523results about "Quinone separation/purification" patented technology

This invention relates to a method for producing Hypericum perforatum hyperoside and hypericin. This invention comprehensively utilizes Hypericum perforatum fruits which are rich in our country to produce both hyperoside and hypericin pharmaceutical active components with high recovery rate, high product purity, and low cost. During the producing process, it achieves the recovery and cycling use of many solvents like ethanol and ethyl ether, and also achieves the regeneration and cycling use of micelle reextracting agent and absorption resin. The plant biological active compounds produced by this invention can be broadly used in heat-clearing and detoxifying, astringing to arrest bleeding and promote diuresis, and antidepressant drug.

A method for separating and purifying coenzyme Q10 from a microorganism comprises the following steps of: (1) crushing, (2) extracting, (3) chromatography and (4) crystallization. With the adoption of the method for preparing the coenzyme Q10, the extraction rate and yield of the coenzyme Q10 can be guaranteed, and the quality conformance of a coenzyme Q10 product can be further ensured. The method is simple in technology, low in production cost and small in environmental pollution and is appropriate for industrial production.

The invention relates to a method for preparing a separation coenzyme Q10, and in particular relates to a method for preparing a high-purity coenzyme Q10 in a large scale. The method comprises the following steps of: carrying out supercritical extraction on dry thallus containing the coenzyme Q10 to obtain extract liquor; and carrying out alkali treatment on the extract liquor to obtain a column loading liquid, carrying out column chromatography on the column loading liquid to obtain an eluent, concentrating the eluent, and crystallizing with ethanol to obtain the high-purity coenzyme Q10 with the purity higher than 99.5%. When the method provided by the invention is used for producing the coenzyme Q10, the overall yield is higher than 90%, and cost is low, thus the method provided by theinvention is applicable to industrial production.

The invention relates to a method for purifying coenzyme Q10. The method comprises the following steps: an upper column solution containing the coenzyme Q10 is subjected to chromatography through a silica gel column; and a mixed solvent of n-hexane and low-grade alcohol or a mixed solvent of n-hexane and low-grade ketone is subjected to elution to obtain eluent; and the eluent is decompressed, is condensed to be dried and is added with ethanol to obtain the coenzyme Q10. Through an elution mode, the method greatly reduces the difficult degree of the reclaiming operation of a subsequent solvent; and simultaneously, the content of effective ingredients of the coenzyme Q10 is improved.

The juglone extracting process includes the following steps: 1. crushing the root, stem, leaf, bark or pericarp of Juglans mandshurica as the material to below 20 mesh; 2. soaking the material in solvent of 1 to 1000 times weight through stirring for 0-12 hr; 3. distilling the soaked material under reduced pressure while replenishing solvent to obtain colorless distillate; 4. separating out the product physically from the distillate and drying to obtain juglone-containing product. The present invention has simple process, short production period, low cost, high product purity and yield, and other advantages.

The extraction method of rhubarb total anthraquinous includes the following steps: (1). mixing rhubarb pieces and concentrated ethyl alcohol according to weight ratio of 1:4-8, extracting for 3 timesby using reflux process; (2). filtering extraction liquor, recovering ethyl alcohol and making the filtrate into extract; (3) adding the extract to macropore adsorption resin column, using dilute ethyl alcohol to flush, then removing flushing liquor and continuously using concentrated ethyl alcohol to flush; (4). taking out eluant and recovering ethyl alcohol, and regualting pH value of eluant toacidity,; (5). filtering eluant and drying solid matter obtained by preciptation to obtain the invented product. Said product can be used preparing medicine for curing renal failure, in which the rhubarb total anthraquinone content must be above 50%.

The present invention belongs to the field of effective Chinese medicine component extracting technology, and is especially supercritical CO2 extraction process of total rhubarb anthraquinone. Rhubarb powder through or through no acid solution treatment is soaked in alcohol or other solvent and extracted in a extracting reactor with supercritical CO2 as extractant and alcohol as entrainer and solvent at pressure of 20-60 Mpa and temperature of 30-60 deg.c for 0.5-3 hr. The extracted matter is decompression separated in a separating tank at 15-45 deg.c, and alcohol solution of total rhubarb anthraquinone is collected and decompression concentrated and dried to obtain total rhubarb anthraquinone.

