47results about How to "Separation environment relaxation" patented technology

The invention relates to a Chinese magnoliavine fruit monomer composition separation preparation method; ethanol extracts from Chinese magnoliavine fruit are extracted by petroleum ether, chromatography is carried out to the petroleum ether extracts by a silicagel column, and then the petroleum ether is eluted by petroleum ether-ethylacetate, and HPLC is used for monitoring, and then crude extract A and crude extract B are fraction-collected, and eluted; the volume ratio of eluant petroleum ether and ethylacetate is 3-5:1, the crude extract A and crude extract B are respectively applied to a high-speed counter-current chromatography for separation, so as to obtain SCHisanhenol, deoxyschizandrin, schizandrin B, schisandrin C, schizandrol A, schizandrol B and schisantherrin B monomers, and the purity is higher than 98 percent.

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 relates to a preparation method for a high-purity glabridin monomer, and relates to the preparation method for the high-purity glabridin monomer by separation from licorice. The preparation method mainly solves the problems of complicated preparation process, low separation efficiency, long separation time, and large consumption amount of a solvent. The method provided by the invention is characterized by comprising the following steps: preparation of a glabridin extract; concentration of glabridin by using a reversed-phase C18 column chromatography: successively eluting the extract with alcohols respectively with a concentration of 50%, 70% and 95%, respectively collecting eluents, and subjecting the collected eluent of the alcohol with the concentration of 70% to vacuum concentration until the eluent is dried so as to obtain crude glabridin; and separation of the above-mentioned crude glabridin with a high-speed countercurrent chromatographic technology: placing a separating solvent in a separatory funnel and carrying out complete shaking, then carrying out standing and layering, dissolving the above-mentioned crude glabridin in the separating solvent, and respectively measuring the concentrations of supernatant and subnatant solutions containing the glabridin with a highly-efficient liquid-phase chromatographic method. The preparation method for the high-purity glabridin monomer provided by the invention has short separation time and high recovery rate, is free of pollution, and saves the solvent.

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 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.

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 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 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 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 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 relates to a method for preparing a high-purity rhynchophylline monomer and belongs to the technical field of separation and purification of active ingredients of a traditional Chinese medicine. The method comprises the following steps: a, loading a rhynchophylline extract sample on a silica gel chromatographic column, eluting with a halogenated alkane-alcohol system, collecting eluate and concentrating to obtain a rhynchophylline crude product; and b, loading the rhynchophylline crude product dissolving solution on high-speed countercurrent chromatograph to respectively obtain a rhynchophylline monomer and a corynoxeine monomer. The method has the advantage that two monomers, namely, rhynchophylline and corynoxeine each of which the purity is more than 96% can be effectively prepared.

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 relates to a preparation method for separating high-purity hispidulin and herba lycopi flavone from common sage herb by high-speed countercurrent chromatography. The preparation method comprises the following steps of: (1) preparing a proper solvent system and standing to laminate so as to obtain an upper phase and a lower phase; (2) selecting the upper phase as a stationary phase and the lower phase as a mobile phase, filling the fixed phase into a countercurrent chromatograph column, adjusting the rotating speed of a host to be 600 to 1,000 rpm, pumping the mobile phase into the column at the flow velocity of 0.5 to 5.0 ml / min, and performing sample introduction by a sample valve after the whole system establishes dynamic balance; and (3) receiving target components according to a detector ultraviolet spectra, concentrating and crystallizing to obtain the high-purity hispidulin and herba lycopi flavones. The method is applicable to various types of high-speed countercurrent chromatographs and preparation of calycosin with different content, and has the characteristics of large separation quantity, high recovery rate and simpleness and convenience of operation.

The invention discloses a method to prepare high-purity capsaicin monomers. The separation solvent system is composed of alkyl halies, alcohol, water, etc. The separation solvent system is arranged inthe separating funnel, and is shaken and then kept still for stratification, the upper phase is taken as fixed phase and the lower phase as mobile phase. A proper dosage of sample is weighed and dissolved in the mixed solution of the upper phase and the lower phase. Firstly, the fixed phase is pumped to fill fully a chromatographic separation column at the specified flow rate, and then the head end of the column is connected with a six-way sample-feeding valve. The speed controller is started; when the rotational speed reaches to 800r / min, the sample solution is pumped into the mobile phase atthe flow rate of 2.0mL / min; when the mobile phase effuses from the chromatographic column, the sample is loaded, and each separated peak is collected; high-performance liquid chromatography (HPLC) is adopted to measure the purity, and three monomers i.e. dihydrocapsaicin, capsaicin and nordihydro-capsaicin are achieved. The method is applicable to the preparation of such three high-purity capsaic in monomers by the crude extracts of the capsaicin obtained through various approaches. The method is characterized in simple operation, low production cost and free of organic solvent residue; and the method can be promoted for the preparation of high-purity capsaicin monomers.

