512 results about "Silica column" patented technology

The invention discloses an isoflavone compound in a tobacco rhizome and a preparation method and application thereof. The preparation method comprises the following steps of: crushing a tobacco rhizome sample, performing ultrasonic extraction for 3 to 5 times by using 95 percent ethanol, combining the extracts, filtering, performing reduced pressure concentration to obtain an extract, primarily separating the extract by using silica gel column chromatography, further separating the extract by adopting high performance liquid chromatography, and thus obtaining the required new compound. Antibacterial activity screening test results show that the compound has strong antibacterial effect on common proteus species, escherichia coli, staphylococcus, bacillus subtilis and the like. The compound used for cigarette tipping paper plays an obvious role in inhibiting microbes for polluting the cigarette tipping paper.

The invention belongs to the technical field of medicaments, and particularly relates to a novel method for preparing weight-losing medicament orlistat by a fermentation method. The method for preparing the orlistat comprises the following steps of: extraction and filtering of fermentation solution, chromatographic impurity removal by macroporous absorption resin, silica column chromatography of orlistat after hydrogenation and the like. By method, the effects of better removing impurities and purifying products are achieved.

The invention discloses a production method for separation and purification of salidroside from rhodiola rosea. The method comprises the following steps: after being smashed, raw materials are thrown in from a throwing hopper; a mainframe of an extraction tank set rotates; the materials are slowly propelled from the front end of the set to the back end; and at the same time, extraction solvent is introduced in the extraction tank from a liquid inlet pipe at the tail end of the set, and penetrates the movable materials from the back end of the tank to flow to the front end; and the solid-phase and liquid-phase materials are fully contacted with each other in the inverse movement so as to extract the effective components of medicinal materials. Medicine dregs are forcedly pushed to a dreg outlet through a discharge conveyer for discharging, and are extruded by using a special juice extruder to extrude residual medicine juice from medicinal material organizations, so that the content of the residual medicine juice of the medicine dregs is reduced, the extraction efficiency is higher, and the extraction is more thorough. The method chooses macroreticular resins and combines with the silica column chromatography to purify, so that better separation effect is achieved. Finished products of salidroside with the highest yield of 1% and the content above 95% can be obtained.

The invention relates to a method for extracting and purifying 6-gingerol from ginger, which comprises the following steps: (1) extraction and concentration of gingerol: heating sliced ginger in ethanol under reflux, and concentrating to obtain a ginger extract; (2) leaching of gingerol: leaching the ginger extract to obtain a leaching solution, and recycling the extract under reduced pressure to obtain a gingerol crude extract; (3) silica gel column chromatography: dissolving the gingerol crude extract in ethyl acetate, adding silica gel, mixing, and after the solvent is volatilized, passing through a silica gel column by a dry process; after carrying out isocratic elution and thin-layer chromatography (TLC) detection, collecting the eluate part containing 6-gingerol, recycling the eluate under reduced pressure to obtain a 6-gingerol crude product; passing the 6-gingerol crude product through the silica gel column, and carrying out elution, detection, collection and solvent recycling to obtain the higher-purity 6-gingerol; and (4) purification by preparative HPLC (high performance liquid chromatography): dissolving the higher-purity 6-gingerol, purifying by preparative HPLC, carrying out isocratic elution, collecting the part with the maximum chromatogram peak, and drying by distillation to constant weight, thereby obtaining the high-purity 6-gingerol. The technique is simple and easy to operate; and the product has the advantages of high yield and good quality.

The invention relates to a method for preparing high-purity stevioside rebaudioside RC, and belongs to the technical field of food additives. In the method, stevioside is used as a raw material, rebaudioside RC content in the raw material is about between 3 and 15 percent, and recrystallization technology and column chromatography technology are combined. The method comprises the following steps of: performing recrystallization by dissolving the stevioside which serves as the raw material in methanol; stirring and crystallizing at the temperature of 4 DEG C for 24 to 48 hours; recovering a solvent from crystallization mother liquor under reduced pressure to obtain a concentrate; performing silica gel column chromatography on the concentrate under the conditions that a stationary phase is silica gel with particle size of between 200 and 300 meshes, the weight of the silica gel mixed with a sample is 2.5 times that of the concentrate and the mass of pure silica gel is 20 to 50 times that of the concentrate; performing elution by using a mixed solvent system of trichloromethane and ethanol in the ratio of 2 to 1 or dichloromethane and ethanol in the ratio of 2 to 1, wherein water content in the ethanol is 2 to 10 percent; and collecting rebaudioside RC-containing main section eluent, mixing, concentrating, drying, detecting and packaging. By the method, a rebaudioside C product with purity of more than 95 percent can be obtained; and the method has a simple process and is suitable for large-scale industrial production.

