Critical Fluid Extraction Research Articles

Antimicrobial Activity of Extract and Fractions of Different Parts and GC-MS Profiling of Essential Oil of Cichorium intybus Extracted by Super Critical Fluid Extraction

Antimicrobial Activity of Extract and Fractions of Different Parts and GC-MS Profiling of Essential Oil of Cichorium intybus Extracted by Super Critical Fluid Extraction

The effect of assorted pretreatments on cellulose of selected vegetable waste and enzymatic hydrolysis

Pretreatment of biomass for the production of biofuels and value added products involves physical disruption of the polymeric linkages of lignocellulosic material which enhances the accessibility of lignocellulases and removes lignin. To investigate the impact of assorted pretreatments on structural changes, low lignin containing vegetable waste was selected as the biomass source. The combined effects of NaCl under different physical conditions on the biomass material were evaluated. Amounts of soluble sugars, monomeric phenols, holocellulose, inhibitors of hydrolysis and fermentation formed were determined. Physical and microstructural alterations of the material were analysed by XRD, FTIR and SEM. Accessibility of enzymes to the cellulose material was evaluated by quantifying the release of sugars in enzymatic hydrolysis for various pretreatment methods. The data revealed that pretreatment with NaCl is cost effective, ecofriendly and the process efficiency is comparable with common pretreatment methods like alkali, acid, ammonia, super critical fluid extraction etc. This is the first report on the use of sodium chloride for the pretreatment of vegetable waste.

Bioguided Fractionation and Purification of Natural Bioactives Obtained from<i>Alpinia conchigera</i> Water Extract with Melanin Inhibition Activity

Crude extracts of Alpinia conchigera a species from the Malaysian Ginger (Zingiberaceae) family and its fractions obtained from various extraction methods were assayed for melanogenesis inhibition activity and cell viability. The crude extract obtained from the ethanolic extraction and the super critical fluid extraction did not exhibit significant melanin inhibition activity and was shown to be toxic to the melanocyte cells in comparison to the water extract. The crude aqueous extracts displayed melanin inhibition of 96.38 ± 1.60% and cell viability 109.90 ± 8.32% at a concentration of 500 μg/mL. Bioassay guided fractionation was performed on the water extracts to isolate the active compounds. The actives were identified as trans-cinnamaldehyde and chavicol glucopyranoside with both compound showing potent anti-melanogenesis activity. At 4.9 μg/ml, both trans-cinnamaldehyde and chavicol glucopyranoside gave 85% inhibition of melanin formation in vitro with 77% and 97% cell viability respectively. In comparison, kojic acid, a known skin lightening agent showed 90.0% inhibition at 100 μg/mL. The bioactive composition comprising the extract, active fraction, purified compounds or mixture thereof of Alpinia conchigera may be used for cosmetic and pharmaceutical applications, particularly for the purposes of reducing skin pigmentation.

문관나무 종자유의 이화학적 특성 분석

본 연구는 문관나무 종자유로부터 새로운 유지자원으로의 활용 가능성을 평가하기 위하여 여러 가지 이화학적 특성 분석을 하였다. 문관나무 종자유를 초임계 추출(420 atm, 50℃), 헥산 추출, 가열압착(160℃, 180℃) 방법으로 추출하였다. 그 결과 추출 수율은 헥산 추출이 53.5±2.5%로 가장 높았으며, 다음으로 160℃ 가열압착 추출이 48.3±6.5%, 180℃ 가열압착 추출과 초임계 추출은 각각 44.7±1.7%, 44.7±2.5%의 수율을 보였다. 산가를 측정한 결과, 초임계 추출 종자유가 3.44 mg/g으로 가장 높았으며 가열압착 추출 종자유가 1.3 mg/g 정도로 가장 낮았다. 문관과 종자유의 과산화물가를 측정한 결과, 가열압착 추출 종자유(160℃)가 3.10meq/kg으로 가장 높았으며 다음으로 가열압착 추출 종자유(180℃)가 2.36 meq/kg, 헥산 추출 종자유와 초임계 추출 종자유가 각각 1.59, 1.13 meq/kg 순으로 나타났다. 문관나무의 종자유로부터 지방산 조성을 분석한 결과 oleic acid(C18:1)와 linoleic acid(C18:2)가 60% 이상 함유되어 있었다. 또한 문관나무 종자유의 총 phytosterol 실험 결과 가열압착 추출 종자유(160℃)의 함량이 65.91±0.62 mg/100 g으로 가장 높았다. 본 연구는 문관나무 종자유의 추출방법별 이화학적 특성 분석을 통해 문관나무 종자유 활용에 대한 기초자료로 활용될 수 있을 것으로 판단된다.

