取结合分子蒸馏纯化生姜精油及其挥发性成分分析

为研究超临界萃取结合分子蒸馏纯化生姜精油的最佳工艺参数,鉴定生姜精油的挥发性成分,以舒城黄姜为原料,通过单因素试验和正交试验优化了超临界CO_(2)流体萃取(supercritical CO_(2)fluid extraction,SFE)生姜油的最佳工艺条件,考察了分子蒸馏(molecular distillation,MD)温度对分离纯化生姜精油效果的影响,并通过气相色谱-质谱联用对生姜精油的挥发性成分进行了分析。结果表明,超临界CO_(2)流体萃取结合分子蒸馏(SFE-MD)纯化生姜精油的最佳工艺条件为萃取压力24 MPa、萃取温度45℃、萃取时间2 h、分子蒸馏温度80℃,在此条件下,生姜精油的综合得率为2.53%,显著高于水蒸气蒸馏精油得率0.96%(P<0.05)。挥发性成分分析显示,α-姜烯、β-倍半水芹烯、β-红没药烯是生姜精油的主要挥发性成分,百分含量达70%以上,其中α-姜烯百分含量为42.13%,高于水蒸气蒸馏生姜精油α-姜烯百分含量40.59%。该方法绿色环保,萃取率高,精油品质好,为生姜精油的进一步研究开发提供参考。

三种柑橘类精油的GC-MS分析及抑菌活性对比

选取陈皮、柠檬和金桔这三种柑橘类植物为原料,利用超临界CO_(2)萃取法高效提取精油。采用GC-MS分析样品成分,进而探究三种精油对金黄色葡萄球菌和烟曲霉菌的抑菌活性。研究表明:柠檬精油中的醇类(3.41%)、醛类(2.55%)、酮类(2.03%)、酯类(7.17%)和除柠檬烯以外的萜烯类化合物(34.06%)含量较高,D-柠檬烯含量是这三种精油中最低的(46.52%);陈皮精油中的萜烯类(86.34%)、酚类化合物(1.82%)含量较高;金桔精油中的酸类化合物(12.71%)和D-柠檬烯(72.69%)含量较高。精油对金黄色葡萄球菌和烟曲霉菌的抑菌活性均为柠檬精油>陈皮精油>金桔精油。在这三种柑橘类精油中D-柠檬烯并非是唯一的抑菌成分,精油的抑菌活性也与除D-柠檬烯以外的抑菌成分密切相关。其中柠檬精油中含量丰富的γ-松油烯和β-蒎烯等其他抑菌成分可与D-柠檬烯协同起到有效提高精油抑菌活性的作用。该方法所提取的精油可为相关天然抑菌产品研发提供一定帮助。

不同加工方式的南瓜籽油的储藏稳定性研究

为探究南瓜籽油的储藏稳定性,对比冷榨(cold pressing,CP)、微波预处理-压榨(microwave pretreatmentpressing,MP)、超临界二氧化碳萃取(supercritical fluid extraction,SFE)3种加工方式制得的南瓜籽油在储藏过程中理化性质、油脂伴随物含量和自由基清除能力的变化。结果表明:室温储藏90 d,SFE南瓜籽油酸价、CP南瓜籽油过氧化值变化最大,分别提高了91.64%和171.74%,p-茴香胺值变化不大;MP南瓜籽油总酚、CP南瓜籽油总甾醇和生育酚损失率最大。MP南瓜籽DPPH和ABTS^(+)自由基清除能力均下降最多。加速氧化储藏28 d,CP南瓜籽油酸价、过氧化值、p-茴香胺值的增幅最显著,MP南瓜籽油的总酚损失大,3种工艺南瓜籽油甾醇减少的比例相差不大。CP南瓜籽自由基清除能力下降最多,DPPH和ABTS^(+)自由基清除能力分别下降了38.48%和50.67%。加速氧化过程中SFE南瓜籽油的稳定性优于CP和MP南瓜籽油。

Study of Oil/Water Interfacial Tension of Vacuum Residual Fractions from Iranian Light Crude Oil

The vacuum residual from Iranian Light crude oil are separated into a series of 16 narrow fractions according to the molecular weight by the supercritical fluid extraction and fractional (SFEF) technology. The chemical element and the UV spectrum of each fraction are analyzed. The effects of several factors on the interfacial tension are investigated, which are the fraction concentration in oil phase, the ratio of oil component, the salts dissolved in the water phase and the pH value. The interfacial tension decreases rapidly as the concentration of the residual fraction in the oil increases, showing a higher interfacial activity of the fraction. The interfacial tension changes, as the amount of absorption or the state of the fractions in the interface changes resulting from different ratios of oil, different kinds or concentrations of salts in water, and different pH values. It is concluded that the intrfacial tension changes regularly, corresponding to the regular molecular parameters of the vacuum residual fractions.

