A Simplified Method for Fractionation and Analysis of Waxes and Oils from Sorghum (Sorghum bicolor (L.) Moench) Bran

In the United States, sorghum is primarily used for animal feed and ethanol production but has potential to provide value-added coproducts including waxes and oil. The surface of sorghum contains 0.1–0.4% wax; however, wax extraction from whole kernels before fermentation may not be economical. An alternative method for this extraction could be facilitated through decortication, abrasion of the surface to remove bran. Decortication increases the starch content of decorticated sorghum, potentially improving ethanol yields, while concentrating wax and oil to the bran. Typically, oil (triacylglycerols) and waxes are extracted from bran in one extraction and waxes are precipitated from oil using cold temperatures then filtration. This research compared traditional fractionation (simulated with a two-step, single-temperature extraction) to a two-step, dual-temperature extraction, whereby oil is first extracted at room temperature and then waxes at elevated temperature. Extractions were performed using an accelerated solvent extractor with hexane or ethanol as solvents. Ethanol extraction showed greater yields (~15% w/w) compared to those of hexane (~11% w/w) because polar materials were extracted. Using hexane, the two-step, dual-temperature fractionation separated waxes from oils via the temperature of extraction solvent with similar purity to the traditional method that fractionated via cold precipitation and filtration. For ethanol, the traditional single-step method fractionated with higher wax purity but lower oil purity compared to the two-step, dual-temperature fractionation.     

Extraction of Lipids from Aqueous Protein‐Rich Streams using Near‐Critical Dimethylether

An extraction process for obtaining lipids from aqueous protein/lipid mixtures has been developed using near‐critical dimethylether (DME) as the solvent. The process has been demonstrated on fresh and reconstituted egg yolks, and on selected dairy by‐product streams. The lipid yield is dependent on the processing temperature, solids content and feed ratio of solvent to liquid. The extent of protein denaturation is also dependent on these parameters. The phase equilibria of DME‐water‐phospholipid mixtures are presented with modeling of the DME‐water system using the Peng‐Robinson equation of state.     

Extraction of α‐tocopherolquinone from vegetable oil deodorizer distillate waste

In industry, deodorizer distillate waste is one of the last products of refined edible oil after the removal of commercially important value components such as fatty acids, sterols, squalene, and vitamin E. The refinery process itself is the cause of a significant amount of loss in vitamin E due to distillation and thermal oxidation. The distillate waste has a very limited commercial value, therefore requires additional costs for a safe environmental disposal. One of the main vitamin E oxidation products found in large quantities in oil waste is tocopherolquinone (TQ). A literature search has revealed that in the past several techniques including a variety of solvent extractions, saponification, or column extraction have been used for TQ isolation with limited success. The present study is a new cost‐effective liquid–liquid extraction method developed to isolate α‐TQ from vegetable oil steam distillate or distillate waste. High recovery results ranging from 31 to 120% were obtained depending on the ratio between the sample and three different organic extraction solvents (acetonitrile, methanol, and hexane) combined.     

Plant Sterol and Policosanol Characterization of Hexane Extracts from Grain Sorghum, Corn and their DDGS

Plant sterols (PS) and policosanols (PC) have been attributed with plasma cholesterol-lowering properties in humans. Hexane extracts from grain sorghum, corn and their distillers dried grain with solubles (DDGS), an important co-product of ethanol production, contain these health promoting compounds, which could be used to develop health promoting dietary products. However, limited information is currently available regarding optimal methods of extraction and their influence on plant sterol or PC levels and compositions. Therefore, the objective of this study was to quantify lipids, particularly PS and PC extracted from grain sorghum and its DDGS using reflux and Soxtec methods. Corn and its DDGS were also extracted to compare lipid yields and PS/PC compositional profiles in these two related cereals. Intact grains were extracted either as whole or ground kernels. Lipid yields from all the corn sources were typically greater than those obtained from grain sorghum. Lipid yields from DDGS were the highest among all the forms of the grains used whereas corn/sorghum DDGS contained the highest levels of PS and PC, respectively. Additional study demonstrated that hydrolysis (acidic and alkaline) of ground sorghum or sorghum DDGS increased the levels of total extractable plant sterols. Overall, the Soxtec method extracted higher amounts of lipids than the reflux method.     