Near critical and supercritical fluid extraction of Cu(II) from aqueous solutions using a hollow fiber contactor

The aim of this work is the experimental and theoretical characterization of the mass transfer in a membrane-based dense gas extraction of metal ions from aqueous solutions using a hollow fiber contactor. Extractions of Cu(II) were conducted in a single fiber membrane contactor operating under steady state conditions. Aqueous CuSO4 solutions were treated using a CO2 phase containing 1,1,1-trifluoro-2,4-pentanedione (TFA) or 1,1,1,5,5,5-hexafluoro-2,4-pentanedione (HFA) at 40°C and pressures ranged between 70 and 90bar.Experiments show that the use of dense CO2 as extraction solvent of Cu(II) ions reaches extraction efficiencies valued up to 98.7%. Simultaneously, a mass transfer model was proposed correlating an effective rate function of the complex formation at the aqueous-CO2 interface.The highest extraction efficiencies were observed at higher pressures and lower pH values, which could confirm that a high content of protons is required to facilitate and stabilize the formation complex by means of keto-enol tautomerism.This work represents the first step in order to propose a novel intensified operation, which could be applied for high valued metals or hazardous materials.

Development and application of a methodology for the recovery of high added value products from peach industry waste

Every year, in Greece, more than 300.000 tones of peach fruit (Prunus persica), are used to produce juices and canned products. Consequently, thousands tones of fruit waste are discarded, aggravating annually the environment by a total of 3 million m3 of liquid and 23.000 tones of solid waste. Peach solid and liquid wastes are rich in phytochemicals like phenolics and carotenoids that have high economic added value, due to their remarkable biological activities that find many applications in food, cosmetic and pharmaceutical industries. Within this project we have developed and apply a method for the recovery of polyphenols with an eco friendly approach using mainly the Adsorption Resin Technology. The methodology has been applied in lab and in pilot scale. In pilot scale 200kg peach pulp were treated with 25kg resin XAD4 type in order to recover polyphenolic compounds. Using a few simple steps of separations we have isolated and identified several phenolic compounds that belong to flavonoids (e.g.luteolin, prunin), phenolic acids (e.g. cafeic acid), lactones (e.g. D-decalactone) and triterpens (e.g.3-epi maslinic acid). In addition, the peach kernel that is another by-product of the industry has been submitted successfully to Super Critical Fluid extraction and we have obtained, in good yields, the kernel oil that is also known as “persic oil” and has commercially high added value in cosmetic industry.

Extraction of Curcumin

Curcumin due to its various medicinal, biological, pharmacological activities is high on demand and has high market potential, high cost. Since curcumin has variety of uses, extracting it in a less expensive method other Super Critical Fluid Extraction is the main aim or objective of this work. Usage of food grade solvents is a main prerequisite of this work and optimization of the parameters in order to find an effective means of extraction sum ups the cause of this project work. Besides working on the extraction of curcumin, other properties such as curcumin's antioxidant, antimicrobial properties are to be envisaged upon. This project work mainly deals with the topic on 'extraction of curcumin' from its common source turmeric, using an effective low cost method of solvent extraction. Different solvents are used either in their pure form or being mixed in definite ratio's, while taking into consideration of other parameters such as particle size, time, temperature, solid: solvent ratio. The qualitative analysis of its antimicrobial property is also done along with the product development of Cake. Keywords - Antiflatulent, Antifibrotic, Antimutagenic, Carcinogenesis, Ulcerogenic 1.1 Chemical composition of turmeric Turmeric contains protein (6.3%), fat (5.1%), minerals (3.5%), carbohydrates (69.4%) and moisture (13.1%). The essential oil (5.8%) obtained by steam distillation of rhizomes has a-phellandrene (1%), sabinene (0.6%), cineol (1%), borneol (0.5%), zingiberene (25%) and sesquiterpines (53%)5. Curcumin

A simple model for super critical fluid extraction of bio oils from biomass

A simple mathematical model to characterize the supercritical extraction process has been proposed in this paper. This model is primarily based on two mass transfer mechanisms: solubility and diffusion. The model assumes two districts mode of extraction: initial constant rate extraction that is controlled by solubility and falling rate extraction that is controlled by diffusivity. Effects of extraction parameters such as pressure and temperature on the extraction of oil have also been studied. The proposed model, when compared with existing models, shows better agreement with the experimental results. The proposed model developed has been applied for both high initial oil content material (cashew nut shells) and low initial oil content material (black pepper).

