Supercritical carbon dioxide extraction of sea buckthorn (Hippophae rhamnoides L.) pomace

BACKGROUND: The goal of this work was to utilize the sea buckthorn pomace, which is the by‐product of a sea buckthorn juice process. Pilot plant supercritical fluid extraction (SFE) experiments were performed in a 5 × 10^?3 m³ volume high‐pressure vessel. The effects of pressure and temperature on extraction yield and recoveries of biologically active components were studied using a 3² full factorial design. The pressure and temperature were varied over the ranges of 30–46 MPa and 313–353 K, respectively. The extract samples were analysed by TLC‐densitometry, UV/VIS spectrofotometry and HPLC methods. RESULTS: The obtained yields changed between 142–164 g kg^?1, according to the solvent power of the supercritical fluid. The recoveries of the different minor components were (g minor components kg^?1 dried raw material): 2.50–4.25 sitosterol, 0.20–1.60 ursolic acid, 0.04–0.18 carotenoid, 0.35–0.42 total tocopherol. CONCLUSION: By evaluation the designed experiments 46 MPa and 333 K were chosen as the optimum conditions. Copyright © 2007 Society of Chemical Industry     

Supercritical CO2 extraction of Chilean hop (Humulus lupulus) ecotypes

Hops (Humulus lupulus L) have very stringent requirements of diurnal light hours during flowering. Thus, the beer industry is permanently assessing new agricultural land to grow hops, southern Chile being an excellent candidate for their introduction. Supercritical carbon dioxide extraction procedures were implemented to assess Chilean hop ecotypes. Based on results of a preliminary study with commercial samples (cv Nugget), 200 bar and 40 °C were selected as extraction conditions. Very limited increases in extraction rate were observed when applying pressures >200 bar; such pressures did not speed up the extraction of α‐acids (bitter flavor principles), but rather increased the co‐extraction of undesirable compounds (hard resins and chlorophyll pigments). On the other hand, the effects of retrograde condensation phenomena were just starting to subside at 200 bar, and thermal damage of samples could increase at >40 °C. Ground cone samples of five local hop ecotypes, originating from Osorno, La Junta, Coyhaique and Elizalde Lake, were subsequently tested. Osorno exhibited a higher yield (65 g kg^?1 oleoresin/substrate) than other Chilean ecotypes. Moreover, Osorno extract had a light yellowish color, as well as a higher content of bitter flavors (157 g kg^?1 α‐acid/extract) and 1.5–7.1 times more representative aroma compounds than extracts of the other ecotypes. However, all these indicators were very low compared with the commercial Nugget sample (134 g kg^?1 oleoresin/substrate, 383 g kg^?1 α‐acid/extract, 14 times more aroma compounds than Osorno ecotype). Copyright © 2003 Society of Chemical Industry     

黄秋葵籽油的超临界CO2萃取 及其软胶囊制备工艺研究

以黄秋葵籽提油率为响应值,采用响应面法优化黄秋葵籽油超临界CO2萃取工艺;以崩解时限为评价指标,采用正交实验对黄秋葵籽油软胶囊制备工艺进行优化。结果表明：超临界CO2萃取黄秋葵籽油的最佳工艺条件为萃取压力30 MPa、萃取温度60?℃、萃取时间60 min,在此条件下提油率为17.23%;黄秋葵籽油软胶囊最佳制备工艺条件为水与明胶质量比1∶?1、明胶与甘油质量比3∶?1、溶胶温度80?℃、溶胶时间10 h,在此条件下黄秋葵籽油软胶囊的崩解时限为30.3 min,符合《中国药典》中软胶囊崩解时限不大于1 h的要求。     

Supercritical carbon dioxide extraction and fractionation of oregano oleoresin

The leaves of Origanum vulgare L. (Lamiaceae) harvested in different countries, three samples from Hungary and one from Turkey, were extracted with carbon dioxide in a high pressure apparatus with a 5 l extractor vessel volume. Total extractions with stagewise precipitation of the extracts were carried out in order to obtain essential oil-rich liquid and pasty products. A fractionated extraction with a stepwise increase of the extraction pressure was also performed to obtain portions of extracts of different quality. The extraction with carbon dioxide was compared to conventional steam distillation and to Soxhlet extraction with hexane, whith the goal of recovering essential oils and oleoresin products, respectively.     