超临界萃取生姜中姜油的研究

研究了应用超临界二氧化碳萃取生姜的工艺条件,结合萃取压力、温度、时间,物料水分、粒度等参数对萃取率的影响。采用单因子变化的实验方法,得出生姜萃取率的最佳工艺条件为：压力20MPa,温度40℃,二氧化碳流量20L／h,时间2h。     

Production of Fatty‐Acid Methyl Esters Via the In Situ Transesterification of Grain Sorghum Bran and Sorghum Distiller's Dried Grains and Solubles

The acylglycerols (AG) in sorghum bran and distiller's dried grains and solubles (DDGS) from sorghum postfermentation have been converted to fatty‐acid methyl esters (FAME) using an in situ transesterification method. The reactions were conducted at 25 or 40 °C by incubating 8 g of feedstock, containing 1.3–2.4 mmol AG, in a solution of 2.4 or 4.8 mmol of NaOMe dissolved in 6.4 or 12.8 mL MeOH. The experimental results confirmed that reducing the moisture to approximately 2% (w/w) within the feedstock was necessary for the reaction to proceed. All of the reactions were monitored using high‐performance liquid chromatography and all performed better at 40 °C than at 25 °C. The most successful reactions used a AG:NaOMe:MeOH molar ratio of 1.0:2.0:131.7. Those reactions used 4.8 mmol NaOMe dissolved in 12.8 mL MeOH producing up to 98.3% FAME when sorghum bran was used as the feedstock. When DDGS from sorghum were used as the feedstock, the yield averaged 32.2% under the previously established optimal conditions.     

响应面法优化荷叶生物碱盐提取工艺及其纯化

在单因素实验的基础上,通过响应面法分析和优化提取条件,考察超声酸提法中酸的种类、酸的质量分数、超声时间、液固比〔液体体积(m L)与固体质量(g)的比值〕、超声功率和温度对荷叶碱提取效果的影响以及D101型大孔树脂对提取物的纯化效果。得到的荷叶生物碱盐的最佳提取工艺条件为:加热温度60℃、超声功率500 W、盐酸质量分数0.3%、超声时间41 min、液固比27,在该工艺条件下荷叶碱的得率为(4.12±0.05)mg/g。以体积分数为70%的乙醇作为洗脱液,纯化后的生物碱盐经分光光度法测得纯度为40.81%。     

响应面优化葛根黄酮提取工艺研究

验以葛根粉为原料、乙醇为溶剂,研究了不同提取时间、不同提取温度、不同乙醇浓度对葛根黄酮提取率的影响,在单因素实验的基础上用紫外分光光度计法进行含量测定,并进行了3因素3水平的Box-Behnken设计优化了葛根黄酮的有关提取参数,最优工艺条件为:提取时间60min、提取温度80℃、乙醇浓度60%。在最佳优化条件下葛根黄酮提取率达到极大值,葛根黄酮提取率为36.64%。该方法快速简单,结果准确,可用于葛根素提取。     

Extraction of Polycyclic Aromatic Hydrocarbons in Barn Owls ( Tyto Alba ) from Northwest Spain by SFE and HPLC-FL Analysis

Supercritical fluid extraction (SFE) and high-performance liquid chromatography-fluorescence detection (HPLC-FL) were used to determine concentration of anthracene, benzo[ a ]anthracene, benzo[ a ]pyrene, benzo[ b ]fluoranthene, benzo[ ghi ]perylene, benzo[ k ]fluoranthene, chrysene, fluoranthene, pyrene, and indeno[1,2,3- cd ]pyrene in six classes of tissue (heart, liver, intestine, muscle, lung, and kidney) of 11 barn owls from Galicia (northwest Spain). We have detected fluoranthene and pyrene in >40.0% of samples, anthracene in 35.4%, and benzo[ a ]anthracene in 12.3%. Mean concentrations were between 0.398 w g/kg dry weight for anthracene and 4.855 w g/kg dry weight for fluoranthene. Lung and intestine tissues were more polluted than the other tissues.     

Amoxicillin Extraction from Aqueous Solution by Emulsion Liquid Membranes Using Response Surface Methodology

The extraction of amoxicillin (AMX) from aqueous solutions by emulsion liquid membranes (ELMs) was investigated for the first time. The liquid membrane phase of the ELM consisted of Aliquat 336 as carrier, Span 80 as surfactant, n‐hexane as diluent, and sodium chloride solution as internal phase. Response surface methodology (RSM) based on central composite design (CCD) was applied to evaluate and optimize the effects of several parameters such as carrier concentration, feed concentration, internal phase concentration, and treat ratio (volume ratio of the external phase to the emulsion phase). A polynomial model was fitted to predict the extraction yield of AMX. Under optimized conditions, the highest extraction yield of AMX was 99.8 %.     