Critical fluid extraction of Juniperus virginiana L. and bioactivity of extracts against subterranean termites and wood-rot fungi

Eastern red cedar ( Juniperus virginiana L.) is an abundant renewable resource and represents a vast potential source of valuable natural products that may serve as natural biocides. Both the wood and needles from J. virginiana were extracted using liquid carbon dioxide (L-CO 2) as well as ethanol (EtOH) and the yields determined. Wood blocks were vacuum impregnated with the extracts and subsequently tested for resistance against eastern subterranean termites ( Reticulitermes flavipes) and two species of brown-rot fungi ( Gloeophyllum trabeum and Postia placenta). Cedarwood oil (CWO) yields (fresh weight) were 2.3% and 5.9% using L-CO 2 (CWO-CO 2) and EtOH (CWO-EtOH), respectively. The yield (i.e., fresh weight) of juniper leaf oil using EtOH was 6.6% of the unground needles. Laboratory termite testing indicated that the ethanol extract of needles was lethal to the termites and resulted in no damage to the test blocks. The CWO-CO 2 and the CWO-EtOH treatments were statistically equivalent and both exhibited significant resistance to termite damage compared to untreated controls. The CWO extracts were significantly more effective against G. trabeum than P. placenta. For G. trabeum, the CO 2-derived CWO was statistically equivalent to the uninoculated control. On the other hand, for P. placenta, only the EtOH-derived CWO conferred any significant inhibition. The ethanol extract of the needles did not inhibit either test fungus. These extracts from J. virginianna may provide a renewable source of safe natural wood preservatives.

Comparison of the effects of critical fluid and reflux-extracted techniques on cornstarch pasting properties

Critical fluid extraction of native lipids from cornstarch using 75/25 (v/v) ethanol/water as the solvent removed over 99% of the native lipid. The percentage of native lipid extracted was altered by changing the solvent/starch ratio. The pasting properties and shear storage modulus of a defatted, critical fluid-extracted sample differed from those of a sample defatted by refluxing with 75/25 (v/v) n-propanol/water, although both samples contained only trace amounts of residual native lipid. The percent soluble starch in the lipid-extracted starches was higher than that of the control starch, which was expected since extraction of native lipids reduced the amount of lipid-complexed amylose within the starch granule and enabled more intragranular amylose to be leached out. This study describes a convenient, non-toxic process for extracting native lipids from cornstarch, and the altered pasting and gelling properties of these extracted starches could result in new end-use applications.

Effects of critical fluid lipid extraction on the gelatinization and retrogradation of normal dent cornstarch

Critical fluid extraction of native lipids from cornstarch using 80/20 (v/v) CO 2/ethanol and 100% ethanol was carried out in order to see what effects each solvent would have on the starch pasting profile. The results were compared with cornstarch defatted by refluxing with 75/25 (v/v) n-propanol/water. Pure ethanol extracted more native lipid than CO 2/ethanol, and extraction improved when the initial moisture content of the starch was increased from 10% to 19%. Granules became less swollen and less deformable with increased lipid extraction. Paste viscosity studies carried out at starch concentrations less than 8% yielded lower peak and setback viscosities of lipid-extracted cornstarch relative to native cornstarch. However, above 8% starch concentration, swollen granules were in more intimate contact, and the added rigidity caused by lipid extraction yielded much higher peak viscosities relative to the starch control. Lipid-extracted cornstarch samples at concentrations above 8% showed plateau rather than peak viscosities reflecting the limited swelling power of the granules, and the defatted samples displayed less viscosity breakdown due to their increased granule rigidity.

Cuticular wax from flax processing waste with hexane and super critical carbon dioxide extractions

The waste material produced when flax fiber is processed has potentially valuable co-products. The dust was extracted with CO 2 under super critical fluid extraction (SCFE) conditions or hexane to isolate the cuticular waxes that contain policosanols. Policosanol is a general term for long chain alcohols and have been shown to improve blood chemistry. SCFE yielded 7.4% wax compared with 4.0% with hexane. There were slight but statistical differences in extract compositions for C-20, C-22, and C-26 alcohols and larger significant differences for C-16, C-18, and C-20 fatty acids depending upon the extraction methods used. Recovery of wax from the waste produced from flax processing can provide an attractive value added product with positive health benefits.