Supercritical carbon dioxide extraction of onion oleoresin

Supercritical carbon dioxide (SC-CO₂) extraction on a laboratory-scale, was applied to produce oleoresin from dried onion (Allium cepa L). The goal of this work was to determine the optimal conditions of extraction for producing oleoresin with the highest yield and the best quality. A polynomial model was developed on the data. The square of correlation coefficient was R²=0·9022 (at P⩽0·05). The statistical analysis showed that the extraction pressure, temperature, and time have significant influence on the yield of the oleoresin. Increasing these parameters resulted in an increase in the yield. Maximum yield was obtained when the extraction pressure and temperature were above 350 bar and 57°C, respectively. At the lowest pressure (150 bar) applied the highest concentration of sulphur was produced in the oleoresin. The concentration of sulphur increased as a function of temperature when the pressure was maintained at 300 and 400 bar. The composition of volatile compounds of oleoresin differed from that of distilled onion oil. © 1998 SCI.     

Supercritical carbon dioxide extraction for identification of adulteration of black pepper with papaya seeds

Supercritical fluid extraction (SFE) using carbon dioxide was used to detect the adulteration of black pepper powder with ground papaya seed. Thin‐layer chromatography analysis of the SFE extracts showed a fluorescent band at 366 nm at R_f 0.172 that proved to be a promising marker for the presence of papaya seed powder in black pepper powder even at a level of 20 g kg^?1. The straight‐chain aldehydes n‐nonanal, n‐decanal and n‐dodecanal were tentatively identified by gas chromatography–mass spectrometry analysis as components of this fluorescent marker and were not present in black pepper extracts. Copyright © 2003 Society of Chemical Industry     

超临界CO2萃取无花果脂肪酸的GC-MS分析

以无花果为实验试材,利用正交实验法对超临界CO2萃取无花果脂肪酸的提取条件进行了研究。结果表明,最佳提取条件为:萃取压力30MPa,温度45℃,流量35kg/h,萃取时间60min,此条件下无花果脂肪酸提取率为4.5%。采用气相色谱-质谱联用技术(GC-MS)测定最佳萃取条件下所得脂肪酸的化学成分及其相对质量分数,共分离出24种成分并鉴定出其中的20种,其中不饱和脂肪酸相对含量约占82.33%。     

超临界CO2萃取苹果皮渣中二十八烷醇的工艺研究

研究以苹果皮渣为试验材料,利用超临界流体萃取技术从苹果皮渣中提取二十八烷醇.结果表明:苹果皮渣中二十八烷醇的超临界CO2流体萃取适宜条件为:萃取压力40MPa、萃取温度50℃、萃取时间75min,流量范围1.5～2.5mL/min.     

Supercritical carbon dioxide extraction of oil and α‐tocopherol from almond seeds

The objective of this study was to extract oil and tocopherols from almond seeds using supercritical carbon dioxide and to compare this extraction with a traditional solvent method. Oil and tocopherol extraction rates were determined as functions of the pressure (350–550 bar), temperature (35–50 °C) and CO₂ flow rate (10–30 kg h⁻¹), using a 10‐l vessel. The effects of matrix particle size on extraction yield were also studied and it was demonstrated that extraction yield is greatly influenced by particle size. Maximum recovery was obtained in the first 2–3 h of extraction at a pressure of 420 bar, a temperature of 50 °C and a flow rate of 30 kg h⁻¹ CO₂. These results suggest that the elevated initial oil and tochopherol solubility is related to the increased proportion of fatty acids in the initial extract. The results were compared with those obtained when hexane/methanol was used as a solvent. Copyright © 2005 Society of Chemical Industry     

