1044 results about "Column chromatography" patented technology

The invention discloses an online component detection method and system based on a salvia miltiorrhiza extracting solution chromatography elution process, and relates to the technical field of traditional Chinese medicine quality control. The method comprises the following steps: carrying out an elution experiment on a salvia miltiorrhiza extracting solution based on a column chromatography technology to obtain a sample set; acquiring near infrared spectrum and ultraviolet visible spectrum data in the sample; matching a spectrum fusion model according to the type of the to-be-detected component, and constructing different spectrum fusion models based on different fusion strategies for the near infrared spectrum and the ultraviolet visible spectrum; and processing data of the near infrared spectrum and the ultraviolet visible spectrum by using different spectrum fusion models to obtain the content of the to-be-detected component. On the basis of NIRS and UV-Vis technologies, online detection and analysis are carried out in the elution process of the salvia miltiorrhiza extracting solution by adopting a spectrum fusion and water spectrum omics method, and dynamic tracking and intelligent terminal point judgment of the salvia miltiorrhiza water-soluble active ingredients are realized.

The invention provides a separation and purification method of urokinase, and relates to the technical field of separation and extraction. The separation and purification method comprises the following steps: S1, regulating the pH value of male urine to 8.5, standing, and taking supernate; s2, mixing the supernate with an adsorption material, and eluting with an eluent to obtain a urokinase crude product solution; the adsorption material is a core-shell silica gel polymer, Fe3O4atSiO2-NH2 is taken as a core, and polystyrene is taken as a shell; the eluent is a sodium citrate buffer solution with the concentration of 0.5 to 0.15 M, acetonitrile with the concentration of 1 to 5 weight percent and EDTA (Ethylene Diamine Tetraacetic Acid) with the concentration of 0.5 to 1.5 mM; and S3, carrying out anion exchange column chromatography on the urokinase crude product solution, eluting with an eluent, and precipitating to obtain the urokinase. The urokinase prepared by the method has the advantages of high polymer urokinase content, high recovery rate and high activity yield.

The invention belongs to the field of natural product extraction, and relates to a method for extracting and separating flavonoid compounds from Artemisia chrysantha, which comprises the following steps: carrying out reflux extraction on the dry overground part of Artemisia chrysantha by using 70% ethanol, loading to a balanced D101 macroporous adsorption resin column, sequentially eluting by using water, a 20% ethanol aqueous solution, a 50% ethanol aqueous solution and a 70% ethanol aqueous solution, and collecting the eluent. Four fractions from Fr. I to Fr. IV are obtained; respectively carrying out polyamide column chromatography separation on Fr.II to Fr.IV, and sequentially eluting with a 20% ethanol aqueous solution, a 50% ethanol aqueous solution and a 70% ethanol aqueous solution to respectively obtain three fractions; and further purifying the Fr.II-1, the Fr.II-2, the Fr.III-1, the Fr.III-2, the Fr.III-1 and the Fr.III-3 by virtue of a Sephadex LH-20 column, so as to finally obtain seven flavonoid compounds. According to the method, only the ethanol water low-toxicity solvent is used for extraction and preparation, organic solvents with high toxicity are not used, the method is green and environment-friendly, the extraction efficiency is high, the number of extracted compounds is large, chemical components of the artemisia europaea medicinal material are enriched, the resource source of active components is widened, and a foundation is laid for follow-up research.

The invention discloses an efficient separation and purification method of MLnM type medium-chain and long-chain triglyceride, and belongs to the technical field of separation and purification. The efficient separation and purification method comprises the following steps: S1, preparing a crude product; s2, mixing the crude product with an adsorbent for static adsorption; and S3, performing column chromatography elution on the static adsorption product, and performing dynamic chromatography to separate the MLnM type triglyceride. According to the efficient separation and purification method of the MLnM type medium-long-chain triglyceride, a neutral aluminum oxide static adsorption and dynamic column chromatography coupling process is adopted, the purity of the MLnM type triglyceride can be greatly improved and is far higher than that of other adsorbents, the whole process steps are clear, the steps of raw material preparation, static adsorption, dynamic chromatography and the like are included, and the method is suitable for industrial production. The operation process is easy for standardized and large-scale production, and does not need to depend on complex equipment such as molecular distillation, supercritical CO2 extraction and the like.

