从黄连中提取黄连素

利用常规的实验仪器,模拟索式提取器原理,设计、组装了一套从黄连中提取黄连素的新实验装置。与传统回流装置、索氏提取装置、恒压漏斗装置进行比较研究。新装置具有提取时间短、提取率高、仪器常规等特点。通过实验确定了用新装置提取5 g黄连的最佳工艺参数为:95%乙醇80 mL,加热回流时间2.5 h。     

Production of linolenic acid from linseed oil

Linolenic acid of more than 95% purity was produced by liquid-liquid extraction of linseed oil fatty acids with wet furfural and hexane in a Podbielniak centrifugal extractor. The minimum ratio of furfural to linseed acids to obtain this purity was 10 to 1. There was no significant change in product purity for solvent ratios between 10 and 15, operating temperatures from 90° to 110°F., and furfural moisture contents between 1.0 and 2.8%. When the solvent ratio is reduced to 8 or the furfural moisture to 0.2%, purity decreases. Oxidation of linseed acids before extraction also results in decreased separation. An estimate based on pilotplant data indicates a “cost to make” (excluding administrative and selling expenses, profit, income taxes, and interest on investment) of 18.0 cents per pound of 97% linolenic acid for a process which includes hydrolyzing linseed oil, separating the fatty acids by liquid-liquid extraction, recovering solvents by distillation, and distilling the fatty acid products. Potential uses for linolenic acid are reviewed.     

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.     

A solvent extractor system for the rapid extraction of lipids and trace bioactive micronutrients in oilseeds

A low-cost laboratory extractor has been designed and constructed that selectively extracts polar and nonpolar components from oilseeds and other matrices. The extractor uses available high-performance liquid chromatography laboratory equipment for pumping the solvent into the extractor. Pressure, temperature, and valving arrangements are automatically controlled by commercially available components. Advantages of this system include low initial investment, reduced solvent consumption, shorter extraction times, quantitative lipid recovery, use of multiple extraction solvents, and reduction in cost per sample. The method has broader applications that include extraction of trace components from a variety of matrices, for example, the extraction of pesticides from foods and polychlorobiphenyls from soil. Class separation of components from different matrices can be achieved easily by selection of solvents with the appropriate polarity characteristics. Very small samples can be extracted simply by changing cell size or by adding an inert material to the cell to fill the void volume. Analyte collection can be accomplished by collecting in a test tube with an appropriate solvent, or on a solid-phase material. Optimization of extraction times, number of extractions, matrices, and solvent used is described. Neutral lipids were extracted from peanut meal in 70 min by the rapid extraction method compared to 1440 min required to extract the comparable amount of neutral lipids from a similar sample by the Soxhlet extraction method.     

圆筒式离心萃取器用于PEG/盐体系萃取提纯α-淀粉酶

根据双水相体系的特点,选择了Ф20(环)圆筒式离心萃取器进行a-淀粉酶的双水相体系萃取实验,考察了萃取器的水力学特性,确定了萃取操作范围,并考察了萃取器转鼓转速、总流量对体系传质特性、a-淀粉酶失活和收率的影响.结果表明,在转速3380～3800r/min、流比0.2～0.5、总流量25～50ml/min范围内,萃取器的轻相夹带量可在10%以内,重相夹带量趋近于零,a-淀粉酶的失活可以忽略不计,萃取效率和收率分别达90%和75%以上.     

Sunflowerseed extraction with a new type of extractor

In this study extraction of sunflowerseeds is performed using a new extractor system which eliminates various operations, such as dehulling and prepressing, of the conventional systems. This new extraction system uses a moving bed of seeds which is continuously washed with fresh solvent sprayed from mobile spray nozzles. To confirm the performance of the Gülbaran extractor for extraction of sunflowerseeds, the effects of extraction temperature, residence time, solvent/meal ratio and particle size on the oil yield are investigated. The experiments performed showed that the optimum extraction conditions are 50–53 C solvent temperature, 40–45 C extractor temperature, 90 min extraction time, 2.7 kg/hr solvent flow rate and 0.9–1.0 mm particle size. The resultant miscella in this system was more dilute than some multicell extractors, thus requiring more evaporator costs. Deceased.     