Extraction of cashew ( Anacardium occidentale) nut shell liquid using supercritical carbon dioxide

This work investigated the extraction of cashew nut shell liquid (CNSL) using supercritical carbon dioxide (SC-CO 2). Effects of process parameters such as extraction pressure, temperature and flow rate of SC-CO 2 were investigated. The yield of CNSL increased with increase in pressure, temperature and mass flow rate of SC-CO 2. However, under different operating conditions, the composition of CNSL varied. The study of physical properties and chemical composition of the oil obtained through super critical fluid extraction (SCFE) showed better quality as compared to the CNSL obtained through thermal route. Experimental results were compared with diffusion based mass transfer model. Based on this simple model, extraction time was optimized.

Microbial and enzymatic methods for the removal of caffeine

Caffeine is a purine alkaloid and is a major constituent of coffee, tea and other beverages. It acts as a central nervous system stimulant and also has negative withdrawal effects. Decaffeinated beverages are being used to overcome its negative effects. Decaffeination is done by different methods like solvent, water and super critical fluid extraction. These methods apart from being non-specific are expensive and involve the usage of toxic organic solvents. Development of a process involving an enzymatic (specific) degradation of caffeine to non-toxic compound is necessary to solve the problems of chemical extraction of caffeine in food products as well as treating the caffeine containing waste products. The different microbial and enzymatic methods of caffeine removal are discussed in this review. The literature revealed that major caffeine degrading strains belong to Pseudomonas and Aspergillus. Though the enzymes involved in degradation of caffeine by microorganisms are known, in vitro enzymatic studies for caffeine degradation is not yet reported.

Purification and some properties of Cu,Zn superoxide dismutase from Radix lethospermi seed, kind of Chinese traditional medicine

Copper–zinc superoxide dismutase (Cu,Zn SOD) has been extracted, purified and characterized from Radix lethospermi seed (RLS), a kind of Chinese traditional medicine. Before extraction, the lipid was removed by super critical fluid extraction (SCF). Partial protein fractionation in the crude extract was affected by using 50–75% (NH 4) 2SO 2. Subsequently, superoxide dismutase was fractionated by column chromatographies on DEAE-52, Sephadex G-200 and DEAE-52 again. Pure Cu,Zn SOD had a specific activity of 4843 U/mg protein and was purified 267.2-fold, with a yield of 23.55%. The purified enzyme has a molecular weight of about 30,500 ± 100 and is composed of two non-covalently joined equal subunits. Purity was confirmed by Sodium dodecyl sulphate-polyacrylamide gel electrophoresis (SDS-PAGE), HPLC and mass spectroscopy. Amino acid content has been investigated. The enzyme was found to remain stable in the pH range 6.0–9.0 at 25 °C and up to 45 °C at pH 7.8 for a 30 min incubation period. RLS Cu,Zn SOD appeared to have significant thermal stability lower than other Cu,Zn SODs, as revealed by irreversible heat inactivation at 60 °C. The enzyme was not inhibited by DTT, NaN 3 and β-mercaptoethanol, but was inhibited by cyanide and hydrogen peroxide. Finally, in the presence of 2 mM ethylendiamine tetra acetic acid (EDTA) and sodium dodecyl sulphate (SDS), the enzyme showed approximately 18 and 34% activity loss.

A benchmark assessment of residues: comparison of Athabasca bitumen with conventional and heavy crudes

Compared to benchmark crude oils, bitumen does not respond well to conventional upgrading processes. In order to improve our understanding of this problem, we compare the chemical and physical properties of fractions from super critical fluid extraction of bitumen pitch with the corresponding fractions of residua from Venezuelan heavy oil, a Saudi Arabian light crude and a Chinese Daqing conventional crude.Relatively minor differences in chemical structure were observed between the corresponding residua fractions from Athabasca bitumen, Venezuelan heavy oil and Saudi Arabian light crude. Only the Chinese Daqing showed significant variance; this sample is much more aliphatic and has greater geometrical dimensions than the corresponding samples from the other residua.The end-cut from Athabasca bitumen pitch contained ultra-fine solids together with much higher levels of nickel, vanadium and nitrogen than the conventional crude end-cuts. These components are among the most intractable in upgrading and could be responsible for the problems encountered in bitumen upgrading, especially by catalytic processes.

