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

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.

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 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 discloses a method for preparing high-purity sucrose fructan monomer by high-speed countercurrent chromatography. First, the hydroxyl groups of fructooligosaccharides are protected to obtain fructooligosaccharide derivatives, and then high-speed countercurrent chromatography is used to analyze the fructooligosaccharide derivatives. Separation is performed to obtain fructotriose derivatives, fructotetraose derivatives and fructopentaose derivatives, and then the hydroxyl protecting group is removed to obtain high-purity fructotriose, fructotetraose and fructopentaose. The purity of fructotriose, fructotetraose and fructopentaose obtained by the present invention are all above 98%, and the separation time is short, the preparation amount is large, the production can be scaled up, the recovery rate is high, the sample is not lost, and the separation environment Moderate, save solvent.

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.