Isolation and Extraction of Total Flavonoids from Epimedium Koreanum Nakai by Supercritical Fluid Extraction

In the present paper is reported the method for the isolation and extraction of total flavonoids of Epimedium Koreanum Nakai by means of supercritical fluid extraction(SFE). By examining pressure, temperature, amounts of modifier and extraction time, the optimized condition of SFE is confirmed as 30 MPa and 60 ℃, with 70% ethanol as the modifier. The samples were statically extracted for 30 min, followed by dynamic extraction for 120 min at a flow rate of 6 mL/min. The quantitative analysis of total flavonoids was performed by UV-Vis spectrophotometry. Compared with the conventional method, the SFE method is more efficient, more rapid and more friendly environmentally.

Simultaneous determination of amino acids in different teas using supercritical fluid chromatography coupled with single quadrupole mass spectrometry

Tea is a widely consumed beverage and has many important physiological properties and potential health benefits. In this study, a novel method based on supercritical fluid chromatography coupled with mass spectrometry (SFC-MS) was developed to simultaneously determine 11 amino acids in different types of tea (green teas, Oolong tea, black tea and Pu-erh tea). The separation conditions for the analysis of the selected amino acids including the column type, temperature and backpressure as well as the type of additive, were carefully optimized. The best separation of the 11 amino acids was obtained by adding water (5%, v/v) and trifluoroacetic acid (0.4%, v/v) to the organic modifier (methanol). Finally, the developed SFC-MS method was fully validated and successfully applied to the determination of these amino acids in six different tea samples. Good linearity (r ≥ 0.993), precision (RSDs≤ 2.99%), accuracy (91.95%-107.09%) as well as good sample stability were observed. The limits of detection ranged from 1.42 to 14.69 ng/mL, while the limits of quantification were between 4.53 and 47.0 ng/mL. The results indicate that the contents of the 11 amino acids in the six different tea samples are greatly influenced by the degree of fermentation. The proposed SFC-MS method shows a great potential for further investigation of tea varieties.

Supercritical Fluid Extraction of Total Flavonoids from Leaves of Acanthopanax Senticosus Harms

The herbal plant Acanthopanax Senticosus Harms is natural herb of Changbaishan in Jilin Province of China, which belongs to the Araliaceae family. As the ingredients of folk medicine, it has long been used to treat a variety of human diseases, such as cerebrovascular disease, diabetes, tumor, isochemic heart diseases, hypertension, rheumatic arthritis, etc. E2,33. Flavonoids, a class of constituent compounds, which have a broad distribution in the nature and are found in Acanthopanax Senticosus Harms, have gained particular attention. A number of studies have shown that flavonoid compounds have wide biological activities, such as anti-aging, anticancer, anti-HIV,

Preparation of TiO_2-MoO_3 nano-composite photo-catalyst by supercritical fluid dry method

A series of TiO 2-MoO 3 nano-composite photocatalysts were prepared by supercritical fluid dry method(SCFD) and an impregnation technique with TiCl 4 and (NH 4) 6Mo 7O 24 ·4H 2O as the starting materials. The catalysts were characterized by the means of XRD, TEM and UV-Vis. Methyl orange was used as model compound for the evaluation of their catalytic activities. The results indicated that the photo-catalyst prepared by SCFD had the advantages of small size(12.84 nm), narrow distribution and good dispersivity. The presence of small amount of Mo in composite catalyst gives rise to the red shift of its absorbance wavelength, decrease of its energy gap and increase of the utility of visible light. Furthermore, higher surface acidity of the photo-catalyst was obtained as the result of the addition of MoO 3. Compared with pure TiO 2, the catalytic activity of the TiO 2-MoO 3 nano-composite photo-catalyst was improved significantly. As the doping concentration of the composite catalysts was controlled at 0.6%(molar percentage), 100% degradation of methyl orange was achieved with in 1.2 h irradiation time.