Application of spectral fluorescence microscopy for the characterization of Athabasca bitumen vacuum bottoms

The relationship between visible light region fluorescence properties and gross chemical composition of ten narrow cut subfractions of Athabasca bitumen separated by super critical fluid extraction has been studied. The objective of this investigation was to evaluate the potential for utilizing spectral fluorescence microscopy for empirically assaying the chemical composition (e.g. wt% saturates, aromatics, resins and asphaltenes) of the bitumen fractions. Two spectral parameters were used to characterize the bitumen fluorescence properties: Lambda max ( L max in nm) or the wavelength of maximum emission intensity, and Q, which is the ratio of intensity at 650 nm to the intensity at 500 nm. Positive linear relationships with high r 2 values were established for L max and Q parameters, which correlated with the wt% of resins plus asphaltenes, aromatic carbon, C/H atomic ratio and wt% of S. In addition, the fluorescence properties displayed a progressive red shift to longer wavelengths. L max and Q versus saturate/aromatic ratio and wt% saturates showed a negative linear relationship consisting of two distinct linear segments. Although L max and Q increased up to about 550 nm and 1.0, respectively, they showed a progressive red shift in the second segment that was accompanied by a decrease in both values. Weight per cent aromatics exhibited a polynomial (?) relationship with fluorescence properties, which may reflect variations in the proportion of mono- and di-aromatics relative to cata-condensed aromatics within the Athabasca bitumen subfractions.

Multiresidue Analysis of Pesticides in Fresh Fruits and Vegetables by Supercritical Fluid Extraction and HPLC.

A screening method was established for the determination of 27 pesticides in fresh fruits and vegetables by a super critical fluid extraction (SFE), cleaned up with cartridge columns and HPLC. The multiresidue and semiautomatic analysis was useful for a screening examination, because the determination methods for pesticides under the Japanese Food Sanitation Law are mostly individual determinations. Reported methodologies for multiresidue analysis by HPLC were not adequate to regulated pesticides in Japan. In this report, multiresidue determination of pesticides and their metabolites are discussed using SFE and HPLC. Details of the proposed method are as follows : Wet samples such as fruits and vegetables were not suitable for the SFE instrument, so the water in the samples was removed with an absorptive polymer (Arasorb[○!R] S-310) prior to SFE. The pesticides were extracted by SFE, the extracts trapped with Extrelut[○!R] NT + Bond Elut[○!R] C18 and then eluted with acetonitrile. The eluate was cleaned up with Sep-Pak[○!R] Florisil+Bond Elut[○!R] PSA cartridges. After washing with n-hexane, the pesticides were eluted from the cartridges with 15% ether/n-hexane, 15 and 50% acetone/n-hexane. These three fractions were individually determined by HPLC with a photodiode-array detector. The pesticides spiked in samples at 0.5ppm showed satisfactory recoveries except for thiabendazole, imazalil and clofentezine. Detection limits were 0.005-0.01ppm for the 27 pesticides.

A rapid method (SFE-TLC) for the identification of irradiated chicken

Cyclobutanones have successfully been used as chemical markers to identify irradiated food. However, existing methods for the isolation of cyclobutanones from the sample matrix often involve a long extraction (6 h) followed by a tedious clean-up regime (overall analysis time 72 h). Two alternative methods of isolation were investigated with a view to reducing the extraction and overall analysis time. Both methods (Soxtec and super critical fluid extraction (SFE)) were found to be rapid (45 min and 20 min respectively) and compared favourably to the existing method. Using the faster of the alternative methods of extraction (SFE), a simple and rapid (2 h) screening method for the detection of irradiation in food is reported.

A group contribution equation of state for associating mixtures

In the present work a group contribution-associating-equation of state (GCA-EOS) is developed for the modeling of phase equilibria found in the near critical fluid extraction and dehydration of oxygenated compounds from aqueous solutions. The new equation of state is obtained by the inclusion of a ‘group’ contribution associating term to the GC-EOS model. The definition of a unique hydroxyl group to represent the association effect of hydrogen bonding in water and alcohols, greatly simplifies the extension of the model to multicomponent mixtures. This approach has been applied to determine the parameters for a common hydroxyl group for water, primary and secondary alcohols. On this basis, revised group and binary interaction dispersive parameters for water, primary and secondary alcohols, alkane groups, light hydrocarbons and CO 2 have been determined. Model predictions for binary and ternary data are presented.