The invention discloses a coumarin compound and a preparation method and application thereof. The coumarin compound is obtained by being separated from tobacco rhizome, the molecular formula of the coumarin compound is C17H14O5, and the structure of the coumarin compound is as shown in the specification. The preparation method of the coumarin compound comprises the following steps: smashing a tobacco rhizome sample, then ultrasonically extracting for 3-5 times by using 90%-99% ethanol; merging extracting solutions; filtering, carrying out reduced-pressure concentration to obtain an extractum; and initially separating the extractum by adopting silica-gel column chromatography, and then further separating by adopting high performance liquid semi-preparation chromatography to obtain the coumarin compound. The coumarin compound disclosed by the invention has the advantages of simple structure, easiness for artificial synthesis realization and better cell activity on tobacco mosaic viruses and can be used as a lead compound resisting the tobacco mosaic viruses.

This invention discloses a method for preparing porous silica gel column material. The macropore sizes are 0.5-3.0 mum, and the mesopore sizes are 3-10nm. The volume of the pores is 2.5-3.5 cu cm/g, and the specific surface area is 250-710 sq cm/g. The compressive strength of the particles is 180-220 N.

The invention relates to a method for preparing ginkgolide compound, belonging to the medicine field. The invention is characterized in that ginkgolide compound raw materials are prepared through the following method that: ginkgo leaves or ginkgo leaf extracts are taken and are extracted in aqueous solution, the obtained extract liquid is filtered and is extracted by using organic solvent, the obtained extract liquid is concentrated and is mixed with 200-mesh to 1,000-mesh silica gel, the obtained mixture is dried, eluent rich in ginkgolide compound is collected by adopting silica column chromatography, the collected eluent is crystallized to respectively obtain ginkgolide A, ginkgolide B, ginkgolide C, ginkgolide J, ginkgolide M and ginkgolide K raw materials, and the contents are respectively 90 percent to 110 percent. The invention has the advantages that the purity of the ginkgolide compound prepared through the method is high; and the preparation process is simple, the transfer rate is high, the cost is low and the industrial scale production can be realized.

The invention discloses diamine monomer containing an asymmetric and non-coplanar structure, and a preparation method of diamine monomer. The structural general formula of the diamine monomer containing the asymmetric and non-coplanar structure is shown in the specification, wherein R represents an alkyl substituent, and Ar represents an aromatic substituent; under nitrogen protection, 2-alkyl substituted aniline and aromatic substitution substituted formaldehyde are heated, in an acidic condition, to obtain a crude product; the obtained crude product is further subject to purification through the silica column chromatography separation method, so that the diamine monomer containing the asymmetric and non-coplanar structure is obtained. The diamine monomer prepared through the invention has a high purity, is stable at normal temperature, has a simple synthesis method, and is suitable for industrial production; the obtained monomer has the asymmetric and non-coplanar structure, so that the prepared poly imide has excellent solubility, excellent thermostability, high optical transparency, low dielectric constant, and other excellent comprehensive properties.

The invention relates to a gain photon crystal optical fiber waveguide, which is composed of a core layer and a coating layer which surrounds the core layer. The inner coating layer of the optical fiber comprise solid microstructure point lattice which is formed by germanium-doped silica column, and forms outer bandgap of the gain optical fiber, the function thereof is that the multimode pump light can be strictly restricted in a second fiber core region which is provided with rare earth dopant ion, and improves the utilizing efficiency of the pump light; the second fiber core of the optical fiber is composed of the solid microstructure point lattice which is formed the rare earth ion silica column to form the inner bandgap of the gain optical fiber, the function thereof is that through the multimode pump light, the generated laser light can be strictly restricted in a first fiber core region which is formed by high pure silica glass. Adopting the solid gain photon crystal optical fiber can greatly improve the utilization efficiency of the pump light, improve beam quality of output laser light, enhance output power of the optical fiber laser, and reduce nonlinear effect of the high-power laser device.

