104results about How to "Large amount of separation" patented technology

The invention discloses a preparation method of amoxicillin sodium and sulbactam sodium for injection and a freeze-dried powder injection thereof as well as a separating and purifying method of the amoxicillin sodium and sulbactam sodium for injection. By adopting high speed countercurrent chromatography, the invention prepares trichloromethane, ethyl acetate, methanol and water to form a solvent system with an immobile phase and a mobile phase and separates and purifies amoxicillin sodium and sulbactam sodium to obtain the amoxicillin sodium and sulbactam sodium for injection; the purity of the obtained product can reach more than 98% and the prepared injection has improved stability.

The invention relates to a method for preparing lactuca indica and lactucin, which is a method for using two separation processes to obtain lactuca indica and lactucin from cichorium glandulosum by a high-speed countercurrent chromatography. The method has the advantages of large fractional dose, small sample loss, high recovery rate, mild separation environment and solvent saving. A great amountof lactuca indica and lactucin crude products can be placed in a countercurrent chromatograph, the separation result achieves the high purity and good separation effect. The method is not only suitable for preparing the product with high purity from plant crude extract, but also suitable for purifying lactuca indica and lactucin crude extracts obtained by various approaches.

The invention belongs to the field of natural organic chemistry, and relates to a method for purifying aloe polysaccharides, particularly a preparation method for enriching and purifying aloe polysaccharides in aloe by a high-speed countercurrent chromatography separation process. The method is characterized by purifying natural plant aloe leaching liquor twice by a high-speed countercurrent chromatography separation process to obtain aloe polysaccharides of which the purity is higher than 95%. The method is suitable for preparing high-purity aloe polysaccharides from natural plants containing aloe polysaccharides and extracts of the natural plants. The method is suitable for preparing aloe polysaccharides by separating with various types of countercurrent chromatographs, and the aloe polysaccharides prepared by the high-speed countercurrent chromatography process can be continuously, efficiently and quickly separated by liquid-liquid partition chromatography; and thus, the method has the characteristics of great separation amount, no sample loss, high recovery rate, mild separation environment, solvent saving and the like.

The invention relates to a method for preparing high-purity costuslactone and dehydrocostus lactone through high-speed countercurrent chromatography, which comprises the following steps of: (1) preparing a proper solvent system, standing and demixing to obtain an upper phase and a lower phase; (2) selecting the upper phase as a fixed phase and the lower phase as a mobile phase, filling the fixed phase in a column of a countercurrent chromatograph, regulating the rotating speed of a main machine to be 600-1,000rpm, pumping the mobile phase into the column at a flow rate of 0.5-5.0ml / min, and sampling through a sampling valve after the whole system is dynamically balanced; and (3) receiving a target component according to an ultraviolet spectrum of a detector, concentrating, and crystallizing. The method is suitable for preparing the costuslactone and dehydrocostus lactone in various contents through various high-speed countercurrent chromatographs, and has the characteristics of large separation amount, high recovery rate, and simplicity and convenience of operation.

A process for preparing high-purity rhodioloside from natural rhodiola rosea by high-speed counter-current chromatography includes extracting by high-speed counter-current chromatography and purifying twice to obtain high-purity product. Its advantages are high purity (98%), and high output rate, and saving solvent.

The invention relates to a method for preparing high-purity soybean saponin A and soybean saponin B by high-speed countercurrent chromatography, which comprises the following steps of: (1) selecting a solvent system which is provided with a fixed phase as an upper phase and a mobile phase as a lower phase and has four components with the volume ratio of 1-5 to 0.5-1 to 1-5 to 5-10; (2) using the fixed phase to fill a countercurrent chromatographic column, regulating the rotation speed of a host to be 600 rpm to 1000rpm and pumping the mobile phase into the column at the flow rate of 0.5 ml / min to 4ml / min; (3) after the whole system is in dynamic equilibrium, introducing samples through an introduction valve; and (4) receiving a target composition according to a UV atlas of a detector, compressing, freezing and crystallizing the fraction to obtain monomers of the soybean saponin A and the soybean saponin B. The soybean saponin A and the soybean saponin B prepared by the method can reach quite high purity and the preparation method has simple operation, high separation efficiency, great separation volume, high recovery rate and good repeatability.