The invention provides bacillus subtilis natto ST188 with CGMCC No. 8400 and a high-yield method for purifying vitamin menadione-7 by using the bacterial strain. The high-yield method comprises the following steps: (1) carrying out spray drying on natto fermentation liquor, and extracting or leaching bacillus natto fermentation liquor spray drying powder by using a solvent so as to obtain a leaching solution; (2) concentrating the leaching solution obtained in the step (1) so as to obtain extract; (3) carrying out column chromatography on the extract obtained in the step (2), carrying out gradient or isocratic elution, and concentrating collected liquid, thus obtaining a menadione-7 crude product; and (4) crystallizing and purifying the menadione-7 crude product obtained in the step (3), thus obtaining the pure vitamin menadione-7 product.

The invention discloses a method for extracting juglone from walnut green husk residue by microwave reflux, which ueses chloroform solvent for extraction by a microwave reflux extraction method, preferably adopting walnut epicarpe (green husk) residue with higher juglone content and can be obtained easily as raw materials for extraction. The method is carried out under the optimal extraction condition that the solid-to-liquid ratio of walnut green husk with average grain size of 50 mesh to the chloroform solvent is between 1:5 and 1:8, and comprises the steps of: subjecting walnut green husk residue to extraction and pumping filtration at soft fire in microwave power level and washing the filter residue with solvent to obtain juglone extraction liquid, collecting all solutions, and preparing the juglone by decompression, rotary evaporation and concentration. After all index measurements, the extraction ratio of the juglone is 92%, the purity of product is 81.5%, and the product yield is 0.20%. The method is rapid and convenient, and has high extraction ratio, and devices in the method are easy to operate, have low energy consumption, consume less solvents which are easy to be recovered, and are suitable for the expanded production in factories. Meanwhile, the problem that juglone is heated and decomposed in a traditional method can be effectively avoided, which guarantees the effectiveness of extractives. The method satisfies the environmental protection and industrialization demands. The extracted juglone can be widely applied, and active ingredients in the juglone have the effects of antibacterial, anticancer and sedation of central nervous system, and have wide application prospects in such fields as medicine, pesticide, dye, pH indicator and the like.

The invention discloses a method for extracting and purifying tanshinone monomeric compounds from red sage root, which comprises the steps of: (1) preparing an extract: smashing the red sage roots, immersing in dichloromethane, extracting by percolation, ultrasound or refluxing, and recovering solvent from an extracting solution to obtain the extract of the red sage root; and (2) purifying with high-speed countercurrent chromatography: purifying the obtained extract by the high-speed countercurrent chromatography with petroleum ether-n-butyl alcohol-methanol-water as a two-phase solvent system, so as to obtain seven monomeric compounds with purity over 95%, including dihydrotanshinone I, 1,2,15,16-tetrahydrotanshinquinone, cryptotanshinon, tanshinone I, neo-przewaquinone A, tanshinone II A and miltirone.

The present invention provides a convergent method for the synthesis of ubiquinones and ubiquinone analogues. Also provided are precursors of ubiquinones and their analogues that are useful in the methods of the invention. The invention further provides an improved method for the carboalumination of alkyne substrates.

The invention discloses a method for extracting and separating a compound of total anthraquinone in rheum. The method takes an amides ionic liquid displayed in formula (1) as an extractant and extracts the compound of total anthraquinone in rheum from a rheum extract. In formula (1), R1, and R2 are respectively the amide of C1-C10 or alkyl of C1 to C10. L- is one of the followings: BF4-, PF6-, OAC-, CF3SO3-, and N (SO2CF3)2-. The invention takes the amides ionic liquid as the extractant to extract and separate the compound of total anthraquinone in rheum from the rheum extract, which improves the extracting effect. The ionic liquid can be repeatedly used, which is safe, stable and environment friendly. The invention is the most economical and practical environmental protection technology.