The invention discloses a method for preparing various bioactive peptides based on bean dreg fermentation, which comprises polypeptides with alpha-glucosidase inhibitory activity, angiotensin converting enzyme inhibitory activity and antioxidant activity, and belongs to the field of microbial biological fermentation. Bacillus amyloliquefaciens sourced from fermented soybeans is used for fermentation, and a mixed product with alpha-glucosidase inhibitory activity, angiotensin converting enzyme inhibitory activity and antioxidant activity is obtained. The invention also provides a method for purifying the polypeptide with alpha-glucosidase inhibitory activity, angiotensin converting enzyme inhibitory activity and antioxidant activity, which is characterized in that the mixed product is purified by combined column chromatography, the combined column chromatography comprises cation exchange resin LXP-01, macroporous adsorption resin HP20, weak base anion exchange resin D941, silica gel resin and Sephadex LH-20. The invention also discloses seven bioactive peptides with biological activity, the amino acid sequences are CKLLL, APGYSC, FPKYG, FPGPLV, FPRSH, FMAV and SVCC, and the bioactive peptides have good alpha-glucosidase inhibitory activity, angiotensin converting enzyme inhibitory activity and antioxidant activity, and can be used for producing functional foods, health care products, cosmetics and the like for assisting in reducing blood sugar, reducing blood pressure, resisting oxidation and the like.

The invention relates to the technical field of extraction and separation of compounds in traditional Chinese medicinal materials, in particular to a method for simultaneously separating and purifying three pentacyclic triterpenoids from a tripterygium hypoglaucum root medicinal material. Three pentacyclic triterpenoid monomers are obtained through the steps of smashing, reflux extraction, normal-phase silica gel chromatography, reversed-phase high-pressure column chromatography, recrystallization and the like, the method is high in extraction efficiency and small in reagent dosage, the three pentacyclic triterpenoid compounds can be obtained at the same time, and the obtained compounds are high in purity and yield, have high social and economic value and are suitable for industrial production. The purity of the obtained plasmin, tripterine and demethylzeylasteral is high, and a foundation is laid for the preparation and production of reference substances of triterpenoid components in the roots of pyracantha fortunei, the subsequent pharmacological activity and the development of new immune drugs.

The invention discloses a novel benzofuran component in eupatorium chinense and application of the benzofuran component in anti-inflammatory activity. The obtained compound is separated from an eupatorium chinense extract. The eupatorium chinense root extract is separated by using an extraction method, macroporous adsorption resin impurity removal, Sephadex LH-20 gel column chromatography, high performance liquid chromatography and other methods. According to the present invention, all the separated compounds and the analogues thereof have good inhibition activity on target cyclooxygenase-2 of inflammation-related diseases, and have good inhibition activity on COX-2 enzyme, and the molecular docking experiment results show that the compounds and the target proteins have good binding energy. Therefore, the compound can be used for preparing drugs for treating inflammatory related diseases, or anti-inflammatory and analgesic drugs, or tumor drugs by inhibiting COX-2 enzyme, such as drugs for rheumatoid arthritis, osteoarthritis, ankylosing spondylitis, Alzheimer's disease and the like, and related natural lead compounds are provided.

The invention discloses a digestion-aiding highland barley fried malt polysaccharide as well as a preparation method and application thereof. The polysaccharide is extracted from highland barley through hot water extraction, ethanol precipitation, deproteinization, ion exchange column chromatography, gel column chromatography and dialysis processes. Animal experiments show that the polysaccharide can significantly improve the small intestine propulsion rate of mice and increase the weight increment, gastric juice amount, pepsin activity and pepsin discharge of rats, and the effect of the polysaccharide is superior to that of traditional roasted barley malt polysaccharide; the highland barley polysaccharide is superior to highland barley crude polysaccharide, highland barley polyphenol, highland barley lipid, highland barley protein and the like. The invention has the advantages of easily available raw materials and green process, is suitable for developing side-effect-free digestion-aiding functional foods such as tea bags, milk tea, yoghurt and biscuits, and has important market value.