The invention discloses a method for separating active ingredients from an aquilaria sinensis lamina by utilizing a high-speed counter current chromatography. The method comprises the following steps of: extracting the dried and smashed aquilaria sinensis lamina by virtue of a percolation extract method at the room temperature to obtain an aquilaria sinensis lamina extracting solution extractum; extracting the extracting solution extractum for 3-4 times by sequentially utilizing petroleum ether,and ethyl acetate, respectively decompressing and concentrating a petroleum ether extract liquor and an ethyl acetate extract liquor to extractums; then respectively separating the petroleum ether part extractum and the ethyl acetate part extractum to obtain an active ingredient A of 7,4'-dimethoxy-5-hydroxy flavone by utilizing the high-speed counter current chromatography; and then separating the ethyl acetate part extractum through high-speed countercurrent chromatography to obtain an active ingredient B of 3,5,7,3',4'-pentahydroxy-flavone and an active ingredient C of 3,5,7,4'-tetrahydroxy-flavone after coarsely separating the ethyl acetate part extractum by virtue of a column chromatography on silica gel. The active ingredients separated by the method are low in loss, high in separation speed, high in purity, stable and easy to apply.

The invention relates to a nitrogen-sulfur co-doped carbon quantum dot fluorescent probe for cysteine detection and preparation and application thereof. The preparation method comprises the followingsteps of: (1) uniformly mixing ethylenediamine, deionized water and DTNB at room temperature to obtain a mixed solution, 2) setting the temperature of the mixed solution in a high-pressure kettle to be 160-220 DEG C, and performing carbonization treatment to obtain a carbonization treatment solution, 3) filtering, concentrating, purifying by silica gel column chromatography and drying the carbonization treatment solution in sequence to obtain N, S-CQDs, 4) preparing N, S-CQDs into an N, S-CQDs solution, and 5) uniformly mixing the N, S-CQDs solution with a palladium source to obtain Pd<2+>/N,S-CQDs. The Pd<2+>/N, S-CQDs are used for detecting cysteine in a water sample. Compared with the prior art, the fluorescent probe has the advantages of being simple in preparation method, high in sensitivity, good in reproducibility and the like, meanwhile, the fluorescent probe shows high selectivity on cysteine, interference of other metal ions or amino acid substances on detection can be effectively reduced, and the detection result has high reliability.

The invention provides triterpenoid compounds, which are prepared by the following steps: pulverizing and leaching a traditional Chinese medicine Lindernia crustacea, separating the extract through a silica gel column, and purifying by high performance liquid chromatography. The in-vitro cytoactive experiment proves that the separated compounds have nerve growth factor NGF-like activity, and the in-vivo animal experiment proves that the separated compounds B have the effect of enhancing the senile dementia model mouse memory function; and therefore, the compounds can be applied to preparation of medicines or foods for preventing and treating senile dementia and other neurodegenerative diseases, and especially to preparation of medicines or foods for treating Alzheimer's disease (AD) and other neurodegenerative diseases. The preparation method provided by the invention is reasonable and simple to operate. The invention provides new therapeutic medicines for treating senile dementia and other neurodegenerative diseases. The structural general formula is disclosed in the specification.

The invention relates to a method for electrochemical synthesis of a carbazole compound. The method comprises the following steps: taking an N-substituted acylamino biphenyl derivative as a substrate,adding the substrate and an electrolyte into an organic solvent, inserting an electrode, stirring, carrying out electrolytic reaction, stirring in nitrogen at room temperature by taking a carbon rodas an anode and a platinum sheet electrode as a cathode, carrying out constant-current reaction, removing the solvent by using a rotary evaporator after the reaction is finished, and carrying out rapid silica gel column chromatography purification on residues to obtain a product. According to the method, the reaction is electrically promoted, expensive metal catalysts and other oxidizing agents are not needed, the reaction can be carried out mildly at the room temperature, the selectivity is good, the yield is high, the whole process is simple and easy to implement, and the concept of green chemistry is met. According to the method, no extra oxidant is needed, the method is simple and efficient, the substrate is wide in applicability, and the yield of compounds with different substituent effect groups can be very high. The preparation method is simple, economical and environment-friendly, and has a certain industrial prospect.

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 discloses a purification method of melanotan II, which mainly solves technical problem of chromatographic column damage caused by strong alkalinity. The purification method comprises the following steps: 1) filtering a melanotan II crude product solution through a 0.45-mu m filter membrane, carrying out gradient elution purification by using a polymer-based filler chromatographic column, a mobile-phase trifluoroacetic acid water solution as a phase A, an acetonitrile trifluoroacetate solution as a phase B, and collecting a peptide solution of primary target peak; 2) carrying out gradient elution purification on the primarily collected peptide solution through a reversed phase silica gel column by using octadecyl bonded silica gel as a stationary phase, a mobile-phase trifluoroacetic acid water solution as a phase A and an acetonitrile trifluoroacetate solution as a phase B, and collecting the peptide solution of target peak; 3) exchanging into acetate by an HPLC (high performance liquid chromatography) salt conversion process; and 4) carrying out rotary evaporation concentration on the final high-purity peptide solution under reduced pressure, and carrying out freeze-drying to obtain the powdery finished peptide product. The purification method disclosed by the method has the advantages of high purity and high yield, sufficiently protects the chromatographic column, lowers the cost, and is convenient for industrialized implementation.