The invention relates to an extraction method of alkannin. In the extraction method, after extracting lithospermum with organic menstruum, aqueous alkali is used for processing. The method is characterized in that after the lithospermum is fully extracted with nonpolar organic menstruum in a backflow mode, aqueous alkali containing sodium hydroxide or potassium hydroxide with the concentration of 0.6-5.5M is used for fully leaching an organic solution after the fully extracting, then the pH value of aqueous alkali extraction solution is acidized to be smaller than or equal to 2, then the lithospermum is fully precipitated and collected. By using the extraction method in the invention, the lithospermum with high purity and yield can be obtained and can be applied to the commercial process.

The invention discloses a method for preparing questin by utilizing an ocean aspergillus flavipes HN4-13 bacterial strain. The method comprises the following steps: conducting separation and purification on antibacterial active substances generated through fermentation of the aspergillus flavipes HN4-13 bacterial strain according to silica-gel column chromatography, Sephadex LH-20 column chromatography, preparation of high performance liquid chromatography (PHPLC) and the like by taking vibrio harveyi as an indicator bacterium, so as to obtain a vibrio harveyi-preventing active compound HY2; indentifying the structure of the active compound HY2 according to spectra data such as ESI-MS, 1H-NMR and 13C-NMR, so as to determine that the active compound HY2 is questin. The questin is obtained through separation of a metabolic product of aspergillus flavipes HN4-13; experiments show that the questin can perform a certain inhibiting function of the pathogenic bacteria, such as vibrio harveyi, vibrio anguillarum, vibrio parahaemolyticus and vibrio cholerae, of aquatic products, and can be used for preparation of medicine preventing pathogenic vibrio of the aquatic products.

The invention relates to a combined extraction and purification technique for multiple active ingredients of a medicinal plant, in particular to a combined extraction and purification technique for multiple active ingredients of polygonum multiflorum. According to the method, stilbene glucoside, rheum emodin and chrysophanol in the polygonum multiflorum can be maximum extracted from the polygonum multiflorum into a solvent by using 70-80 percent of ethanol as an extraction solvent and are separated from starch in residual slag; water-soluble differences of the stilbene glucoside, the rheum emodin and the chrysophanol are used and water is used as a solvent so that the stilbene glucoside in alcohol extracts can be separated from the rheum emodin and the chrysophanol, and a crude product is obtained; the rheum emodin and the chrysophanol can be respectively separated from the alcohol extracts by successively using 5 percent of sodium carbonate and 5 percent of sodium hydroxide as solvents, and the rheum emodin and chrysophanol crude product can be obtained through an acid precipitation; and the polygonum multiflorum ethanol extract residual slag is washed by using water, and the starch with a purity of 85-87 percent can be obtained through precipitating water washing liquid. The invention has the characteristics of low cost, high efficiency, no pollution and high product purity.

The invention relates to a method for extracting shikonin from lithospermum, which comprises the following steps of: crushing lithospermum raw materials and adding alkaline aqueous solution with the pH value being 9 to 10 for percolating and extracting; regulating the pH of the extracting solution to 7, 5 and 3, adding a macroporous resin column to adsorb for three times, eluting by using 70 to 80-percent ethanol, concentrating the eluent and crystallizing in ethanol; dissolving in sodium bicarbonate solution with the pH value being 10 to 11, regulating the pH value to 1 to 3 and precipitating, and refluxing and dissolving the precipitates in acetone and ethyl acetate in turn and recrystallizing. The method for producing the shikonin can reduce the use amount of toxic reagent and reduce production cost. The process is simple in operation and easy in industrialization.