The invention discloses a stationary phase of a novel zwitterionic monomer containing a multi-charge structure as well as a preparation method and application of the stationary phase, and belongs to the technical field of hydrophilic interaction chromatography (HILIC) stationary phases. According to the method, multi-charge zwitterions are used as hydrophilic monomers, the multi-charge structure of the multi-charge zwitterions endows the monomers with higher hydrophilic performance, and the multi-charge zwitterions are immobilized on the surface of a matrix by utilizing an active free radical polymerization method, so that a series of novel super-hydrophilic HILIC stationary phases are finally prepared. The multi-charge zwitterionic monomer adopted by the invention not only has better hydrophilic performance and higher charge density, but also can efficiently, simply and conveniently realize matrix surface grafting and modification. The developed stationary phase is suitable for HILIC column chromatography separation analysis, and the HILIC chromatographic performance can be greatly improved; the method can also be applied to the fields of biological sample pretreatment, material science, marker clinical diagnosis and the like, and has high economic and social values.

The invention provides an extraction and purification method of tetraacetyl phytosphingosine. Comprising the following steps: pretreatment and plate frame filtration of tetraacetyl phytosphingosine fermentation liquor, flash evaporation drying of a thallus wet filter cake, microwaves of bacterial powder and reflux extraction of a solvent, reverse extraction, enrichment and impurity removal of an extracting solution, preparation of a crude extract, primary crystallization of the crude extract by a polar solvent, alternate solvent crystallization of a crystallized primary product and the like. The tetra-acetyl phytosphingosine is extracted from the bacterial powder obtained by flash evaporation and drying after thallus separation by adopting a microwave and extraction solvent condensation reflux technology, and the method has the advantages of small solvent dosage, high extraction speed and high extraction yield. Besides, silica gel column chromatography separation and purification are replaced by means of reverse extraction, enrichment and impurity removal and alternate solvent crystallization, use of a mixed solvent and generation of silica gel solid waste are avoided, the purposes of saving cost and reducing environmental pollution can be achieved at the same time, and the method has wider application prospects and better industrial production potential.

This invention discloses a butyrolactone compound with multidrug resistance reverse transcription activity, its preparation method, and its uses. The compound's structural formula is shown in Figure I. The preparation method includes the following steps: fermenting *Aspergillus pyrolyticus* (accession number CCTCC NO: M2014086) to obtain a butyrolactone fermentation product; extracting the fermentation product with ethyl acetate to obtain a crude extract; degreasing the crude extract with hexane and dichloromethane to obtain a final extract; and purifying the final extract using normal-phase silica gel column chromatography, reversed-phase medium-pressure column chromatography, and reversed-phase semi-preparative high-performance liquid chromatography. The advantage of this butyrolactone compound is that it possesses multidrug resistance reverse transcription activity and the ability to regulate P-gp-mediated drug efflux in multidrug-resistant cell lines, making it a potential drug for treating multidrug-resistant cancers.

The invention discloses a synthesis and purification method of a trihydroxy phenol compound, which comprises the following steps: dissolving a crude product of resorcinol or a derivative thereof in methanol to obtain a solution, dropwise adding a methanol solution of p-toluenesulfonic acid and a ketone compound into the solution, and carrying out catalytic reaction at 50-70 DEG C to obtain a reaction solution; dropwise adding the obtained reaction liquid into deionized water at the temperature of 0-5 DEG C at the speed of 1-3 mL / min, stirring to separate out a white solid, and performing suction filtration to obtain a crude product; dissolving the crude product in ethyl acetate, adding column chromatography silica gel powder, stirring and adsorbing, separating supernate, and concentrating; and dissolving the concentrated solution in a mixed solvent of methanol and water, heating to 60-65 DEG C, dissolving, cooling to below 5 DEG C at a rate gradient of less than or equal to 0.5 DEG C / min, crystallizing, filtering, and drying to obtain the high-purity target compound. The method is simple and rapid in process synthesis, short in production period, low in production cost, high in target product total yield and suitable for industrial production.

The invention relates to the technical field of biological medicines, in particular to a polycyclic polyisopentenyl cyclopentanone compound as well as a preparation method and application thereof. The polycyclic polyisopentenyl cyclopentanone compound provided by the invention has a structural formula as shown in a formula 1; the preparation method comprises the following steps: by taking dry fruits of hypericum berry as raw materials, carrying out percolation extraction and concentration to obtain an extract, suspending the extract in water to obtain a suspension, and extracting and concentrating the suspension with petroleum ether to obtain a crude extract; the crude extract is taken and subjected to positive and negative phase silica gel column separation, MCI medium-pressure column chromatography, Sephadex LH-20 gel column chromatographic separation, high performance liquid chromatography preparation and CHIRALPAK IG chiral column resolution, and the polycyclic polyisopentenyl cyclopentanone compound is obtained. The protection activity of the compound on AC16 myocardial cell injury induced by cold ischemia is evaluated, and the compound can be used for preparing the polycyclic polyisopentenyl cyclopentanone compound. The compounds can be used as lead compounds for developing medicines for preventing and treating myocardial cold ischemia injury.