Sustainable oil-in-water analysis using a supercritical fluid carbon dioxide extraction system directly interfaced with infrared spectroscopy

A direct aqueous supercritical fluid extraction （SFE） system using carbon dioxide provides a sustainable means by which a vast range of industries may continue to depend on well established infrared （IR） techniques to determine oil-in-water. The SFE-IR method provides an environmentally friendly substitute for current national standard IR reference methods for measuring oil-in-water that rely on using increasingly restricted ozone depleting solvents whose manufacture is being phased out in accordance with international law. The SFE-IR analysis of a 500 mL water sample can be accomplished in 15 min. A rapid on-line SFE-IR calibration method has been implemented. With this calibration method, SFE-IR accuracy for determining diesel oil in 500 mL spiked water samples using single wave number measurement was 86.0%-98.8% with precision （RSD） ranging from 2.5%-7.0%. Using a general purpose calculation which involves measuring infrared absorbance values at three different wave numbers, SFE-IR method accuracy for determining diesel oil in 500 mL spiked water samples was 83.7%-92.2% with RSD 1.0%-9.3%. Data is presented that indicates current long established national standard IR reference methods involving three wave number calculations should be reviewed since, without careful consideration, the inclusion of calculated aromatic hydrocarbon species contributions to final oil-in-water concentration values may provide less accurate results.

不同提取工艺下海黄牡丹精油组分及其抗氧化活性的比较

【目的】分析不同提取工艺下海黄牡丹鲜花和烘干花瓣精油的化学成分及其体外抗氧化活性的差异,为海黄牡丹精油的综合利用与深度开发提供参考依据。【方法】采用同时蒸馏提取(SDE)法和超临界CO_(2)萃取(SFE)法分别提取海黄牡丹新鲜和烘干花瓣精油,利用气质联用技术(GC-MS)对精油成分进行分析,测定不同质量浓度精油对DPPH和ABTS自由基的清除率及其总抗氧化能力,并测定精油中生物活性成分总酚和总黄酮含量。【结果】采用SFE法提取的海黄牡丹精油得率明显高于SDE法,用SFE法从新鲜花瓣中提取精油得率最高,为0.76%。从2种不同方法提取的海黄牡丹鲜花和干花精油中检测到了108种化合物,其中SFE法提取的鲜花瓣精油中有41种、烘干花瓣精油中有52种,SDE法提取的鲜花瓣精油中有33种、烘干花瓣精油中有13种,植酮、正十九烷、正二十一烷3种主要成分在4种精油中同时存在。不同方式提取的海黄牡丹花精油中化合物成分主要有烷类、醇类、烯类、酮类、酯类、醛类、酸类、酚类和其他共9类化合物,其中烷类和醇类化合物的数量和含量显著高于其他类别化合物。不同方式提取的海黄牡丹精油对DPPH和ABTS自由基均具有一定的抗氧化清除活性,并且也具有一定的抗氧化能力,表现出SFE法提取的精油清除率高于SDE法,从新鲜花瓣中提取的精油清除率高于烘干花瓣。SFE法提取的新鲜花瓣精油中总酚含量最高,SDE法提取的烘干花瓣精油中总酚含量最低;总黄酮含量以SFE法提取的烘干花瓣精油中最高,SDE法提取的烘干花瓣精油中最低。【结论】不同方法提取的海黄牡丹鲜花和烘干花瓣精油的得率和化合物组成存在一定差异,SFE法提取的新鲜花瓣精油在体外的抗氧化活性优于其他提取方式。

超临界萃取结合分子蒸馏提取苍山冷杉油及其成分分析

研究超临界萃取结合分子蒸馏提取苍山冷杉油得率的影响及成分变化。采用单因素结合正交实验优化了超临界萃取工艺,并利用分子蒸馏对提取精油进行分离纯化,GC/MS对苍山冷杉松针和所得精油进行成分分析。超临界萃取苍山冷杉油最佳工艺条件为萃取压力34 MPa,萃取温度为45℃,CO_(2)流量20 L·h^(-1),萃取时间90 min;分子蒸馏对超临界萃取获得苍山冷杉油进行分离纯化,苍山冷杉油得率为1.42%;相比水蒸气蒸馏提取,超临界萃取结合分子蒸馏提取获得精油得率提高了2.16倍,分离纯化后精油颜色为无色液体;GC/MS结果显示,超临界萃取结合分子蒸馏提取获得精油与苍山冷杉松针所包含主要成分接近,而水蒸气蒸馏所得精油组分与苍山冷杉松针所含主要组分差别较大。

