Microscale recovery of total lipids from fish tissue by accelerated solvent extraction

A number of techniques are available for the extraction of lipids from a variety of tissues; however, conventional methods are characteristically labor intensive, typically involve large volumes of toxic solvents, and usually require at least 1 g of tissue. With the availability of accelerated solvent extraction (ASE) technology, the opportunity exists to modify classical lipid extraction techniques such that automated high-pressure, high-temperature extractions may be performed with the use of far smaller volumes of costly and harmsul solvents. Moreover, the high extraction efficiency attainable by ASE suggests that significantly less tissue would be required than is routinely used. This paper describes the adaptation of previously developed lipid extraction solvent systems for use with ASE toward the purpose of extracting total lipids from 100 mg of fish tissue. The efficacy of three solvent systems for lipid extraction from representative fish tissues, including a standard reference material, was explored using gravimetry and FA analysis by GC. A TG was used as a surrogate to monitor overall method performance. The findings herein demonstrate that microscale ASE represents an effective and efficient alternative to traditional lipid extraction techniques based on quantity and composition of extracted lipid, surrogate recovery, and precision.     

驱油用石油磺酸盐中无机盐含量分析新方法——梯度索氏浸提法

根据"相似相溶"原理,采用梯度索氏浸提法定量分析了石油磺酸盐工业品中无机盐含量。主要讨论了梯度浸提所需溶剂种类和用量、溶剂对各组分浸提效果、以及各组分浸提完全时所需浸提时间和循环次数,并与直接滴定法和SY/T6424-2000行业标准方法进行了比较。实验结果表明,应按照极性递增顺序选用系列有机溶剂在其沸点对石油磺酸盐进行索式浸提;未磺化油经2次浸提后总回收率可达100%;石油磺酸盐经4次浸提后总回收率可达99.86%,无机盐不被有机溶剂浸提,回收率100%。溶剂用量应确保提取管中样品被浸没。分析时间取决于样品用量,约6~7 h可浸提完全。无机盐含量分析结果小于上述2种方法,无机盐纯净,准确度高。该方法具有操作简单、不需昂贵的分析试剂和仪器、溶剂可重复回收利用等优点。     

An extrapolation procedure for determining solubilities of mixtures

Summary Successive extractions of mixtures are used to determine the percentage of the more soluble components present. A plot of the amount extractedvs. the extraction number results in a section of a hyperbola, which is then extrapolated to the limiting value. The solubility thus obtained is independent of arbitrary ratios of weights of solute to solvent. The method is applied to the determination of the alcohol-soluble fraction of sugar cane wax, and a laboratory extractor operating at constant temperature is described. Also the method may be used to analyze other extraction data,e.g., extraction with the Soxhlet extractor, to determine the amount of soluble material left unextracted after a given time.     

Effect of various extraction conditions on the phenolic contents of pomegranate seed oil

Pomegranate seeds are byproducts of the pomegranate juice industry. Because of the presence of large amounts of certain pharmaceutical and nutraceutical components in the seeds, a proper extraction method to obtain these components is highly demanded in the food industry. In this study, the effect of different extraction methods on the total phenolic contents of the oil extracted from pomegranate seeds of the Malas variety from Shahreza, Iran, was investigated. Four different extraction methods including normal stirring, Soxhlet, microwave irradiation and ultrasonic irradiation using two types of organic solvents as well as a supercritical fluid extraction (SFE) method using CO₂ as solvent were applied. The different organic solvents of this study did not indicate any significant differences in the total phenolic contents of the extracted oils, but the extracted oils from the various conditions of SFE indicated wide changes in the amount of phenolic compounds (7.8–72.1 mg/g). The total phenolic content of the extracted oil from one of the SFE runs was several times greater than those in the extracted oils using organic solvents.     

Advances in Lipid Extraction Methods—A Review

Extraction of lipids from biological tissues is a crucial step in lipid analysis. The selection of appropriate solvent is the most critical factor in the efficient extraction of lipids. A mixture of polar (to disrupt the protein-lipid complexes) and nonpolar (to dissolve the neutral lipids) solvents are precisely selected to extract lipids efficiently. In addition, the disintegration of complex and rigid cell-wall of plants, fungi, and microalgal cells by various mechanical, chemical, and enzymatic treatments facilitate the solvent penetration and extraction of lipids. This review discusses the chloroform/methanol-based classical lipid extraction methods and modern modifications of these methods in terms of using healthy and environmentally safe solvents and rapid single-step extraction. At the same time, some adaptations were made to recover the specific lipids. In addition, the high throughput lipid extraction methodologies used for liquid chromatography-mass spectrometry (LC-MS)-based plant and animal lipidomics were discussed. The advantages and disadvantages of various pretreatments and extraction methods were also illustrated. Moreover, the emerging green solvents-based lipid extraction method, including supercritical CO₂ extraction (SCE), is also discussed.     