The invention discloses a high-speed counter-current chromatography separation preparation method for high-purity agarotetrol and 4'-methoxy agarotetrol monomers. The method comprises the following steps of: preparing a crude agilawood extract serving as a sample introduction substance; preparing a two-phase solvent system of a stationary phase and a mobile phase; filling the stationary phase in a counter-current chromatograph separation column; rotating a main machine, and pumping the mobile phase into the column; introducing a sample by using a sample introduction valve; and receiving target components according to ultraviolet detection absorption peaks. The solvent system consists of four components (A, B, C and D), wherein the component A is normal paraffin, cycloparaffin or halogenated hydrocarbon; the component B is halogenated hydrocarbon; the component C is fatty alcohol or fatty ketone; and the component D is water. The upper phase is the stationary phase, and the lower phaseis the mobile phase. By the method, high-purity agarotetrol and 4'-methoxy agarotetrol can be obtained, and the purity can reach over 97 percent; and the method can ensure high-peak resolution, has high separation amount, mild separation environment and high reclamation rate of target compounds, and is simple and convenient to operate and easy to popularize and use.

The invention relates to a preparation method for obtaining isobenzofuran ketone compound from a crude extract of a fennelflower by adopting a method of high-speed countercurrent chromatography. A solvent used by the preparation method of the invention is petroleum ether or n-hexane or n-heptane or a four-component solvent system composed of n-pentane, acetic ether and methanol or ethanol or methyl cyanide and water and the isobenzofuran ketone compound is separated from the fennelflower by a separation step. The method has lager separation amount, no damage to samples, high recovery rate and moderate separation environment, and saves the solvent. Adoption of a countercurrent chromatograph can ensure that a large amount of crude samples can be brought in directly or compounded to a compound and the separation can realize higher purity and obtain good separation effect. The preparation method of the invention is not only applicable to preparing products with higher purity from the crude extract of plants but also applicable to purifying the crude extract of isobenzofuran ketone substances which are obtained through various means and separating the isobenzofuran ketone substances by the countercurrent chromatographs of different types.

The invention belongs to the field of separation of natural products, in particular to a method for preparing crocin-I by high-speed countercurrent chromatography. The method is to take ethyl acetate, ethanol and water to mix and separate layers, take the upper phase to fill the high-speed countercurrent chromatographic column, turn the host, pump the lower phase into the mobile phase, dissolve the gardenia yellow pigment in the lower phase and inject the sample through the injection valve , detected by an SP-200 ultraviolet detector, collect the target components according to the spectrum, and dry the fraction under reduced pressure to obtain. The process of the invention is simple in operation, short in preparation period and high in yield, can obtain more than 98% of the crocin-I product, and can realize continuous production.

The invention discloses a method for isolating carbazole from anthracene oil and belongs to the field of deep processing technology of coal tar. The method employs countercurrent chromatography technology, and has the following advantages that: (1) the method is directly applicable to separation of carbazole from anthracene oil, crude anthraene, decrystalized anthracene oil and the like, isolated carbazole contains a little amount of aromatic nitrogen-containing compounds, and high-purity carbazole with purity of 98% or more can be obtained after the isolated carbazole is recrystallized with xylene; (2) a to-be isolated sample can be fully contacted with a liquid-state stationary phase, and the method has the advantages of being no loss in sample, efficient, rapid, large in isolating amount, high in recovery rate and the like; (3) the boiling point of a solvent system is medium, so that the toxicity is substantially reduced, also airtight operation can be performed in the chromatogram system, there is no pollution, the sample is recoverable almost completely, and the solvents of stationary phase and mobile phase are recoverable and reusable; and (4) the isolation process of carbazole is simplified substantially, and the separation technology of anthracene oil, crude anthracene and the like is simplified.