The invention discloses a preparation method of crocodile liver peptide for improving liver injury, and relates to the technical field of bioactive peptide extraction, and the preparation method comprises the following steps: crocodile liver pretreatment: cutting fresh crocodile liver into blocks, mixing with deionized water, homogenizing, and adding a zirconium phosphate molecular sieve to obtain crocodile liver homogenate; enzymatic hydrolysis reaction: adjusting the pH value of the homogenate, and adding a compound enzyme preparation for enzymatic hydrolysis; carrying out enzyme deactivation treatment, namely heating, cooling, centrifuging and taking supernate; performing ultrafiltration separation, namely filtering the supernate through an ultrafiltration membrane, and collecting a small molecule peptide solution; purifying and refining: purifying through sephadex column chromatography, and freeze-drying to obtain a crocodile liver peptide product; a double-particle-size zirconium phosphate molecular sieve is constructed to cooperate with a compound enzyme preparation for enzymolysis, electron transfer is enhanced by combining phosphorylation modification, the defects of metal inhibition enzyme activity, insufficient concealed peptide fragment cutting and oxidative damage are overcome, meanwhile, the application of the crocodile liver peptide in the aspect of improving the liver function is researched, and the crocodile liver peptide has a good application prospect. And a new choice is provided for prevention and treatment of liver diseases and liver health care.

The invention relates to the technical field of natural medicines, in particular to a 3 / 6 / 5 / 6 / 5 pentacyclic phloroglucinol compound as well as a preparation method and application thereof. The 3 / 6 / 5 / 6 / 5 pentacyclic phloroglucinol compound disclosed by the invention has a structure as shown in a formula I; the method comprises the following steps: extracting hypericum monogynum by using ethanol and petroleum ether, sequentially eluting the obtained petroleum ether extract through silica gel column chromatography, MCI resin column chromatography, Sephadex LH-20 gel column chromatography and ODS medium-pressure column chromatography, and purifying the collected eluate through preparative ODS liquid chromatography and semi-preparative ODS liquid chromatography to obtain the 3 / 6 / 5 / 6 / 5 pentacyclic phloroglucinol compound. The 3 / 6 / 5 / 6 / 5 pentacyclic phloroglucinol compound is extracted from hypericum monogynum for the first time, and the compound has great development value as a novel medicine for preventing or treating calcified aortic valve diseases.

The application belongs to the technical field of natural medicinal chemistry, and discloses a benzofuran compound in Jinyunming and a preparation method and application thereof. The benzofuran compound is separated from Jinyunming of the plant Dalbergia hupeana Tutch in the family of Leguminosae. The heartwood of Jinyunming is extracted and concentrated to obtain extract, the extract is sequentially separated by multiple silica gel column chromatography, medium-pressure ODS column chromatography and gel column chromatography, and then purified by semi-preparative high-performance liquid chromatography, so that the benzofuran compound can be obtained. The application establishes an inflammation model by inducing RAW 264.7 cells with lipopolysaccharide (LPS), and shows that the compound has good anti-inflammatory activity, the IC50 is 14.33 μM, and the expression of inflammatory factors interleukin-6 (IL-6) and interleukin-1β (IL-1β) can be inhibited.

The invention belongs to the technical field of data processing, and discloses an elution behavior prediction method and system, terminal equipment and a storage medium, and the method comprises the following steps: collecting a target liquid separated out in a simulated column chromatography elution process for multiple times at equal time intervals; carrying out near infrared spectrum collection on the obtained simulated collection samples in batches and carrying out preprocessing, training a long-short-term memory network combination model by using a sliding time window mechanism and using a plurality of batches of obtained simulated spectrum data sequenced according to time, and predicting a column chromatography elution process by using the trained model. According to the method, the key nodes in the column chromatography elution process are predicted, so that the key nodes in the elution behavior can be efficiently and accurately identified, and an operator can accurately master the elution time of a target component.