滇红玫瑰精油超临界CO_(2)萃取工艺、挥发性成分及抗氧化活性研究

目的:综合利用云产滇红玫瑰花资源,提高产品附加值。方法:以玫瑰花精油得率为判别指标,通过单因素试验和响应面试验优化超临界CO_(2)萃取玫瑰花精油的提取工艺;通过气相色谱—质谱技术分析不同精油的成分及相对含量,并评价不同玫瑰精油的抗氧化活性。结果:超临界CO_(2)萃取玫瑰花精油的最佳工艺参数为:玫瑰花粉末颗粒40目,萃取压力25.5 MPa、萃取温度45.5℃、萃取时间123 min,CO_(2)流量20 L/h,该工艺条件下玫瑰花精油得率为1.185%;不同产地滇红玫瑰精油中共鉴定出74种挥发性成分,安宁产的滇红玫瑰花精油挥发性物质总量最高;不同产地滇红玫瑰花精油均具有较好的自由基清除能力,但不同产地的抗氧化能力存在明显差异。结论:超临界CO_(2)萃取的滇红玫瑰花精油品质较好,可作为一种天然抗氧化剂应用。

3种茉莉花净油化学成分及其抗氧化活性

采用超临界流体萃取法(supercritical fluid extraction,SFE)对云南种植的3个品种茉莉花进行净油提取。通过气相色谱质谱联用技术(gas chromatography-mass spectrometry,GC-MS)研究不同品种茉莉花净油挥发性成分和相对含量的差异,并采用DPPH法和ABTS法评价不同品种茉莉花净油的抗氧化特性。结果表明:3个品种的茉莉花净油萃取得率、外观、香气、化学成分和抗氧化活性均有一定差异,从净油中共鉴定出98种化合物,共有成分有49种;从单瓣茉莉花净油中鉴定出84种化合物,双瓣茉莉花净油中鉴定出56种,多瓣茉莉花净油中鉴定出82种;3个品种净油中相对含量最多的为酯类化合物,不同种类致香物质的数量和相对含量差异明显;3种茉莉花净油都具有较好的自由基清除能力,但抗氧化活性有一定差异,双瓣茉莉净油的抗氧化能力明显高于其他两个品种。

Extraction Technology of Chinese-fir Heartwood by Supercritical Fluid Carbon Dioxide

Taking extraction rate as an indicator,the extraction technology of Chinese-fir heartwood by supercritical carbon dioxide treatment was studied, and the extraction rate of the SFE-CO2 method was compared to that of traditional extraction method. The results show that when extraction processing condition were:extraction pressure 30 MPa,extraction temperature 40℃,extraction time 120 m,and flow velocity 20 kg/h,the extraction rate of SFE-CO2 was 0.99%,0.20%more than that of the traditional extraction method.However,taking the cost into consideration,it is proposed that the traditional extraction is used unless there are specific requirements.

超临界流体萃取气相色谱法测定鱼肉中的毒死蜱残留

建立了利用离线超临界CO2萃取气相色谱(SFE-GC)测定鱼肌肉中毒死蜱残留量的分析方法.超临界CO2萃取鱼肌肉中毒死蜱的适宜条件为: 温度100℃,压力41.370 MPa,CO2流量为1 mL/min,动态萃取30 min,静态萃取时间15 min,调节剂甲醇(添加量0.5 mL),收集液丙酮.最小检出量为0.01 ng;添加回收率为77.3%～105.1%;相对标准偏差(RSD)为2.4%～15.4%,符合残留分析要求.全程分析时间小于2 h.

CO_2超临界流体萃取技术提取甜橙皮精油的研究

采用甜橙皮作为实验材料，研究在超临界状态下，粉碎度、温度、压力、静态萃取与动态萃取对油脂萃取率的影响，为批量生产提供了依据。

超临界CO_2萃取技术在油脂和脂肪酸分离中的应用

综述了超临界CO2 萃取分离油脂、脂肪酸的研究进展 ,讨论了影响萃取效果的主要因素 ,指出可通过在体系转变压力下、温度略高于溶剂临界温度的操作条件范围内寻找最优操作条件 。

小麦胚芽VE营养油制备方法的比较研究

本课题对不同方法直接萃取小麦胚芽油及用超临界CO2流体精馏麦胚油的方法进行了比较研究。结果表明:用乙醚提取的小麦胚芽油中维生素E的含量比用乙醇(90%)提取的要高;用超临界CO2萃取在压力为33MPa,温度为45℃时有最高的维生素E含量;用超临界CO2精馏在压力为19MPa,温差为△t=9℃时有较好的维生素E浓集效果。