The invention discloses a method for simultaneously determining multi-index ingredients of Simotang preparation, comprising the step of detecting the sample solution of the Simotang preparation by adopting high performance liquid chromatography (HPLC), wherein the chromatographic column is octadecyl silane bonded silicagel column, the flowing phase A is acetonitrile, the flowing phase B is aqueous formic acid with the volume percentage of 0.1%, gradient elution is adopted and the detection wavelength is 283nm. The invention also discloses a method for establishing fingerprint chromatogram of the Simotang preparation; by carrying out detection with the determination method and carrying out simulation with a computer, the fingerprint chromatogram of the Simotang preparation can be obtained.The determination method can be operated simply and conveniently, has strong specialization, excellent stability, precision, reproducibility and average recovery, can comprehensively detect various main effective ingredients in the Simotang preparation so as to obtain the scientific and reasonable fingerprint chromatogram of the Simotang preparation, and can wholly and exactly evaluate the effectiveness, safety, stability and quality homogenate of the Simotang preparation.

The invention provides an enhanced type fluorescent probe for detecting hydrogen sulfide. The fluorescent probe is an NRS fluorescent probe, the structural general formula of the NRS fluorescent probe is shown as (I), the preparation method comprises the following steps: adding nile red, 2,4-dinitrofluorobenzene and potassium carbonate into dimethylformamide, heating to 70-80DEG C, performing reflux reaction for 3 hours, extracting the reaction liquor by dichloromethane and collecting an organic phase, drying the organic phase with anhydrous magnesium sulfate, and purifying through silica column chromatography to obtain a target product. The probe has a mitochondrial location function, can perform real-time and on-site online detection to mitochondria, and can help us to further master the physiological function of the hydrogen sulfide and promote the understanding of physiological action of H2S, and provide a visible detection tool for research and development of novel cardiovascular drugs.

The invention discloses an adamantyl-modified near-infrared squaraine dye as well as a preparation method and application thereof. The preparation method comprises the following steps: (1) mixing an adamantine-modified aniline derivative with squaric acid, dissolving the mixture in proper solvents, connecting the solution with a water knockout drum, and carrying out reflux for several hours under the protection of N2; (2) cooling the reaction mixture obtained in the step (1) to the room temperature, and removing the solvents at reduced pressure, thus obtaining a crude product; (3) washing the crude product with petroleum ether for several times, and then purifying the product through silica gel column chromatography, thus obtaining the adamantyl-modified near-infrared squaraine dye product. The adamantyl-modified near-infrared squaraine dye and the preparation method have the prominent advantages that the squaraine dye has good stability and excellent optical property; the solubility of the dye in the water solution can be effectively improved after the squaraine dye is included by cyclodextrin; the squaraine dye can serve as a fluorescently and colorimetrically responsive pH probe; the 2-adamantyl-modified near-infrared squaraine dye is successfully applied to intracellular imaging of living cells so as to detect intracellular pH values.

The invention discloses a method for separating and extracting apigenin, acacetin-7-O-beta-D-glucoside and apigenin-7-O-beta-D-glucoside from dendranthema indicum, which belongs to a method for extracting chemical substances from a natural plant. The method is sequentially carried out according to the following steps of: 1. extract preparation; 2. extraction: sequentially extracting the extract of the dendranthema indicum by using petroleum ether, chloroform and ethyl acetate; and 3. separation and extraction: (1) carrying out normal-pressure and reduced-pressure silica column chromatography on the extracted part by using the ethyl acetate; and (2) separating fractions through a semi-preparative high-efficiency liquid chromatographic instrument to obtain the acacetin-7-O-beta-D-glucoside, the apigenin-7-O-beta-D-glucoside and the apigenin as compounds. In the method, the semi-preparative high-efficiency liquid chromatographic instrument is directly adopted for separation to obtain the three compounds after silica column chromatography is adopted, and the method has good separation effect, short time, high product purity and less environmental pollution.