用离心萃取器连续逆流提取氢化可的松的研究

采用环隙式离心萃取器进行了提取氢化可的松的研究。用醋酸丁酯从发酵液中萃取氢化可的松 ,其传质过程受扩散因素控制 ,且分配系数随平衡水相浓度的增大而增大。开发了用环隙式离心萃取器连续逆流提取氢化可的松的工艺流程 ,当转速为 340 0～ 380 0r/min ,总流量为 40～ 75mL/min ,V(O ,有机相 )∶V(A ,水相 )为 (0 35～ 0 42 )∶1 0 0时 ,氢化可的松的萃取率为91 0 8%～ 93 16 % ,而厂家现行生产工艺采用的V(O)∶V(A)是 0 7∶1 0 ,氢化可的松的萃取率为90 %。因而 ,新工艺提高了氢化可的松的萃取率 ,降低了萃取剂耗量     

Coal particle integrity in high-temperature solvents,with and without agitation

The physical characteristics of W. Kentucky (bituminous) and Wyodak (subbituminous) coal particles after exposure to hydrogen-donor solvents at temperatures of 400–450°C have been observed. It is found that for exposures of up to 2 min, with pyridine extraction yields of up to 86% maf, particles do not disintegrate if no mechanical stresses are applied to them. By contrast, with modest rates of stirring at 400 °C the particles do disintegrate at times as short as 2 min even with corresponding pyridine extraction yields of as low as 52% maf. The mineral matter appears to comprise a major part of the physical skeletal structure which maintains particle integrity, in the absence of mechanical stresses, even after most of the organic matter has been removed.     

Extraction of lipids from Yarrowia Lipolytica

BACKGROUND: Microorganisms have often been considered for the production of oils and fats as an alternative to agricultural and animal resources. Extraction experiments were performed using a strain of the yeast Yarrowia lipolytica (Y. lipolytica), a high‐lipid‐content yeast. Three different methods were tested: Soxhlet extraction, accelerated solvent extraction (ASE) and supercritical carbon dioxide (SCCO₂) extraction using ethanol as a co‐solvent. Also, high pressure solubility measurements in the systems ‘CO₂ + yeast oil’ and ‘CO₂ + ethanol + yeast oil’ were carried out. RESULTS: The solubility experiments determined that, at the conditions of the supercritical extractor (40 °C and 20 MPa), a maximum concentration of 10 mg of yeast oil per g of solvent can be expected in pure CO₂. 10% w/w of ethanol in the solvent mixture increased this value to almost 15 mg of yeast oil per g of solvent. Different pretreatments were necessary to obtain satisfactory yields in the extraction experiments. The Soxhlet and the ASE method were not able to complete the lipid extraction. The ‘SCCO₂ + ethanol’ extraction curves revealed the influence of the different pretreatments on the extraction mechanism. CONCLUSION: Evaluating the effectiveness of a given pretreatment, ASE reduced the amount of material and solvent used compared with Soxhlet. In all three cases, the best total extraction performance was obtained for the ethanol‐macerated yeast (EtM). Addition of ethanol to the solvent mixture enhanced the oil solubility. Oil can be extracted from Y. lipolytica in two different steps: a non‐selective ethanol extraction followed by TAG‐selective SCCO₂ purification. © 2012 Society of Chemical Industry     

Reactive extraction of oilseeds with dialkyl carbonates

Using dialkyl carbonates as reagents for lipase‐catalyzed transesterification, the reaction is driven by the evolvement of carbon dioxide as the co‐product and thus no longer an equilibrium reaction. Therefore this transesterification method is faster and quantitative conversions can be obtained. Short‐chain dialkyl carbonates, like other short‐chain esters, are also suitable solvents for seed oil extraction. Thus, extraction and transesterification can be combined in a single reaction. This reaction, called reactive extraction, was carried out in a standard Soxhlet apparatus with rapeseed, linseed and calendula seed as the raw materials and with dimethyl and diethyl carbonate as extraction solvent and transesterification reagent at the same time. Fatty acid methyl esters and ethyl esters respectively were obtained with higher yields than those achieved by conventional two step extraction / transesterification. In the case of linseed fatty acid esters and especially calendula seed fatty acid esters, the iodine values of the products obtained by one‐pot‐two‐step reactive extraction were significantly higher.     

荔枝皮抗氧化性研究

用索氏提取器以正己烷、乙酸乙酯、φ(C2 H5OH) =95 %的乙醇依次提取成熟荔枝皮 2、2、4h ,提取率分别是 3 6 6 %、1 4 3%、9 35 % ,添加相当于猪油质量 0 0 2 %的此 3种提取物于猪油中 ,正己烷、乙酸乙酯提取物可使猪油的氧化酸败的时间延长 2 6倍以上 ,φ(C2 H5OH) =95 %的乙醇提取物可延长 1 7倍以上。以 φ(C2 H5OH) =95 %的乙醇提取成熟荔枝皮 6h ,提取率为12 2 4 % ,添加此提取物为猪油质量 0 .0 4 % ,在猪油中的抗氧化效果优于 0 0 2 %的BHT ,且提取物的抗氧化性随添加量的增加而增强。以 φ(C2 H5OH) =95 %的乙醇室温浸提未成熟荔枝 (生理落果 )皮 4d ,提取率达 2 8 7%以上 ,抗氧化性也很强。经层析分离 化学显色初步推断荔枝皮抗氧化成分中有酚酸、黄酮类物质     