The invention relates to a method for separating various isoflavone components from astragalus. It comprises two steps: (1) enriching plant extrant containing astragalus saponins with silica gel column; (2) separating the target component by reversed phase preparative liquid chromatography.The invention is characterized by low cost, high production and good repeatness, and it can provide new processes for preparing isoflavone components.

The method for separating magnolol and honokial from Chinese medicinal material magnolia bark includes the following steps: (1) using organic solvent to repeatedly extract magnolia bark powder, combining extracts, concentrating, drying to obtain magnelia bark crude product; (2) pouring thue solvent white can be used in counter-current chromatographic separation into liquid separator so as to form mutually-insoluble two phase of solvent; (3) dissolving magnolia bark crude product in equivolume two-phase mixed solvent in the step (2); and (4), injecting one phase of two phase of solvent into separation column of counter-current chromatograph as immobile phase, injecting the solution obtained in step (3) into sample-injecting ring of coutner-current chromatograph, starting the counter-current chromatograph, and injecting another phase of two phase of solvent as mobile phase, making continuous separation and collection so as to respectively obtain purified magnolol and honokiol.

The method of separating oridonin from rabdosia is one continuous liquid-liquid distributing adverse current chromatographic method without needing of any solid support and thus caused adsorption, loss, property change and other troubles. The method has high peak form resolution, great separation amount, no sample loss, high recovering rate, mild separating circumstance and low solvent consumption, and may be used in separating great amount of coarse oridonin product to reach purity over 97 %. In addition, the present invention adopts relatively simple and cheap adverse current chromatograph and economic mixture solvent comprising two or more of normal alkane, halohydrocarbon, fatty alcohol, aliphatic ketone, aliphatic ester, ether and water.

The invention relates to a method for separating and purifying flavonoid compounds in polygonum multiflorum leaves through high-speed counter-current chromatography, which comprises the following steps: (1) preparing an ethyl acetate phase of the polygonum multiflorum leaves, (2) adopting a water-methanol-ethyl acetate-normal hexane solution with the volume ratio of 1: 1: 1: 0.5-2: 2: 5: 1 as a solvent system, and pumping a stationary phase and a mobile phase into a high-speed counter-current chromatograph; when the two-phase solvent system is balanced in the high-speed counter-current column, dissolving the polygonum multiflorum leaf ethyl acetate phase in the two-phase solvent system, and carrying out high-speed counter-current chromatographic separation; during high-speed countercurrent chromatography separation, an ultraviolet detector detecting a wave peak, performing collection from peak appearance until the peak disappears, collecting different fractions respectively, and performing vacuum concentration and freeze drying to obtain myricetin, quercitrin and kaempferol-3-O-rhamnoside. The separated and purified flavonoid compound monomer is high in purity, small in loss, easy to operate, large in preparation amount, economical and environmentally friendly.

The invention relates to a method for separating a base oil family composition and mainly aims at solving the technical problems of complex separation method and a large using amount of a solvent in the prior art. The method provided by the invention comprises the following steps: a) diluting base oil with the solvent which is inert to the base oil; b) separating the base oil family composition by using a liquid preparative chromatograph; c) detecting an obtained product by using an ultraviolet detector, and collecting products according to analysis results of the ultraviolet detector; and d) obtaining total quantity of saturated hydrocarbons, total quantity of aromatic hydrocarbons and total mass of rubber after the treatment of the products. By adopting the technical scheme, the problems are solved in a relatively good manner, and the method can be used in industrial production for separating the base oil family composition.

