Supercritical Fluid Extraction of Essential Oil from Dry Rhizome of Ligusticum chuanxiong Hort and Their Characterization by GC/MS

Supercritical fluid extraction (SFE) of essential oil from dry rhizome ofLigusticum chuanxiong Hort was developed. GC/MS was used for the determination of the composition ofessential oil. Forty-four compounds were identified. The conventional extraction method wasconducted in parallel for comparison. The extracts were qualitatively compared by GC/MS. The yieldsof SFE and steam distillation-extraction were 4.16 % ( v/w) and 0.8 % ( v/w), respectively.Application of SFE of zessential oil from dry rhizome of Ligustiaan chuanxiong Hort was preferable.

Advances in Supercritical Fluid Crystallization

The supercritical fluid crystallization technique is a novel technology for preparing ultrafine particles. This paper introduced the concept and features of the technique with an emphasis on three kinds of supercritical fluid crystallization techniques, i.e. rapid expansion of supercritical solutions, supercritical fluid anti-solvent and particles from gas saturated solutions Some questions and the prospect of this technique were also discussed.

Fast analysis of derivatives of polycyclic aromatic hydrocarbons in soil by ultra-high performance supercritical fluid chromatography after supercritical fluid extraction enrichment

An efficient and environment-friendly method for simultaneous determination of 13 typical derivatives of polycyclic aromatic hydrocarbon(PAH)in petroleum-polluted soil with nitro-,oxy-and alkylfunctional group was developed using supercritical fluid extraction(SFE)followed by ultra-high performance supercritical fluid chromatography(UHPSFC).Parameters of UHPSFC,including type of stationary phase and mobile phase modifiers,gradient elution process,backpressure,column temperature,and the flow rate of mobile phase,were systematically optimized,achieving a fast separation within4.2 min.Limits of detection(LOD)were 0.005-0.1μg mL^(-1)or 0.1-2.0 ng g^(-1),respectively,with a good repeatability(RSD<5.0%).Before UHPSFC-PDA analysis,the PAH-derivatives in soil samples were effectively enriched in 15.0 min using SFE with an online carbon nanotubes(CNTs)collection trap.The soil samples were analyzed by the proposed method and the results were verified by GC-MS.Thus,SFE equipped with an online CNTs trap followed by UHPSFC-PDA analysis,which only consumed about2.0 mL organic solvent for a whole run,has been demonstrated to be an efficient way for screening and quantitative analysis of trace-level PAH-derivatives in soil samples.

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

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Overview of the Analytical Lifecycle of Supercritical Fluid Chromatography Methods

In recent times, the overall interest over Supercritical Fluid Chromatography (SFC) is truly growing within various domains but especially for pharmaceutical analysis. However, in the best of our knowledge modern SFC is not yet applied for drug quality control in the daily routine framework. Among the numerous reported SFC methods, none of them could be found to fully satisfy to all steps of the analytical method lifecycle. Thereby, the present contribution aims to provide an overview of the current and past achievements related to SFC techniques, with a targeted attention to this lifecycle and its successive steps. The included discussions were therefore structured accordingly and emphasizing the analytical method lifecycle in accord with the International Conference on Harmonisation (ICH). Recent and important scientific outputs in the field of analytical SFC, as well as instrumental evolution, qualification strategies, method development methodologies and discussions on the topic of method validation are reviewed.

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.

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,

Carotenoids Particle Formation by Supercritical Fluid Technologies

Based on the solubility in supercritical CO2,two strategies in which CO2 plays different roles are used to make quercetine and astaxanthin particles by supercritical fluid technologies.The experimental results showed that micronized quercetine particles with mean particle size of 1.0-1.5 μm can be made via solution enhanced dispersion by supercritical fluids(SEDS) process,in which CO2 worked as turbulent anti-solvent;while for astaxanthin,micronized particles with mean particle size of 0.3-0.8 μm were also made successfully by rapid expansion supercritical solution(RESS) process.

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.

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 a Novel Template from Mesoporous Zirconia and the Effect on Porous Structure

Mesoporous zirconia was synthesized by a new and simple method. Zirconium n-propoxide was used as the zirconium source. A small, inexpensive nonsurfactant, triethanolamine, was used as the template. The template was removed by thermal treatment in air and supercritical fluid extraction using CO2. The structure of the resulting materials was characterized by X-ray diffraction, transmission electron microscopy, and N2 adsorption-desorption analyses. The materials are found to have narrowly distributed average pore diameters and wormhole-like pore channels. However, higher surface area and larger pore volume are exhibited after supercritical fluid extraction with CO2. The removal of the template by thermal treatment also leads to condensation and mild shrinkage of the zirconia framework.