铁观音绿茶茶多酚提取工艺研究

将有机溶剂提取法这一技术应用于提取绿茶的有效成分---茶多酚.采用正交实验法优化茶多酚的最佳提取条件,选择浸提温度、浸提次数、浸取时间和有机溶剂的浓度作为考察因素,以茶多酚的提取率为评价指标,通过单因素试验的考察,每个因素选取4个水平.得出最佳的提取工艺为:温度65℃,洗提次数3次,有机溶剂提取时间35 min,有机溶剂浓度55%.在这种条件下从绿茶中提取的茶多酚的收率为最高.并采用红外波谱法对提取出的产品进行定性分析,检测得出绿茶提取物的主要成分为茶多酚.     

Alternative hydrocarbon solvents for cottonseed extraction

Hexane has been used for decades to extract edible oil from cottonseed. However, due to increased regulations affecting hexane because of the 1990 Clean Air Act and potential health risks, the oil-extraction industry urgently needs alternative hydrocarbon solvents to replace hexane. Five solvents,n-heptane, isohexane, neohexane, cyclohexane, and cylopentane, were compared with commercial hexane using a benchscale extractor. The extractions were done with a solvent to cottonseed flake ratio of 5.5 to 1 (w/w) and a miscella recycle flow rate of 36 mL/min/sq cm (9 gal/min/sq ft) at a temperature of 10 to 45°C below the boiling point of the solvent. After a 10-min single-stage extraction, commercial hexane removed 100% of the oil from the flakes at 55°C; heptane extracted 100% at 75°C and 95.9% at 55°C; isohexane extracted 93.1% at 45°C; while cyclopentane, cyclohexane, and neohexane removed 93.3, 89.4, and 89.6% at 35, 55, and 35°C, respectively. Each solvent removed gossypol from cottonseed flakes at a different rate, with cyclopentane being most and neohexane least effective. Based on the bench-scale extraction results and the availability of these candidate solvents, heptane and isohexane are the alternative hydrocarbon solvents most likely to replace hexane. Presented in part at the AOCS Annual Meeting & Expo, Atlanta, Georgia, May 1994.     

Effect of the extraction solvent polarity on the sesame seeds oil composition

This study highlights the effect of solvent polarity on the yield (Y%) and properties of oil extracted from Algerian sesame seeds. Extractions were carried out under Soxhlet conditions with the following solvents: hexane (Hx), ethanol (Eth), acetone (Ac), dichloromethane (Di), isopropanol (Iso), hexane:isopropanol (Hx:Iso), and chloroform:methanol (Chf:Me). The sesame oil yield obtained using different solvents ranged from 28.86 to 52.83%. Fatty acids and sterols analyses were performed by GC on capillary column. γ‐Tocopherol was the major tocochromanol compound detected by HPLC‐fluorescence. Fourteen fatty acids were identified, with the predominance of oleic and linoleic acids. The main sterol in sesame oil was β‐sitosterol, followed by stigmasterol, campesterol, and Δ⁵‐avenasterol which were present in lower concentrations. High correlations were found between arachidic, gadoleic, behenic, and lignoceric acids concentrations; these results were explained by the metabolic biosynthesis pathway of the biologically active long‐chain PUFA by successive elongation and desaturation. Principal component analysis (PCA) of the data obtained from sesame oil composition enabled an easy comparison of the different extraction solvents, and correlated their properties with the most characteristic components of the extracted oils with a view to understand solvent–oil interaction, and to establish the effects of extracting solvent on such oil composition. Practical applications: This study showed that the choice of solvent depends largely on the desired fraction to be extracted. Sesame oil was better extracted with less‐polar solvents but membrane‐associated lipids are more polar and require polar solvents capable of breaking hydrogen bonds or electrostatic forces. Owing to the differences in solvent capacity, the fatty acids, sterols, and tocopherols extracted along with the oil vary, leading to differences in the quality of the extracted oil. The results obtained in this study could be applied in industrial extraction to encourage the use of alternative extraction solvents.     