Recent progress in supercritical fluid science for biofuel production from woody biomass

Owing to an environment-friendly utilization of resources, increased attention has been focused on fuels and chemicals from biomass as an alternative to fossil resources. In addition, supercritical fluid technology has been considered to be an environmentally-benign treatment. Therefore, its technology was applied for a conversion of biomass to useful fuels and chemicals in order to mitigate environmental loading. For example, supercritical water treatment has demonstrated that lignocellulosics can be hydrolyzed to become lignin-derived products for useful aromatic chemicals and carbohydrate-derived products, such as polysaccharides, oligosaccharides and monosaccharides of glucose, mannose and xylose used for subsequent ethanol fermentation. If this treatment is prolonged, lignocellulosics were found to be converted to organic acids such as formic, acetic, glycolic and lactic acids which can be converted to methane for biofuel. When alcohols, such as methanol and ethanol, were used instead of water, some other useful products were achieved, and its liquefied products were found to have a potential for liquid biofuel. In this study, therefore, our research achievements in supercritical fluid science of woody biomass will be introduced for clean and green chemistry for a sustainable environment.

Advances of supercritical fluid chromatography in lipid profiling

Supercritical fluid chromatography(SFC) meets with great favor due to its high efficiency, low organic solvent consumption, and the specialty for the identification of the isomeric species. This review describes the advances of SFC in targeted and untargeted lipid profiling. The advancement of the SFC instruments and the stationary phases are summarized. Typical applications of SFC to the targeted and untargeted lipid profiling are discussed in detail. Moreover, the perspectives of SFC in the lipid profiling are also proposed. As a useful and promising tool for investigating lipids in vitro and in vivo, SFC will predictably obtain further development.

Improved dissolution and bioavailability of silymarin delivered by a solid dispersion prepared using supercritical fluids

The objective of this study was to improve the dissolution and bioavailability of silymarin(SM).Solid dispersions(SDs)were prepared using solution-enhanced dispersion by supercritical fluids(SEDS)and evaluated in vitro and in vivo,compared with pure SM powder.The particle sizes,stability,and contents of residual solvent of the prepared SM-SDs with SEDS and solvent evaporation(SE)were investigated.Four polymer matrix materials were evaluated for the preparation of SM-SD-SEDS,and the hydrophilic polymer,polyvinyl pyrrolidone K17,was selected with a ratio of 1:5 between SM and the polymer.Physicochemical analyses using X-ray diffraction and differential scanning calorimetry indicated that SM was dispersed in SD in an amorphous state.The optimized SM-SD-SEDS showed no loss of SM after storage for 6 months and negligible residual solvent(ethanol)was detected using gas chromatography.In vitro drug release was increased from the SM-SDSEDS,as compared with pure SM powder or SM-SD-SE.In vivo,the area under the rat plasma SM concentration-time curve and the maximum plasma SM concentration were 2.4-fold and 1.9-fold higher,respectively,after oral administration of SM-SD-SEDS as compared with an aqueous SM suspension.These results illustrated the potential of using SEDS to prepare SM-SD,further improving the biopharmaceutical properties of this compound.

Supercritical Fluid Extraction of Saponins from Ginseng

Introduction Ginseng（ Panax ginseng C. A. Meyer, Araliaceae） is one of the most valuable Chinese crude drugs and has been used widely for over 2000 years. Studies have demonstrated that ginseng can act on the central nervous system, the cardiovascular system and the endocrine system; it can enhance immune function and metabolism; it possesses a biomodulation action, anticancer effect, anti-stress and anti-ageing activities, and so on.

Synthesis of Ti-Ce-Si Binary and Ternary Nanocomposite Photocatalyst by Supercritical Fluid Drying Technology

Ti-Ce, Ti-Si binary and Ti-Ce-Si ternary novel nanocomposite oxide photocatalysts were prepared with cheap inorganic salts TiCI4, Na2SiO3·9H2O and Ce（NO3）3·6H2O as precursors by supercritical fluid drying （SCFD） technology. The catalysts were characterized by means of XRD and TEM. The particle size of nanocomposite oxide photocatalysts synthesized by SCFD method is about 6 - 11 nm, which is smaller than those obtained by common drying method （CD）. The phase transformation from anatase to rutile was inhibited by SCFD technology. The peaks of SiO2 and CeO2 in XRD patterns indicate that a SiO2 amorphorous phase exists in all the samples and CeO2 is well dispersed on the surface of TiO2. The orthogonal test was designed to optimize the preparing conditions. It is found that ceria dop;.ng enhances the photocatalyric activity markedly, and the optimum doping of CeO2 is 0.1%. The thermal stability of photocatalyst can be improved ; the growth of particle-size and the decrease of surface area can be prohibited by doping of SlOe. Heat-treatment is a necessary factor to induce chemistry change of Ti-Si surface. The optimum heat-treating temperature is 600℃. A novel and efficient Ti-Ce-Si ternary nanocomposite was prepared by SCFI） method with strong thermal stability and high photoactivity in the photodegratation of phenol.