The invention discloses a method for preparing shionone by utilizing a high-speed countercurrent chromatography. The method provided by the invention comprises the following steps of: a, crushing Tatarian aster root as a medicinal material and reflowing and extracting by utilizing methanol with the concentration of 80-90%; adding active carbon into an extracted solution to de-color and filtering when the solution is hot; concentrating the solution until the concentration of the alcohol is 50-70%; standing and crystallizing to obtain a rough crystal; b, separating the crystal by utilizing the high-speed countercurrent chromatography; collecting target components according to an ELSD (Evaporative Light Scattering Detector) detector map; and decompressing, concentrating, crystallizing and then drying to obtain a product. The method provided by the invention has the advantages of simplicity for technological operation, short preparation period and high yield; and the method can be used for obtaining the shionone product with the content of more than 98% and is suitable for the industrial production.

A process for preparing liensinine, iso liensinine and methyl liensinine from the core of lotus seed by counterflow chromatography method features that its separating solvent is the mixture of two or more in n-alkanes, halohydrocarbon, emtrol, lipone, fatty ester, ether and water.

The invention discloses a method for preparing high-purity sucrose fructan monomers by high-speed counter-current chromatography, which comprises the following steps: protecting hydroxyl of fructooligosaccharide to obtain fructooligosaccharide derivatives, carrying out high-speed counter-current chromatography to separate the fructooligosaccharide derivatives to obtain a kestose derivative, a nystose derivative and a glucopyranoside derivative, removing the hydroxyl protecting group to obtain the high-purity kestose, nystose and glucopyranoside. The purities of the kestose, nystose and glucopyranoside are respectively higher than 98%. The method has the advantages of short separation time, high preparation quantity,, high recovery rate, no sample loss, mild separation environment and solvent saving, and can implement scale-up production.

The invention discloses a method for separating inosine from styela plicata. According to the method, a compound inosine is extracted, separated and identified from the styela plicata for the first time, the styela plicata can be sufficiently recycled and utilized and wastes are avoided; high-speed counter-current chromatography is used for carrying out separation so that the method has the advantages of no sample loss, no pollution, high efficiency, rapid speed and great separation amount; specific separation steps are simple and easy to operate; the separated inosine has wide application inthe fields of pharmaceuticals and the like and has very important meanings on researches of effective components of ocean natural products.

The invention relates to a method for separation and preparation of alkaloids from walnut green seedcase, the alkaloids is separated and prepared by multistage extraction and HSCCC (high speed counter-current chromatography) after auxiliary processing of the walnut green seedcase as a raw material by an ultrasonic microwave extraction device, a mixture with the ratio of methanol: water of 4: 1 is used as an extraction agent, the material liquid ratio is 10 to 1, after 15min of auxiliary processing by the ultrasonic microwave extraction device, a chloroform methanol water alkaloid extraction solution can be obtained by multistage extraction; according to the HSCCC method, chloroform and methanol are used, a solid phase carrier is not required, the loss caused by irreversible adsorption and degradation of a sample in the solid phase carrier can be eliminated, recovery rate is high, sampling can be repeated, the separation process can keep stable, reproducibility is good, gradient elution and reversed-phase elution can be realized; repeated sampling can be realized, separation efficiency is high, and the separation amount is large.

The present invention is high speed countercurrent chromatographic process for preparing high purity taxol compound. The process includes the following steps: 1. pre-treatment including heating and dissolving coarse taxol extract and fixed phase; 2. high speed countercurrent chromatographic separation through shaking the solvent system, standing to separate upper phase and lower phase, using the upper phase as the fixed phase, pumping the mobile phase into column, feeding sample through the valve and accepting target component based on the detected ultraviolet spectrum; and 3. post-treatment including collecting taxol component, decompression concentrating to obtain white solid, dissolving and recrystallizing, filtering and drying to obtain white needle crystal. The HPLC detection shows that the product has purity over 99 %, and the process has high yield and low cost.