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.

Dynamic Supercritical Fluid Devolatilization of Polymers

A number of studies have been reported on the applications of supercritical fluids to polymeric processes. The presence of volatiles can affect the end-use properties of polymer materials. Therefore, these volatiles must be reduced to a level below the maximum permissible limit. Conventional heat-relevant techniques for polymer devolatilization sometimes have limited effectiveness. Devolatilization with supercritical fluids, however, can enhance removal of volatiles from polymers. A model for diffusion-limited extraction is used to characterize dynamic supercritical fluid devolatilization of spherical polymer particles. The rate of supercritical fluid devolailization for styrene/polystyrene system is measured at 343 K and 18 MPa and at CO2 flow rate of 1.93, 3.27 and 5.62 L·min^-1, respectively. The model analysis, which is consistent with experimental results, indicates that the supercritical fluid devolatilization is not solubility-limited but diffusion-limited when CO2 flow rate is above 4.00 L·min^-1.

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.

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.

Chiral Separation of Ibuprofen by Supercritical Fluid Chromatography

The separation method using chiral stationary phase （CSP） for the preparation of enantioselective compound was widely used. In this work, supercritical fluid chromatography（SFC） was proposed to resolve the chiral mixtures. To determine the optimum operating conditions for the chiral separation of the racemic ibuprofen, the retention factors and resolutions with the change in pressure, temperature and the content of IPA （%, by volume） in supercritical CO2 were investigated. Experiments showed that the retention factor decreased with the increase of pressure and decrease in temperature. The retention factor was also influenced by the content of IPA in mobile phase, as the content of IPA in the supercritical fluid increased, the retention factor decreased. The resolution of the enantiomers became worse with the increase of IPA in the supercritical fluid. Through optimizing the experimental conditions, a SFC procedure with 13MPa, 311.15K and 4% IPA in CO2 was obtained. The peak shape of the enantiomers was symmetric with supercritical fluid chromatography when compared to the asymmetric peak shape obtained by the conventional liquid chromatography. This work demonstrated that the developed supercritical fluid chromatography procedure was suitable for the chiral separation of ibuprofen enantiomers.

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.

Simultaneous Removal of Surfactant Template from MCM-41 and Implantation of Transition Metal Complexes into Mesopores with Supercritical Fluid

The simultaneous removal of up to 92% of the surfactant template and chemical implantation of transition metal complexes into mesopores has been successfully achieved by treating as-synthesized pure siliceous MCM-41 with supercritical CO2 modified with CH2Cl2/MeOH mixture, resulting in the formation of functionalized material with uniform pore structure.

Effect of co-existent components in CO2 supercritical fluid extract of Angelica Sinensis Radix on metabolism of Z-ligustilide after oral administration in rats

Objective:To establish a basis for Angelica Sinensis Radix(ASR)as a dietary supplement for colorectal cancer chemoprevention,the effect of co-existent components in supercritical fluid extract(SFE)of ASR on the pharmacokinetics of Z-ligustilide after oral administration was investigated in vitro and in vivo.Methods:Incubation in gastrointestinal contents and incubation in rat liver tissue homogenates post-mitochondrial supernatant(PMS)experiments were used to study changes in the levels of Z-ligustilide in vitro.Results:Within 4 hours,the level of Z-ligustilide in SFE declined at a slower rate than in its pure form.Clearance of Z-ligustilide after administration in its pure form was significantly slower than that of SFE of ASR(CL,0.96±0.16 mL·min/kg versus 1.24±0.21 mL·min/kg P<0.05;AUC,243.37±16.84 versus 176.69±12.59 mg·min/L).Conclusion:These phenomena may be attributed to the interactions between the co-existent components in SFE of ASR and Z-ligustilide enhancing the stability of Z-ligustilide.These results suggest that the bioavailability of Z-ligustilide in SFE of ASR is improved.However,stabilization of plasma concentration was not sustained,so that the efficacy of active components could not be maintained.Thus,further processing of SFE of ASR is required.

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.