Extraction of El-Lajjun Oil Shale

Abstract

Extraction of the bitumen fraction of El-Lajjun oil shale was carried out using 17 different solvents, pure and combined. Out of all the solvents used, toluene and chloroform were found to be the most efficient for extraction of the bitumen to perform the major part of the experiments. This selectivity was based on the quality and quantity of the yield and on the quantity of solvent recovered. Extraction was carried out using a Soxhlet extractor. For complete recovery of solvent the extract phase was subjected to two stages of distillation, simple distillation followed by fractional distillation, where different cuts of oil were obtained. It was found that an optimum shale size of 1.0 mm offered better solvent recovery. One hour was the optimum time needed for complete extraction. The yield of oil was determined from the material balance gained from fractional distillation after testing for the existence of any traces of solvent trapped in the different cuts by using a gas chromotography technique. When chloroform was used, it was found that the average amount of bitumen extracted was 0.037 g/g of shale, which corresponds to 98% of the actual bitumen trapped in the oil shale (by assuming the bitumen represents 15% of the organic matter) and 84.1% of solvent recovered. When toluene was used, it was found that the average amount of oil extracted was 0.0293 g/g of shale, which corresponds to 78% of the actual bitumen trapped in the oil shale (by assuming bitumen represents 15% of the organic matter) and 89.9% of solvent for extraction with toluene.     

逐层组装多层膜对苝的固相萃取性能研究

利用聚电解质逐层自组装技术在氨基硅胶表面构筑聚(乙烯-alt-马来酸)的苯乙胺衍生物(PEMAPEA)/聚烯丙基胺盐酸盐(PAH)多层膜,制备性能稳定的新型固相萃取吸附材料。利用HPLC-UV/Vis检测,研究其对水体中苝的萃取性能,考察柱填料量、样品量、上样流速、洗脱溶剂等对多层膜萃取性能的影响。结果表明:含150 mg固相萃取填料的3 mL萃取小柱,以10 mL·min-1的流速萃取200 mL苝的水溶液,用丙酮作洗脱剂,萃取回收率达到90%以上。     

乙醇回流法提取葡萄渣总黄酮化合物的工艺研究

对葡萄渣中的总黄酮的含量和提取工艺进行了研究,通过单因素试验和正交实验得出乙醇回流法提取的最佳工艺为:乙醇浓度80%,温度65℃,固液比1:50(g:mL),提取时间105 min,提取次数为2次,提取的黄酮含量为54.42 mg/g。     

Solvent Extraction: Kinetic Study of Major and Minor Compounds

The effects of temperature and contact time on lipid extraction from sunflower collets was investigated in a batch extractor with hexane as solvent. The total removed material varied in quantity and composition due to changes in temperature and contact time. Higher temperatures enhanced oil extraction as well as increased the tocopherol and phospholipid contents of the oil. The kinetic data for triglycerols, phospholipid and tocopherols extraction were interpreted by using an equation that considers extraction as the sum of two components: diffusion and washing. Effective diffusion coefficients for oil, tocopherols and phospholipid at different temperatures were determined. Control of temperature and contact time are essential to obtain good quality oil and reduce refining costs. Extraction at 60 °C and short contact times (30 min) obtained high oil yield (98%) accompanied by significant tocopherol extraction (>99%) and reduced phospholipid extraction (66%).     

Solvent degradation during coal liquefaction in a flowing-solvent reactor

We have previously observed that primary coal extracts recovered from the flowing solvent reactor appeared to be of large molecular mass. Short residence times in the reaction zone following the solubilisation of the extracts tended to limit their thermal degradation. This observation offered the vista of detailed characterisation and analysis of most (∼80-90%) of the coal mass in solution-and in a state relatively free of thermal degradation. Point of Ayr coal was extracted with tetralin and with non-donor solvents, quinoline and NMP at 350 and 450 °C. Structural evaluations have been carried out using size exclusion chromatography, UV-fluorescence spectrometry, GC-MS and probe-MS. Little coal derived material could be found in the pentane-soluble part of the reaction mixture; solvent dimers and trimers were prominent and coal-derived components, such as alkanes, were only minor components. In attempting to characterise the main, pentane-insoluble fraction of the coal extract, the level of interference from solvent-derived material emerged as the decisive parameter for the success or failure of the general method. However, the predominantly pentane-insoluble coal extracts from each solvent were contaminated by solvent polymerisation products. For all three solvents, the level of contamination of extracts with solvent derived material tended to interfere with the detailed characterisation/analysis of material extracted from the coal.     

超声波乙醇提取葡萄渣中总黄酮的工艺研究

以葡萄渣为原料,探讨超声波乙醇浸提法提取葡萄渣中总黄酮的实验条件,通过单因素实验与正交实验法确立了超声波提取工艺最佳条件为：乙醇浓度95％,超声波作用时间90min,料液比1：50（g：mL）,温度为60℃,提取次数2次,此时可获得较高的黄酮含量78．12mg／g。     

Ethanol extraction of polyphenols in an immersion extractor. Effect of pulsing flow

A comparative study on polyphenol extraction from sunflower press cake in a semicontinuous pulsed-flow immersion extractor and in a conventional laboratory immersion extractor was developed. The solvent was 96% (vol/vol) ethanol. No difference in the residual polyphenol content in the cake was observed at short times, but after 10 h, the pulsed extractor showed a higher polyphenol concentration in the outlet miscella. In addition, the effective diffusivity of polyphenols in sunflower press cake was estimated.     