The invention discloses a preparation method of high-purity peiminin A and peiminin B, which adopts high-speed countercurrent chromatographic technology, and comprises the following steps: preparing Fritillaria japonicus extract as a sample; configuring to form a stationary phase and a mobile phase Solvent system; when the stationary phase and flow are the same, the pump is pumped into the column; the main engine rotates, the sample is injected by the injection valve, the elution solvent is detected, the target component is received, and the product is collected. The solvent system used can be composed of chlorinated alkanes, aliphatic alcohols or aliphatic ketones, dilute acidic solutions. The method can obtain high-purity monomeric alkaloids: peimin A and peimin B from the crude extract of Fritillaria japonicus, and the purity is as high as 98% and 95% respectively. The method is simple and convenient to operate, low in cost, high in recovery rate and easy to popularize and use.

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.

The invention relates to a method for preparing a high-purity rhynchophylline monomer and belongs to the technical field of separation and purification of active ingredients of a traditional Chinese medicine. The method comprises the following steps: a, loading a rhynchophylline extract sample on a silica gel chromatographic column, eluting with a halogenated alkane-alcohol system, collecting eluate and concentrating to obtain a rhynchophylline crude product; and b, loading the rhynchophylline crude product dissolving solution on high-speed countercurrent chromatograph to respectively obtain a rhynchophylline monomer and a corynoxeine monomer. The method has the advantage that two monomers, namely, rhynchophylline and corynoxeine each of which the purity is more than 96% can be effectively prepared.

The invention relates to a method for separating and preparing echinacoside in herba cistanche. The method comprises the following steps of: dissolving an ethanol extractive of a herba cistanche medicinal material in water; adopting polyamide column chromatography and eluting with water and ethanol; recovering a solvent, decompressing and concentrating; purifying by adopting intermediate-pressurepreparative chromatography, wherein a chromatographic column is a C18 column, methanol and 0.5 percent acetic acid aqueous solution are used as an eluant, and the volume ratio of the methanol to the 0.5 percent acetic acid aqueous solution is (1-2.5):(4-1.5); HPLC monitoring; collecting a sample containing the echinacoside and drying by distillation; separating the sample containing the echinacoside by adopting a high speed counter current chromatograph; arranging a solvent system containing n-butyl alcohol, ethylacetate, ethanol and water in a liquid separating funnel; and sufficiently shaking the solvent and then standing still for 12 hours for layering, wherein an upper phase is used as a fixed phase, a lower phase is used as a flowing phase, and the volume ratios of the n-butyl alcohol to the ethylacetate to the ethanol to the water is (1-5):(1-5):(0.2-1):(5-10). The method is used for preparing the echinacoside, and the purity of the prepared echinacoside is higher than 98 percent.

The invention provides a method for preparing high-purity arundoin. The method provided by the invention comprises the following steps of: crushing cogongrass rhizome and leaching by using an ethanol solution; decompressing and concentrating to obtain an ethanol extractive; extracting the ethanol extractive through utilizing trichloromethane and carrying out a chromatography on a decompressed and concentrated trichloromethane layer through utilizing a silica gel column; eluting by using trichloromethane-acetone and collecting eluent flowing from 2-4 column bed volumes; decompressing and concentrating the eluent and then standing and crystallizing; filtering the crystal, separating by taking n-hexane-ethyl acetate-methanol-water as a solvent system and utilizing a high-speed countercurrent chromatography, and detecting by an ultraviolet detector; collecting fluid and recycling reagents; and then re-crystallizing by using methanol and drying to obtain the product. The method provided by the invention is used for purifying the arundoin; and the method has the advantages of simple and easily-operated process, high efficiency and high product content so that the method is suitable for the industrial preparation.

The invention adopts high-speed countercurrent chromatography (HSCCC) to provide a preparation method of a high-purity paclitaxel compound. The method comprises steps: (1) pretreatment, 200mg-5g paclitaxel crude extract is heated and dissolved with 20ml-250ml stationary phase for use; , component D according to the volume ratio of 3-7:3-7:3-7:3-7, shake well and stand to separate the upper phase and the lower phase, the upper phase is used as a stationary phase, and the mobile phase is pumped into the column Inside, the sample is injected by the injection valve, and the target component is received according to the ultraviolet spectrum of the detector; (3) post-processing, the collected paclitaxel fraction is concentrated to dryness under reduced pressure to obtain a white solid, which is dissolved and crystallized, and obtained after filtration and drying. Needle-like crystals, the crystals are detected by HPLC, and the purity is above 99%. The method 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 thecomponent 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.