The invention discloses a method for preparing high purity z-ligustilide and cnidilide A, which is characterized by adopting high-speed countercurrent chromatography and comprises the following steps: preparing the crude extract of rhizoma ligustici wallichii or angelica as a sample injection substance; preparing a solvent system forming stationary phase and mobile phase; filling the stationary phase into a countercurrent chromatography column; then rotating a host machine, pumping the mobile phase into the column, or simultaneously pumping the stationary phase and the mobile phase into the column and then rotating the host machine; and injecting samples from an injection valve, receiving target components according to a map of a detector and obtaining the z-ligustilide and cnidilide A through separation. The solvent system is formed by four components (A, B, C and D). The component A is n-alkane, the component B is fatty ether, the component C is fatty alcohol or fatty ketone and the component D is water. The z-ligustilide and cnidilide A with purity higher than 95% can be obtained by the method. The method is simple and convenient, easy to operate, high in recovery and easy to promote and use.

The invention relates to a method for purifying the papain by using a chelating affinity membrane of a cobalt ion metal, which comprises the following steps: (1) an activated nylon membrane is modified by the bonding of the chitosan; (2) the modified nylon membrane reacts with the mixed solution of epichlorohydrin, sodium hydroxide and sodium borohydride, then the membrane is immerged respectively into the mixed solution of sodium carbonate, sodium borohydride and coupling agent, and cobalt chloride solution to obtain the metal affinity membrane of the chelating cobalt ion; (3) the metal affinity membrane is piled up to a membrane stack, put onto a membrane bridge, transferred into Tris-HCl buffer and eluate by a peristaltic pump, then into the papain solution, is eluted by eluting agents, and then the papain is produced; and (4) the activity of enzyme and the protein content are measured, and the multiple of purification is calculated. The method has the advantages of rapidness, high efficiency, simpleness and big separation capacity. The extracted enzyme is good in activity and applicable to commercial production.

The invention belongs to the field of traditional Chinese medicine pharmacy, and relates to a method for separating and purifying amentoflavone, in particular, a method for enriching and purifying the amentoflavone through a high speed countercurrent chromatography method. The method is characterized in that: two mutually-immiscible solvent systems are utilized to perform the separation and purification in a mode of high-speed planetary motion in a support pipe; the method is applicable for the countercurrent chromatographies with various types to separate the amentoflavone, and has advantages of no irreversible adsorption, no loss of sample, no pollution, high efficiency and speed, high recovery rate, mild separating environment, high product purity and large quantity separation, and is applicable for industrial production.

The invention belongs to the technical field of separation and purification of radix scrophulariae iridoid compounds and discloses a separation and purification method of three iridoid components in radix scrophulariae. The separation and purification method comprises the following steps: weighing 10kg of the radix scrophularia; adding purified water which is 15 times of the radix scrophularia; adjusting the pH (Potential of Hydrogen) value to 3.5; carrying out crude separation; refluxing and extracting for 2h at the temperature of 60 DEG C; filtering and collecting filtrate; extracting filtrate from filtering dreg according to the above method; combining the filtrate of the two times; evaporating on a rotary evaporator to obtain extract, wherein the yield of the extract is about 31.5 percent; purifying by high-speed counter-current chromatography. The separation and purification method disclosed by the invention has the characteristics of great separation amount, no sample loss, highrecovery rate, mild separation environment, solvent saving and the like and is widely applied to preparation, separation and purification of chemical substances in the fields including biology, medicines, environment protection and the like.

The invention discloses a method for preparing high-purity quercetagetin and belongs to the technical field of flavonoids compound extraction. The method comprises the following steps of: extracting fermented residue subjected to marigold flower lutein ester extraction by using 5 to 90 percent aqueous solution of ethanol to obtain a crude extract of quercetagetin, concentrating under reduced pressure to obtain a paste, and dissolving in a mobile phase to obtain solution containing the quercetagetin; separating and purifying the quercetagetin from the solution containing the quercetagetin by adopting a preparative high-speed countercurrent chromatograph; and performing high performance liquid chromatography (HPLC) detection, wherein the product with the purity of over 95 percent is qualified. The method has the advantages of low requirement on solvent purity, large separation amount, low loss of samples, high recovery rate and the like, and is suitable for separating and preparing the quercetagetin on various scales from laboratory preparation to industrial production.