超临界萃取技术的应用研究进展

超临界流体萃取技术开辟了分离工业的新领域，是一种新型的分离技术。综述了超临界萃取技术的研究进展，介绍了超临界萃取技术在金属离子、香料化妆品、天然中草药、石油加工、保健食品等方面的应用和研究进展，提出了超临界萃取技术新的研究领域，随着研究工作的不断深入，更加理想萃取剂的发现，必将使超临界萃取技术的应用前景更加广阔。     

Pressurized Water Extraction of Hydrolysable Tannins from Phyllanthus niruri Linn

Pressurized water extraction (PWE) was studied for the extraction of hydrolysable tannins from Phyllanthus niruri Linn. The effects of operating conditions (pressure, temperature, and the water flow rate) on the extraction yields were investigated. The results showed that the extraction yields increased with increasing temperature and with decreasing water flow rate, whereas pressure gave no significant effect. At 100 bar, 100°C and 1.5 ml/min, the extract had higher component contents (%g/g extract) of gallic acid (0.65%), corilagin (4.11%), and ellagic acid (8.91%) than a commercial HEPAR-P? extract (0.21%, 2.64%, 4.17%, respectively). It was also found that the dynamic PWE had a faster extraction rate and lower solvent consumption (0.018 m³/kg) compared to the Soxhlet extraction and ultrasonication.     

蜂窝(FG)型规整填料萃取塔的性能研究

本文对新开发的蜂窝(FG)型规整填料萃取塔的流体力学和传质性能进行了系统的实验研究。结果表明,这种新型填料萃取塔的通量(比负荷)大,传质效率较高,已成功地应用于汽油脱硫醇的萃取过程中。     

Rice hull biocomposites,part 2: Effect of the resin composition on the properties of the composite

A free radical thermoset resin consisting of a copolymer of conjugated linseed oil (CLO) or conjugated soybean oil (CSO), n‐butyl methacrylate (BMA), divinylbenzene (DVB), and maleic anhydride (MA) has been reinforced with rice hulls. Composites containing 70 wt % of the filler were compression molded, the conjugated oil content in the resin was kept constant at 50 wt %, and the relative amounts of BMA, DVB, and MA were varied to afford composites with different resin compositions. Tensile tests, DMA, thermogravimetric analysis, and Soxhlet extraction of the different composites prepared have been used to establish the relationship between resin composition and the properties of the composites. Overall, the mechanical properties tend to improve when MA is introduced into the resin. Scanning electron microscopy of selected samples showed a better filler–resin interaction for MA‐containing composites and samples prepared from CLO exhibit better properties than those prepared from CSO. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2011     

Soybean and linseed oil‐based composites reinforced with wood flour and wood fibers

Composites consisting of a conjugated linseed or soybean oil‐based thermoset reinforced with wood flour and wood fibers have been prepared by free radical polymerization. The thermoset resin consists of a copolymer of conjugated linseed oil (CLO) or conjugated soybean oil (CSO), n‐butyl methacrylate (BMA), divinylbenzene (DVB), and maleic anhydride (MA). The composites were cured at 180°C and 600 psi and postcured for 2 h at 200°C under atmospheric pressure. The effect of varying filler load, time of cure, filler particle size, origin of the fillers, and resin composition has been assessed by means of tensile tests, DMA, TGA, Soxhlet extraction followed by ¹H‐NMR spectroscopic analysis of the extracts, and DSC. The best processing conditions have been established for the pine wood flour composites. It has been observed that the addition of MA to the resin composition improves the filler‐resin interaction. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2012     