Simultaneous extraction and preparative fractionation of egg yolk lipids using the principle of adsorption

A new approach describing the simultaneous extraction and preparative fractionation of egg yolk lipids is described, a method which can be extended to other tissues. In this method, egg yolk is adsorbed on activated thin layer chromatography grade silicic acid and sequentially extracted with different solvents to get a crude fractionation of its lipids into nonpolar and polar components. These crude concentrates help achieve larger yields of high purity lipids per unit column load during subsequent chromatographic subfractionation.     

Anwendungsmöglichkeiten der Gasextraktion im Bereich der Fette und Öle

Application Feasibilities of Gas Extraction in the Field of Fats and Oils During the extraction of relatively not volatile substances from solid material the effort which is to expect fairly depends on the capacity of the solvent. The available loading can significantly be increased by the appropriate choice of the solvent, by solvent mixtures and by the extraction in the “completely miscible” field. The material transport resistance of ground oil seed is mainly in the extracting medium. Further possibilities of gas extraction are found in the separation of fatty acids, fats and fat accompanying components. The results of recent work are submitted.     

Separation of aromatic components from light cycle oil by solvent extraction

To improve the versatility of light cycle oil (LCO), separation of aromatic compounds from LCO by solvent extraction was investigated. LCO was analyzed to identify 35 components: 19 aromatics and 16 alkanes. The batch liquid–liquid equilibrium extraction of LCO was performed using furfural, sulfolane, and methanol as extraction solvents. In each solvent, the aromatics present in LCO were selectively extracted relative to the alkanes. The separation selectivities of aromatics relative to alkanes were larger in sulfolane than in the other solvents. Among the aromatic components, di- and tricyclic compounds were selectively extracted relative to the monocyclic ones.     

Analysis of cholesterol and desmosterol in cultured cells without organic solvent extraction

Cultured cell sterols such as cholesterol and desmosterol are usually extracted into organic solvents before they are quantified with cholesterol esterase and oxidase. A method to quantify these cultured cell sterols using cholesterol enzymes without prior organic solvent extraction is described. In this method, a suspension or monolayer of cultured L-M, U-937, or PC-12 cells is digested with 0.1% sodium dodecyl sulfate (SDS), and the digest treated with microbial cholesterol enzymes. The quantity of oxidized sterols produced by the reaction can be measured easily with high-pressure liquid chromatography, when a mixture of sterols is present, or by the production of hydrogen peroxide when only one sterol is present. This method is easier and safer to use than solvent extraction and can greatly expedite the quantitation of cultured cell sterols. Preliminary data show that other lipids such as choline phospholipids, triglycerides, and fatty acids can also be directly quantified in SDS cell digest by using specific enzymes to transform these lipids into hydrogen peroxides.     

Performance of Green Solvents in the Extraction of Sunflower Oil from Enzyme-Treated Collets

The main goal of this work is to evaluate the extraction of sunflower oil from enzyme-treated collets using ethanol and isopropanol (IPA) as solvents. The sunflower collets are pretreated with the multienzyme complex Viscozyme L prior to solvent extraction by the Soxhlet method. The influence of the moisture content of the collets, pretreatment, processing time, and solvent type on the amount of total extracted material and the oil extraction efficiency is studied. Some quality parameters such as phospholipid content of the oil and chlorogenic acid content of the residual meal are also analyzed. At low moisture content (7%) the solvents exhibit similar oil extraction ability (98–99%), but with increasing moisture the extraction efficiency of ethanol decreases to about 85%, while no significant differences are observed for IPA. The enzymatic treatment increases the extraction efficiency for all times, especially for ethanol. It is observed that IPA is more efficient in the extraction compared to ethanol, and the amount of nonlipid material is reduced by ≈70%. In addition, the oil extracted with IPA have lower phospholipid content and the residual meal presents a higher chlorogenic acid content. Practical Applications:This work would contribute toward the use of green solvents in the extraction of sunflower oil from collets. Ethanol and isopropanol, used as solvents, present attractive advantages, including low toxicity, good operational security, as well as being obtained from a renewable source. The obtained data provide up-to-date information on the use of these alcohols in the extraction of sunflower oil from collets and the influence of operating conditions, such as moisture content, enzymatic pretreatment of the collets, and the extraction time. Information about oil and meal quality is also reported.