The invention belongs to the field of natural organic chemistry and relates to a method for purifying eugenol, in particular to a preparation method for enriching and purifying eugenol in Chinese pink herb by using a high-speed countercurrent chromatographic separation method. The method is characterized by comprising the steps of: processing leach liquor of natural plant Chinese pink herb by using the high-speed countercurrent chromatographic separation method and purifying twice to obtain the eugenol with the purity of 90%. The method is suitable for natural plants containing the eugenol, and the extract of the natural plants is used as a raw material for preparing high-purity eugenol. The method is suitable for preparing the eugenol by adopting various models of countercurrent chromatographic instruments in a separation manner, liquid-liquid distribution chromatographic separation can be continuously, efficiently and rapidly carried out by adopting the high-speed countercurrent chromatographic method to prepare the eugenol, and the characteristics of high separation capacity, no sample loss, high recovery yield, alleviated separation environment, solvent saving and the like canbe achieved.

The invention discloses a method for preparing high-purity oleanolic acid from Aralia taibaiensis, belonging to the technical field of natural product extraction separation. The method comprises the following steps: 1) washing an Aralia taibaiensis oleanolic acid crude product with water, taking the insoluble substance, adding analytic methanol into the insoluble substance, sufficiently and evenly mixing, filtering, and taking the supernatant to obtain a loading solution; 2) filling a high-pressure preparative liquid chromatography column with octadecylsilane bonded silica gel, loading the loading solution to the high-pressure preparative liquid chromatography column, and eluting by using a methanol-water system as an eluate; and 3) carrying out sectional collection under the detection of an ultraviolet detector to obtain an oleanolic acid solution, concentrating the oleanolic acid solution under reduced pressure, and washing with water to obtain the high-purity oleanolic acid. The method can be used for directly and quickly separating out the oleanolic acid, and has the advantages of short separation time and high separation quantity; the yield is up to 85% above, and the purity is up to 98% above; and the method has the characteristics of less generated waste, small required eluate volume, recyclable filler and solvent and environment friendliness, and is suitable for industrial production.

The invention relates to the technical field of organic chemical synthesis and separation, and provides an efficient separating device based on a chromatographic theory. The device is composed of a pentagonal chromatography carrier unit and a fraction collecting unit, and organically integrates a thin-layer column chromatography separating method and a column chromatography separating method, so that the good separating effect of the thin-layer chromatography is kept, and the continuous chromatography characteristic of the column chromatography is also kept, and therefore, the efficient separating device has the characteristics of high separating efficiency, good separating effect and the like. Besides, separating speed can be further increased if the device is connected with a decompression device, so that separating time is reduced, consumption of a used mobile phase is saved, and complex TLC (Thin-Layer Chromatography) tracking work further can be saved, and therefore, the separating working efficiency is greatly improved. Besides, preparation is simple and regulation is convenient, so that the device is expected to be widely applied to the organic chemical field, especially quick separation of micro, semi-micro and small-scale organic compounds.

The invention discloses an extraction method for pomegranate foline and belongs to the chemical field of natural medicines. The method comprises the following steps: taking dry leaves of macaranga tanarius as raw materials, putting into a flash type extractor; taking hydrous ethanol as an extraction solvent for flash type extraction; filtering to obtain an extract liquid, followed by concentration; putting concentrated solution on a big-hole adsorption resin column; eluting by using water and 50-65 percent ethanol in sequence; adopting an anion exchange resin column, performing eluting by the NaOH solution; collecting the eluant; collecting the off-column liquid by using the cation exchange resin column, and obtaining the pomegranate foline through decompression and concentration. The method adopts flash type extraction and resin separation technology, is efficient and environment-friendly, and therefore is suitable for large-scale industrial production.