Synthesis and Characterization of TiO_2-CeO_2 Nanocomposite by Supercritical Fluid Drying

TiO_2-CeO_2 nanocomposite particles were prepared with Ce(NO_3)_3·6H_2O and TiCl_4 as precursors by the codeposition method and supercritical fluid drying (SCFD) technology. The particles prepared were characterized by means of XRD, TEM and FTIR. The results show that SCFD can give rise to the direct synthesis of the anatase TiO_2-CeO_2,and the particle size is 6～11 nm under 500 ℃ thermal-treated,smaller than that by common drying (CD). The phase transformation from anatase to rutile is inhibited by supercritical fluid drying technology. The peak of CeO_2 is not observed in XRD patterns,Ce-O band vibration was present in FTIR spectrum,which indicates that CeO_2 is well dispersed on the surface of TiO_2.

Optimization of conditions for supercritical fluid extraction of flavonoids from hops (Humulus lupulus L.)

Waste hops are good sources of flavonoids. Extraction of flavonoids from waste hops (SC-CO2 extracted hops) using supercritical fluids technology was investigated. Various temperatures, pressures and concentrations of ethanol (modifier) and the ratio (w/w) of solvent to material were tested in this study. The results of single factor and orthogonal experiments showed that at 50 °C, 25 MPa, the ratio of solvent to material (50%), ethanol concentration (80%) resulted in maximum extraction yield fla- vonoids (7.8 mg/g). HPLC-MS analysis of the extracts indicated that flavonoids obtained were xanthohumol, the principal prenylflavonoid in hops.

Review: Isomer Separation, Chiral Resolution, and Structure Elucidation Analyses Are the Future of Analytical Supercritical Fluid Chromatography—Mass Spectrometry

In 1822, almost 200 years ago, Baron Charles Cagniard de Latour (1777-1859) discovered the critical phenomena or critical state [1] [2]. At that time, it was described as a curiosity. However, it is now used as an advanced extraction and analytical technology in industry and research. Extraction with supercritical fluids (SFs) was welcome from the very beginning. In the present paper, the application to chromatography of the critical phenomena of compressed gases or overheated liquids as supercritical fluids will be discussed. Supercritical Fluid Chromatography (SFC) received an uneasy welcome, mainly because of the lack of commercially available analytical instruments. Even today, only a small number of industrial companies are manufacturing SFC instrumentation. A very small spectrum of columns is manufactured specially for SFC. SFC is not accepted by Pharmacopeia committees for the analysis of drugs and medical forms to the same extent as Gas Chromatography, High-Performance Liquid Chromatography or even Thin Layer Chromatography. The present status and future perspectives for SFC will be discussed.

Determination of polycyclic aromatic hydrocarbons with supercritical fluid extraction and chromatography（SFE／SFC）

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PURIFICATION OF BILIRUBIN AND MICRO-PARTICLE FORMATION WITH SUPERCRITICAL FLUID ANTI-SOLVENT PRECIPITATION

1 INTRODUCTIONA supercritical fluid is one existing at temperatures and pressures above its criticalpoint values(T_c,p_c) [1].Supercritical fluid has unconventional thermophysical prop-erties,exhibiting higher density,greater compressibility,lower viscosity between the gasand liquid extremes.Its solute binary diffusion coefficient is considerably higher thanthat in liquids[2-4].Supercritical fluid extraction(SFE)has been suggested as a viablealternative to other separation technologies.