The invention relates to a method for producing alkannin by utilizing Arnebia euchroma(Royle)Johnst hairy root. The method includes selection and processing of Arnebia euchroma(Royle)Johnst explant, activation culture of agrobacterium rhizogene, infection of cotyledon explant and induction of hairy root, obtaining of sterile Arnebia euchroma(Royle)Johnst hairy root system and liquid culture of Arnebia euchroma(Royle)Johnst hairy root as well as alkannin production. The used hairy root has the characteristic of rapid and autonomous growth on culture medium without exogenous hormones, thus the method not only can overcome the defects that cell culture grows slowly and hormone is required to be additionally added to maintain the growth thereof when utilizing cell culture to produce alkannin, and the method has the advantages of stable alkannin throughput, simple operation in cultivation, lower cost and no restriction of climate and land natural conditions. Especially the invention provides a stable and continuable novel medicine source for producing alkannin by utilizing hairy root culture method and provides reliable source and material basis for alkannin mass production by applying bioreactor in the future.

The invention discloses a method for supercritical fluid extraction of juglone in walnut seed green skin waste residue. In the invention, supercritical CO2 fluid in the supercritical fluid extraction method is adopted for extracting, walnut seed external skin (green skin) waste residue which is high in juglone content and easily available is preferably selected as the raw material for extraction. The best conditions are as follows: flow rate of the supercritical CO2 fluid is 1-3L/min, the extraction pressure is 10-18MPa, the extraction temperature is below 65 DEG C and the extraction time is within 20min. In the invention, one-time extraction yield of the juglone reaches 87%, the product purity is 92%, the productive rate is 0.21%. The method of the invention features not only high extraction yield but also innocuity, no taste, incombustibility, no erosion, low price and easy recovering of the extraction liquid, thus meeting the requirements of environmental protection and industrialization. The extracted juglone is wide in application, the active ingredients play a role in resisting bacterium and cancer and calming nervus centralis, thus enjoying very wide application prospect in medicine, agricultural chemical, dye and pH indicator and other fields.

The present invention relates to the preparation process of extract containing three active components including hypericin, Hyperforin and flavones in the total content not less than 50% from hypericum perforatum or other congeneric plant. The three active components are separated from the polar solvent extracted liquid via biphase extraction with non-polar solvent selected based on their difference in polarity. They are then purified separately based on their difference in acid-base property to obtain the extract A with high hypericin and flavones content and extract B with high Hyperforin content. The two extracts are merged through dissolution to obtain hypericum perforatum extract with total active component content not less than 50%. The extract has the obvious activity of resisting depression and may be used as the material of depression treating medicine or functional food.

The present invention belongs to the technical field of medicine, and relates to a high-speed countercurrent chromatography continuous circulation method for separating and preparing naphthoquinone compounds from Arnebia euchroma (Royle) Johnst. According to the method, the natural naphthoquinone compounds represented by a formula (I) are separated and prepared by using a high-speed countercurrent chromatography continuous circulation separation method, n-hexane, ethyl acetate, acetonitrile and water are used as a two-phase solvent system for high-speed countercurrent chromatography separation, an online storage technology and a circulation elution mode are combined, the fractions containing the target compound are subjected to continuous circulation elution, and the fractions are collected to obtain shikonin with a purity of more than 95%, propionylshikonin with a purity of more than 95%, deoxyshikonin with a purity of more than 95%, (beta,beta-dimethylacryl)shikonin with a purity of more than 95% and isovalerylshikonin with a purity of more than 95%. With the method of the present invention, the high purity naphthoquinone compounds can be obtained through the one separation purification, such that the method has advantages of simple operation, rapidness and high efficiency, and is suitable for the separation and preparation of naphthoquinone and a variety of natural compounds. The formula (I) is defined in the specification.