不同黄秋葵籽粒产量与品质比较

以不同来源的6个黄秋葵品种(咔里巴、ACF、红秋葵、杨贵妃、白秋葵、纤指)为研究材料,初步测定了籽粒产量、产量构成因素、含油率、蛋白质含量、脂肪酸含量和氨基酸含量。结果表明:杨贵妃的籽粒产量最高,纤指的蛋白质含量最高;6个品种籽粒的平均含油率为19.37%,供试品种籽粒中亚油酸含量最高;在黄秋葵籽粒中检测到17种氨基酸,其中谷氨酸含量最高。     

超临界CO2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,并可通过添加适当的夹带剂和改善体系传质状况提高萃取效率。     

Supercritical carbon dioxide extraction of volatile oil from Italian coriander seeds

Supercritical CO₂ fluid extraction of the volatile oil from Italian coriander seeds was carried out under different conditions of temperature (40 and 50 °C), pressure (90, 100 and 150 bar), mean particle size (0.4, 0.6 and 0.8 mm) and CO₂ flow rate (0.79, 1.10 and 1.56kg/h) in order to evaluate their influence on the yield and composition of the volatile oil. Hydrodistillation with the same mean particle sizes was performed and used as a comparative method. The best supercritical fluid extraction conditions were found to be 90 bar, 40 °C, 1.10 kg/h and 0.6 mm. The chemical composition of each supercritical fluid extraction sample was analysed by GC and GC–MS and the global composition was compared with that obtained by hydrodistillation. The dominant components were linalool (65–79%), γ-terpinene (4–7%), camphor (3%), geranyl acetate (2–4%), α-pinene (1–3%), geraniol (1–3%) and limonene (1–2%). Moreover, supercritical fluid extraction samples were collected at specific intervals of amount of CO₂ consumed, during each extraction, and the contribution of the main volatile components from each sample, for the global volatile compositions, was evaluated. In general, the first sample of each extraction contained up to 50% of the mass of each component.     

超临界CO2萃取燕麦油的技术研究及其脂肪酸分析

利用正交实验设计,研究超临界CO2从燕麦麸皮中萃取燕麦油的工艺参数,且用GC-MS分析了燕麦油的脂肪酸组成,为开发功能性油脂提供一定的理论参数.实验结果表明,最佳工艺参数是压力15MPa、温度35℃、时间3h.所得燕麦油澄清透明,呈现金黄色,具有特殊的麦香味.其脂肪酸主要有棕榈酸、硬酯酸、反-9-十八碳烯酸、亚油酸、亚麻酸、顺-9-十八碳烯酸,相对含量分别为15.30%、2.24%、44.84%、33.81%、1.69%和2.12%,而且不饱和脂肪酸占82.26%.     

超临界CO2流体萃取打瓜籽油的工艺研究

采用超临界CO2流体从打瓜籽中萃取打瓜籽油。以打瓜籽油得率及亚油酸提取量为指标,采用单因素试验研究打瓜籽粉碎粒度、萃取压力、萃取温度、萃取时间对超临界CO2流体萃取打瓜籽油的影响。通过正交试验得到最佳萃取条件为:粉碎粒度80目,萃取压力30 MPa,萃取温度40℃,萃取时间20 min。在最佳萃取条件下,打瓜籽油得率为42.42%,亚油酸提取量为185.77 mg/g。     

Application of response surface methodology to optimise supercritical carbon dioxide extraction of oil from rapeseed (Brassica napus L.)

Supercritical CO₂ fluid extraction technology was used to extract oil from rapeseed. Extraction temperature, pressure, time and the sample particle size were selected and optimised by response surface methodology. Conventional solvent extraction was applied as a comparative method. The maximum extraction yield of 32.65 ± 1.01% was achieved at a temperature of 40 °C and a pressure of 345 bar, using an extraction time of 3 h and a 60‐mesh particle size. The chemical compositions of rapeseed oil using esterification method were investigated by GC–MS. The result indicates that the main fatty acids are palmitic acid (2.60%), oleic acid (16.54%), linoleic acid (9.62%), linolenic acid (4.77%), eicosenoic acid (11.20%) and erucic acid (47.09%), respectively. Supercritical fluid extraction has been proved to be an effective technique for extracting oil from Brassica napus L.     