从卤水中提取碘的研究进展

对采用空气吹出法和离子交换法从卤水中提取碘进行了综述,对所述技术的优缺点进行了探讨,指出离子交换法具有实际的应用价值。     

Identification of Sulfur‐Containing Impurities in Biodiesel Produced From Brown Grease

Fatty acid methyl esters (FAME) from waste grease usually contain higher concentrations of sulfur (S) than allowed to meet the specified quality standard for biodiesel (<15 ppm). Brown grease lipid‐derived FAME was produced and fractionated by two passes through a wiped‐film evaporator (WFE) to produce three fractions: (1) a 120 °C pass distillate, (2) a 170 °C pass distillate, and (3) a heavy residue. Solid phase extraction (SPE) was used to concentrate the S species from the distillate fractions so that they could be detected by a gas chromatography–pulsed flame photometric detector (GC–PFPD) and GC–mass spectrometry (MS). The ethyl acetate and methanol (MeOH) fractions obtained by SPE of the 120 °C WFE distillate and methyl tert‐butyl ether and acetone fractions obtained by SPE of the 170 °C WFE distillate had the highest concentration of S and were, therefore, the best candidates for GC–PFPD analysis. GC–PFPD methods were developed to separate the S species adequately enough for those peaks to be analyzed by GC–MS which matched fragmentation patterns identified by the MS chemical library as tetrahydrothiophenes, dithiolanes, and thiophenes. MS fragmentation patterns were used to identify other, larger, S‐bearing species as sulfides and disulfides cross‐linking between two FAME molecules. The results obtained from this study provide a foundation for developing effective purification methods to remove S‐containing impurities from waste grease‐derived biodiesel.     

Evaluation of the Phenolic Content and Antioxidant Activity of Different Seed and Nut Cakes from the Edible Oil Industry

The objective of this work was to extract water‐soluble compounds from different seed and nut cakes under the same conditions and compare the phenolic content and antioxidant activity of the cake extracts. Seed cakes of sunflower, pumpkin, flaxseed and defatted sesame, and nut cakes of almond, pecan, macadamia and hazelnut were used in the experiments. Extracts were obtained by solid–liquid extraction with a water/ethanol solution (20:80, v/v). Total phenolic content, flavonoids, flavan‐3‐ols and condensed tannins in the extracts were determined using spectrophotometric analysis. Antioxidant properties of the extracts were determined by the DPPH and ABTS radical scavenging methods, and by determination of the reducing power and chelating activity. The extract from pecan nut cake presented the highest amounts of all compounds analyzed, followed by sunflower seed and hazelnut cake extracts. These samples also had the highest effects on the ABTS and DPPH radicals, as well as the uppermost reducing powers. The extracts from pecan nut and sunflower and sesame seeds were analyzed using HPLC and individual phenolics were further characterized.     

Box-Behnken响应面法优化藤梨根总黄酮超声提取工艺

目的:优化藤梨根总黄酮超声提取工艺。方法:超声提取药材,利用分光光度计法于510 nm波长处测定总黄酮含量,运用Design-Expert 8.0.6 Trial软件建立以总黄酮提取率作响应值,液料比、乙醇体积分数和提取时间为三因素的Box-Behnken响应面并进行多元二次回归分析。结果:最佳提取工艺条件为液料比12.45,乙醇体积分数78.09%,提取时间39.66 min,总黄酮的提取率为7.49%,与预测值7.58%偏差1.19%。结论:该工艺稳定可行,可用于藤梨根中总黄酮的工业化生产。     

万寿菊叶黄素提取工艺的研究

介绍了以万寿菊干花粉为原料,通过改变溶剂种类、提取时间等条件对叶黄素提取率的影响进行了研究.结果表明:浸提溶剂采用氯仿-乙醇3:2的混合溶液,浸提次数2次,物料比1:10,浸提时间每次浸提2 h,皂化时NaOH的浓度5%,皂化时间8 h,提取效果最佳.     

从水溶液中提取琥珀酸

琥珀酸是一种用途广泛的有机酸，但现有的制备过程工艺复杂、成本较高。本文提出了一个有效的萃取体系，用以提取废液和稀溶液中的琥珀酸。并对其萃取体系及其萃取机理进行了较为全面的研究，进而提出了一个从水溶液中提取琥珀酸的建议流程。     

Separation of perillyl alcohol from Korean orange peel by solvent extraction and chromatography

Perillyl alcohol, abundant mainly in oranges, has chemotherapeutic activity against carcinogenesis. The peel of Korean oranges was extracted by methanol, and the extract was partitioned by methanol-extract/water/chloroform, (20/5/30 vol%). To concentrate perillyl alcohol of the water-phase in the previous partition step, a glass column (2.5 i.d. x 15 cm) with reversed-phase C₁₈ packings (40–63 μm) was used. Finally, to obtain perillyl alcohol in a pure form, reversed-phase high-performance liquid chromatography (RP-HPLC) was applied. Mobile phases used were water, methanol, and acetonitrile. The flow rate of the mobile phase was 1 ml/min and UV wavelength was fixed at 205 nm. The resolution of perillyl alcohol from Korean orange peel was achieved on a μ-Bondapak C₁₈ column (3.9x300 mm, 10 μm) and in-house Chromatographic column packed with 15 μm C₁₈ preparative packings. From the experimental results, the mobile phase composition was water/acetonitrile, (65/35 vol%) and the retention time of perillyl alcohol was 20.5 min in the analytical μ-Bondapak column. The effect of injection volumes was investigated in the preparative column.