The invention provides a deep eutectic solvent which is composed of lactic acid, D-(+)-glucose and water, wherein the mole ratio of the lactic acid to the D-(+)-glucose in the deep eutectic solvent is (1-2):(1-5), and the water content is 0-80% (V/V). The invention also provides application of the deep eutectic solvent and a method for extracting anthraquinone from radix et rhizoma rhei by using the deep eutectic solvent. When being used for extracting anthraquinone from radix et rhizoma rhei, the deep eutectic solvent replaces chloroform and other toxic organic solvents in the traditional extraction, reduces the environmental pollution of the radix et rhizoma rhei industry, and thus, is green and environmentally friendly. The deep eutectic solvent has high extraction efficiency and is recyclable and reusable, thereby greatly lowering the extraction cost, and providing a new technical means for reasonable development and utilization of radix et rhizoma rhei resources.

The invention relates to an extraction method of chemical components in walnut green tangerine peel, particularly an extraction method of juglone and derivative in the walnut green tangerine peel. The extraction method comprises the following steps: pealing fresh walnut green tangerine peel, and sieving by a screen mesh of 40-80 meshes after washing, drying and crushing; putting the sieved walnut green tangerine peel powder into a container, and adding pure water according to a solid-liquid quality ratio of 1: (8-12); adding pectase and cellulase in the container, sealing the container after regulating the ph values of the solution in the container to 5.5-6.7, and then oscillating the resultant at the constant temperature of 20-40 DEG C for 36-60h; reducing pressure of and condensing the solution after enzymatic hydrolysis to obtain a concentrate; and extracting the resultant by petroleum ether after freezing and drying the concentrate to obtain juglone and derivative. In the invention, walnut green tangerine peel cell wall is destroyed by enzymatic hydrolysis, and recovery rate is raised by microwave ultrasonic wave processing; the technology of obtaining juglone and derivative by petroleum ether extraction is simple with high recovery rate, and the problems of low pericarp salvaging and low quinone substance recovery rate in walnut plucking and processing are solved.

The invention relates to a continuous separation device for p-benzoquinone crystals. The continuous separation device comprises a crystallizing kettle, a cyclone separator, a horizontal centrifuge and a PLC (Programmable Logic Controller) control circuit. The continuous separation device has the advantages of energy conservation, environment friendliness and high production efficiency; a mixed liquid containing the p-benzoquinone crystals is subjected to warming, stirring and shock cooling by virtue of the crystallizing kettle so as to generate products, the products are conveyed to the cyclone separator through a discharging pipe of the crystallizing kettle, the mixed liquid containing the high-concentration crystals is conveyed to the horizontal centrifuge from the bottom of the cyclone separator and is subjected to solid-liquid separation, a p-benzoquinone mother solution is conveyed to a water film generator at the upper part of a p-benzoquinone stripping tower from the top of the cyclone separator or returns into the crystallizing kettle, and a mother solution separated by the horizontal centrifuge returns into the crystallizing kettle as well; the processes are continuously and circularly carried out, so that the continuous separation of the p-benzoquinone crystals and the cycle use of the mother solution can be finished, and the outward draining is avoided. According to the continuous separation device, the problems that an existing device cannot continuously work and is low in efficiency are well solved, and the continuous separation device has excellent economic and social benefits.

The invention discloses a method for separating and purifying 2-ethyl anthraquinone from sulphuric acid. The method comprises the following steps of: slowly adding a 2-ethyl anthraquinone concentrated sulphuric acid solution obtained by a closed-loop reaction to well-measured water to carry out acid separation; carrying out countercurrent extraction to the feed liquid subjected to acid separationand an extraction solvent at a temperature of 75-80 DEG C, separating a small amount of dilute sulphuric acid contained in the extract liquor from the 2-ethyl anthraquinone obtained through extraction; then, respectively carrying out caustic washing and rinsing to separate a small amount of water contained in the feed liquid; and finally, respectively carrying out room-pressure distillation and reduced-pressure distillation in a distillation kettle to obtain product of 2-ethyl anthraquinone. The invention utilizes an extraction principle and a reduced-pressure distillation principle for the post-treatment of the 2-ethyl anthraquinone concentrated sulphuric acid solution so as to lighten the labor intensity, improve the operating environment, enhance the operation safety, decrease the production cost and shorten the production flow of the post-treatment, and the product obtained through separation has high purity and stable quality.