Supercritical fluid extraction of fish oil from fish by-products: A comparison with other extraction methods

Fish and fish by-products are the main natural source of omega-3 polyunsaturated fatty acids, especially EPA (eicosapentaenoic acid) and DHA (docosahexaenoic acid), both of them with a great importance in the food and pharmaceutical industries. Comparing to conventional fish oil extraction processes such as cold extraction, wet reduction or enzymatic extraction, supercritical fluid extraction with carbon dioxide under moderate conditions (25 MPa and 313 K) may be useful for reducing fish oil oxidation, especially when fish oil is rich in omega-3 such as salmon oil, and the amount of certain impurities, such as some species of arsenic. Furthermore, taking profit of the advantages of supercritical carbon dioxide as extractive solvent, a coupled extraction-fractionation process is proposed as a way to remove free fatty acids and improve fish oil quality, alternatively to physical and chemical refining procedures.     

响应面法优化超临界CO2提取羊尾油工艺条件及理化性质研究

以羊尾油得率为考察指标,采用单因素和Box-Behnken响应面试验优化超临界CO₂提取阿勒泰大尾羊尾油的工艺条件,并对羊尾脂肪和羊尾油的理化指标进行了测定。当脂肪大小为1.41 cm³,萃取温度为49.28℃,萃取时间为3.31 h,萃取压力为25 MPa的条件下,羊尾油得率达到最高84.61%。羊尾粗脂肪含量为(88.01±0.025)%。羊尾油主要脂肪酸为油酸(40.26±0.047)%、棕榈酸(28.48±0.046)%、硬脂酸(14.27±0.044)%、肉豆蔻酸(8.49±0.017)%。可以为羊尾油的提取及工业应用提供依据。     

Clustering of instrumental methods to characterize the texture and the rheology of slimy okra (Abelmoschus esculentus) suspensions

Okra (Abelmoschus esculentus) is one of the ingredients widely used in African gastronomy because of the unique slimy texture it gives to sauces. However, processing and formulation can affect the textural and rheological properties of these sauces, leading to unacceptable quality for the African consumer. The aim of this study was to select the instrumental measurements best enabling (a) characterization of the rheology and texture of slimy sauces prepared from okra and (b) monitoring its evolution during the preservation process. Thirty-seven slimy suspensions (sauces and purées) were measured with 16 rheological and textural parameters. A principal component analysis revealed that flow consistency index K and flow behavior index n were well correlated with visco-elastic, adhesive, and shear thinning properties, and that stringiness was well correlated with elongational, cohesive, and ductile properties. These two sets of measurement methods are sufficient to characterize their rheological and textural properties, and necessary to discriminate them according to their process and formulation.     

Changes in chemical composition of lupin seeds (Lupinus angustifolius) after selective α‐galactoside extraction

A selective procedure for the extraction of α‐galactosides has been employed in two sweet lupin seeds (Lupinus angustifolius var. Troll and var. Emir) in order to reduce flatulence‐causing factors. Different nutritional parameters (proteins, fat, ash, dietary fibre, starch, sucrose, vitamins B₁, B₂, E and C) and antinutritional factors (α‐galactosides, trypsin inhibitor activity and inositol phosphates) were studied in raw and processed seeds. The α‐galactoside content in both varieties was reduced by 87–100%. The extracted lupins seeds presented a high retention in protein and fat (109–136% and 95–104%, respectively). Sucrose and soluble dietary fibre, however, decreased significantly as a result of processing and retentions ranged between 5 and 29%. The vitamin B₁, B₂, and E contents decreased during selective extraction, the retentions being in the ranges 25–47%, 38–40%, and 48–54%, respectively, for var. Troll and Emir. However extracted lupin seeds still contained important amounts of vitamins and insoluble dietary fibre, compounds with nutritional importance. Raw and processed lupins did not contain starch. TIA and vitamin C were not detected, and total inositol phosphates were modified slightly after extraction. In conclusion, the lupin seeds obtained by the extraction of α‐galactosides can be an adequate proteic ingredient to be incorporated in functional foods. Copyright © 2005 Society of Chemical Industry