Separation of Sesamin and Sesamolin by a Supercritical Fluid-Simulated Moving Bed

This work shows how the sesamin and sesamolin in sesame seed can be extracted, enriched and purified by the related technologies of supercritical carbon dioxide. Sesame oil is first obtained from the sesame seeds by supercritical carbon dioxide extraction (SFE);lignans in the oil are enriched and precipitated as the top product by supercritical fluid fractionation technology (SFF);the crude lignans are then separated by supercritical fluid-simulated moving bed chromatography (SF-SMB) to obtain pure sesamin and sesamolin. The simulated moving bed is a continuous chromatography;the use of supercritical carbon dioxide as the desorbent simplifies the downstream treatment. By experimental validation, this work also shows that replacing liquid by SF as the desorbent for the SMB automatically creates a gradient operation for the SMB and enlarges the separable range of the operating conditions. Both the design and operation of the SF-SMB are introduced in this paper. The application of SF-SMB to the separation of sesamin and sesamolin provides a novel example for demonstrating the diversity of SF and the potential applications for the production of natural products and the development of botanical drugs.

Separation of Enantiomers of Clopidogrel on Chiral Stationary Phases by Packed Column Supercritical Fluid Chromatography

A packed column supercritical fluid chromatography (SFC) method for the separation of clopidogrel enantiomers on a chiral stationary phase and CO2 with modifier as mobile phase has been developed at an analytical scale. Among 11 different 2 stationary phases the Chiral cel OD-H column showed by far the best separation properties. The influence of different modifiers, injection solvents, temperature, and pressure, and density of the fluid, respectively, on the separation behaviour has been studied. It was found that the separation behaviour strongly depends on the type of modifier and the modifier content. Temperature and pressure are of less influence.

Effect of process parameters on the recrystallization and size control of puerarin using the supercritical fluid antisolvent process

The purpose of this study was to investigate the influence of the supercritical CO2 processing on the particle size and morphology of puerarin crystals. The process parameters included solvents, temperature, pressures, antisolvent times, addition volumes, antisolvent addition rates and solute concentrations. After being processed, the dramatic reduction of the dimensions and the change of the crystal shape were noticed. Decreasing the antisolvent addition rate, increasing the temperature and the addition volume below 50 ml led to a decrease in size. The new crystal of puerarin generated at the optimal conditions was 30.34 μm.The solvent of methanol and the concentration of 60 mg/ml were found to determine the type and degree of crystallinity of particles. These results showed that this process has the potential to produce a drug recrystallization product with newly generated crystal forms and the size of drug particles could be controlled through the tuning of various experimental conditions.

Impregnation of Crushed Stone with Bitumenous Compounds Using Propane/Butane Impregnation Process Carried out in Supercritical Fluid Conditions

An efficient technology of impregnation of carbonate crushed stone by oil-product based on SCF-impregnation process usage with propane/butane solvent was developed. Regular impregnation throughout the volume of crushed stone sample is achieved. As a result of the appliance of proposed technology, the humidity of the treated crushed stone samples decreased down to 0.54%.

Preparation of (Ti, Sn)O_2 Nano-Composite Photocatalyst by Supercritical Fluid Dry Combination Technology

A series of TiO2-SnO2 nano-sized composite photo-catalysts containing Sn (9.3%-30.1%) were prepared from TiCI4 and SnCl4·5H2O by using sol-gel, supercritical fluid dry and solid-phase reaction (SCFD) combination technology. Characterizations with X-ray diffraction (XRD), transmission electron microscopy (TEM) and Fourier Transform Infrared Spectroscopy (FTIR) showed that, in addition to anatase type TiO2, a new active phase (Ti, Sn)O2 (with particle size of 2.0-4.3 nm) formed, and there were no SnO2 crystals observed in the range of the doping concentration studied. Photo-catalytic reaction of phenol was used as a model reaction to evaluate the catalytic activities of the obtained catalysts. Compared with pure TiO2 or Ti-Sn catalyst prepared with general sol-gel method, Ti-Sn nano-composite photo-catalyst thus obtained showed significant improvement in catalytic activity. The photo-catalytic degradation rate of phenol could reach as high as 93.5% after 7 h. The preparation conditions of the new phase (Ti, Sn)O2 were investigated and its catalytic mechanism was proposed. The photo-catalytic particles prepared using SCFD combination technology exhibited small particle size, large surface area and high activity.