Zu den Veränderungen von Rapsöl und Leinöl während der Verarbeitung

Changes of rapeseed and linseed oil during processing During processing of crude oil in a large oil mill, three samples each of rapeseed and linseed were investigated at each processing stage, i.e. press oil, solvent-extracted oil, mixed oil, and degummed/caustic refined oil. In the case of rapeseed also bleached and desodorized oils (230°C; 3.0 mbar for 2 h) were investigated. Rapeseed and linseed oil showing the typical major fatty acids contained less than 1% trans-isomeric fatty acids (trans fatty acids = TFA). Linseed oil had a similar TFA-concentration as rapeseed oil, and the concentrations did not change during the processing stages up to degummed/caustic refined oil, and were also unchanged in the bleached rapeseed oil. Desodorization of rapeseed oil, however, trebled the TFA concentration to 0.58%. The detected tocopherol patterns were typical of rapeseed and linseed oils. There was no difference between mixed oil and degummed/caustic refined oil in the total concentration of tocopherols. Neither had bleaching any effect. Rapeseed oil desodorization diminished total tocopherol concentration by 12% from 740 mg/kg to 650 mg/kg. Due to degumming/caustic refining the phosphorus concentration of both oils decreased to less than a tenth compared to mixed oil. Other elements determined in degummed/caustic refined rapeseed oil were not detectable (manganese < 0.02 mg/kg, iron < 0.4 mg/kg, copper < 0.02 mg/kg, lead < 10 μg/kg) or only as traces zink 0.1 mg/kg, cadmium 2 μg/kg). In linseed oil, which initially showed a higher trace compounds concentration, a significant decrease was found by degumming/caustic refining. Iron could not be detected. There were traces of zinc, manganese, copper, lead, and cadmium. There was no difference between the acid values of rapeseed and linseed crude oil. Acid value decreased drastically already during the degumming/caustic refining stage. The crude linseed oils had a higher peroxide value, anisidine value and diene value than the corresponding crude rapeseed oils. With peroxide values of ≤ 0.1 mEq O₂/kg found in almost all investigated rapeseed oils, no effect of refining could be detected. The anisidine value showed an increase after bleaching. Desodorization trebled the diene value.     

中药植物战骨总黄酮的提取

用传统索氏提取法及现代提取方法——微波萃取法、超声波萃取法、内部汽化法4种不同的提取方法对战骨中的总黄酮进行了提取工艺研究。采用上述4种方法对战骨中总黄酮进行提取,并进行了后3种方法的L9(34)正交设计性实验。测定了以上4种方法的战骨提取液的总黄酮含量及回收率,并将后3种方法与索氏提取法进行比较。结果表明,微波萃取法、超声波萃取法、内部汽化法的最优方案的收率分别为2.07%,1.90%,1.78%,平均回收率分别为100.60%,105.12%,99.92%,相对标准偏差分别为1.40%,1.47%,1.16%。索氏提取法提取的收率为0.95%。现代方法的收率均高于传统索氏提取法。     

Extraction Kinetics and Anethole Content of Fennel (Foeniculum vulgare) and Anise Seed (Pimpinella anisum) Extracts Obtained by Soxhlet,Ultrasound, Percolation,Centrifugation, and Steam Distillation

Foeniculum vulgare (fennel) and Pimpinella anisum (anise) extracts were obtained by Soxhlet, cold percolation, ultrasound assisted extraction, and centrifugal extraction using ethanol as solvent; anise extracts were also obtained by steam distillation. Soxhlet presented the highest yields for both fennel and anise seed (16.8% and 23.3%, respectively). The highest anethole content among ethanolic extracts was obtained for centrifugal extraction (6.8 mg/g and 143 mg/g for fennel and anise extracts, respectively). Steam distillation presented low yield (0.26%), but high anethole content (68–98%, area). Anise ethanolic extracts also tested positive for flavonoids.     

Optimization of supercritical fluid extraction of linseed oil using RSM

The objective of the present study was to develop a supercritical fluid extraction (SFE) method, suitable for extraction of total oil content from linseed, and to be used as a preparative technique for fatty acid determination. Optimum conditions (volume of added ethanol as a co‐solvent, dynamic extraction time (DET), and pressure) were predicted in order to obtain the maximum yield of the extract. Response surface methodology (RSM) and central composite rotatable design (CCRD) were used for modeling the process. Variable values ranged as follows: co‐solvent 0–1 mL, DET 36–60 min, and pressure 45.57–62.05 MPa (6000–9000 psi). Effects of co‐solvent volume and extraction pressure were well described by simplified polynomial equation (R² = 0.85), since DET had no significant influence (p>0.05) on the extract yield. The maximum yield of oil, calculated from experimental results, was obtained with 1 mL of co‐solvent, and pressure of 62.05 MPa. Optimized conditions were used for extraction of oil from four samples of linseed, ground to pass through 1, 2, 3, and 4 mm‐sieve, to determine adequate granulation for SFE. Finally, results for yield and fatty acid composition of the extract obtained using SFE were compared with the results of Soxhlet extraction. Practical applications: The obtained extracts can be used for fatty acid analysis, since they have not been damaged and their fatty acid compositions have not been degraded by reagents or aggressive extraction conditions. It is shown that the selection of appropriate milling equipment for grinding of samples is necessary to achieve adequate granulation and avoid fractionation of sample.