The invention discloses a smallanthus sonchifolius diterpenoid acid and the salt as shown in general formula (I), drug combination using the compound as active component, the preparation method and the application of the compound and the drug combination in treating diabetes. The smallanthus sonchifolius diterpenoid acid and the salt is characterized in that: smallanthus sonchifolius leaf is extracted using water or hydrous ethanol; the extractant is concentrated to get concentrated extractant for smallanthus sonchifolius leaf which is arranged onto macroporous resin column; firstly water is used for elution until outflow of sample is decreased; 95% of ethanol is used for elution; 95% of ethanol eluent is then collected and decompressed and concentrated to get extraction; the extraction is arranged onto silica column; chloroform - methanol gradient is used for elution to get 1 to 8 of fractions; the fraction 1 is taken to prepare HPLC; ODS is used as a fixed phase and MeOH-H2O 74 : 26 is used as mobile phase; refractive index detector is used for detecting; relative chromatographic peak can be collected, thereby getting needed products through the preparation.

The invention discloses a method for extracting and purifying cannabidiol in industrial hemp. The method comprises the following steps: (1) crushing of raw materials; (2) drying; (3) leaching: addinga leaching agent into dried floral leaf powder, and carrying out leaching to obtain a crude extract with a content of 10-15%; (4) dewaxing: dissolving the crude extract with ethanol having a mass concentration of 85-100%, and carrying out freezing and filtering to obtain a CBD enriched product with a content of 25-40%; (5) molecular distillation: carrying out molecular distillation on the CBD-enriched product, wherein the content of collected CBD oil is 35-70%; (6) column chromatography separation: carrying out silica gel column chromatography separation on the CBD oil, reducing a pressure, and conducting concentrating to obtain coarse CBD crystals with a content of 95% or above; (7) recovery of eluate; and (8) recrystallization of CBD: dissolving the coarse CBD crystals with a crystallization solvent, and conducting filtering and the like to obtain a finished CBD product with a content of 99.5% or above. The method is advanced, stable and feasible in process, and has the advantages oflow investment, high benefit, high purity, high extraction rate and low pollution.

The invention discloses a method for preparing kestose and nystose through yacon. Method of water extraction by alcohol sedimentation is adopted and supernate thereof is taken, concentrated, frozen and dried to obtain faint yellow yacon oligosaccharide. The yacon oligosaccharide is analyzed through high pressure liquid chromatography with a chromatography condition as follows: a chromatographic column is APS-2HYPERSIL, a column temperature is 30 DEG C, a moving phase is acetonitrile-water (75 to 25, V/V), a flow velocity is 0.8ml/min, a sample size is 20 Mul and a differential detector is arranged. The yacon oligosaccharide comprises fructose, glucose, saccharose, kestose, nystose and 1F-Fructofuranosyl nystose with contents respectively as 38,30 percent, 16.44 percent, 14.58 percent, 12.29 percent, 12.17 percent and 6.2 percent. Silicagel column chromatography is implemented on a prepared oligosaccharide sample; glacial acetic acid, chloroform, absolute ethyl alcohol and water with a proportion of 3 to 11 to 11 to 1 are used as an eluant for elution; the eluant is collected in sequence and then is concentrated, frozen and dried to obtain the kestose and nystose. The purity of the kestose and nystose prepared through high pressure liquid chromatography can be more than 90 percent.

The invention relates to a flavonoid glycoside compound in flos elaeagni angustifoliae, and a preparation method thereof. The method comprises the following steps: taking flos elaeagni angustifoliae medicines as raw materials, extracting by solvent, extracting by solvent, carrying out separation through two or three ways including positive phase and reverse phase silica gel column chromatography,or glucan gel LH-20 column chromatography and a semi-preparation high-performance liquid chromatography, adopting thin-layer chromatography and the high-performance liquid chromatography to detect andanalyze to obtain two new flavonoid glycoside compounds, wherein the first compound is flos elaeagni angustifoliae glycoside A, and the second compound is flos elaeagni angustifoliae glycoside B. Through the measurement of in vitro inhibition of COX (cyclo-oxygense) enzyme activity, an experiment result indicates that the flavonoid glycoside compound separated from the flos elaeagni angustifoliaecan inhibits the COX enzyme activity in different degrees, and the flavonoid glycoside compound in flos elaeagni angustifoliae can be used for preparing anti-inflammatory medicines.

The present invention discloses a method for separating and enriching small DNA fragments from a DNA-containing sample. The method comprises: centrifugating a sample to prepare a cell-free sample, lysing, binding to a silica column, washing, carrying out partial elution, re-binding, washing, and carrying out elution. With the method of the present invention, the low content free fetus DNA in the blood plasma can be effectively enriched, the method is simple, practical and effective, and is suitable for simultaneous treatment of multiple samples, harmful substances such as phenol-chloroform and the like are not required, the obtained small DNA fragment has the high purity and can be used directly in downstream PCR, real time fluorescence quantitative PCR, sequencing and the like, and the good application prospects are provided.