The invention discloses application of benzofuran components in eupatorium chinense to reduction of uric acid, compounds 1-3 are obtained by being separated from an eupatorium chinense extract, and the compound 1 is a new compound. The eupatorium chinense root extract is separated by using an extraction method, macroporous adsorption resin impurity removal, HW-40F gel column chromatography, high performance liquid chromatography and other methods to obtain the benzofuran compound. According to the present invention, the inhibition activity of the gout disease related target xanthine oxidase of the separated compound 1-3 is tested, the experimental result shows that the compound 1-3 has good inhibition activity on the xanthine oxidase, and the molecular docking experiment shows that the compound 1-3 has good binding energy with the target protein. Therefore, the compounds 1-3 can be used for preparing a natural lead compound for delaying or treating diseases caused by xanthine oxidase and providing a natural lead compound in the field of treatment of hyperuricemia and gout.

The invention belongs to the technical field of medicine and health care, and discloses oleander oligosaccharide and a preparation method and application thereof, the molecular weight of the oleander oligosaccharide is 2900 Da, and the oleander oligosaccharide is composed of glucose, mannose, galactose and arabinose; the preparation method comprises the following steps: degreasing oleander roots with ethanol, respectively carrying out water extraction and gradient concentration alcohol extraction, and then sequentially carrying out ceramic membrane-ultrafiltration-nanofiltration enrichment, ion exchange column chromatography and molecular sieve gel column purification on the alcohol extract to obtain the oleander extract. The oligosaccharide can be applied to preparation of immunological enhancement drugs, corresponding tumor immune drugs or health care products. The preparation method is efficient and safe, and the prepared product is good in quality and can be applied to preparation of immunological enhancement drugs, corresponding tumor immune drugs or health care products.

The invention discloses a preparation method of 6-nitro-m-cresol, and belongs to the technical field of organic synthesis.The method comprises the steps that raw materials are subjected to esterification, water washing, sulfonation, nitration, desulfonation and refining in sequence, and the 6-nitro-m-cresol is obtained. According to the method, it can be guaranteed that the intermediate product is the 6-nitro derivative, generation of isomer impurities such as 2-site and 4-site is greatly reduced from the source, the reaction path is clear, and atom economy is good. The method does not need to depend on complicated means such as time-consuming column chromatography or precise fractionation, the requirement for high purity can be met only through conventional extraction and crystallization operation, the technological process is simple, the method is very suitable for large-scale production, and the product purity (measured through HPLC (High Performance Liquid Chromatography)) can stably reach 98% or above.

The invention relates to the technical field of organic synthesis, in particular to a method for synthesizing cyclopentane compounds through [3 + 2] cycloaddition reaction of aryl cyclopropane and olefin under the synergistic catalysis of bromide ions / visible light. The method comprises the following steps: in a nitrogen atmosphere, sequentially adding aryl cyclopropane, a benzyl malononitrile derivative, pyridine tribromide and a photocatalyst into a reaction solvent to obtain a mixture, stirring the mixture at the temperature of 40 DEG C under the irradiation of a 12W blue light LED lamp until the reaction is complete, and performing concentration and column chromatography purification to obtain the cyclopentane compound. The method has the advantages of mild reaction conditions, simple operation, simple and easily available raw materials and low cost.

The application provides a method for synthesizing an eplerenone intermediate N-1 by one-pot method, and belongs to the technical field of organic synthesis. The method is characterized in that: the eplerenone intermediate N-4 is dissolved in dichloromethane, a potassium carbonate aqueous solution and dibromohydantoin are added to perform an opening ring reaction; after the reaction is completed, hydrochloric acid is directly added to perform a rearrangement reaction; then water is separated and methanol is added in the organic layer to perform an ozonation reaction; then sodium sulfite is added to perform a reduction reaction; then hydrochloric acid is added to perform a methyl esterification reaction, so as to obtain the eplerenone intermediate N-1 crude product, and finally the eplerenone intermediate N-1 fine product is obtained through refining. The method realizes the one-pot synthesis of the eplerenone intermediate N-1 from the eplerenone intermediate N-4 through the continuous reactions of opening ring, rearrangement, ozonation, reduction and methyl esterification, and can avoid column chromatography purification, so that the method becomes a green chemical process route with greatly reduced organic solvent consumption and wastewater.

The invention belongs to the technical field of material science, and relates to a preparation method and application of an unsaturated bond extended tetraphenyl ethylene siloxane compound. An unsaturated bond is introduced into a siloxane group, and the siloxane group containing the unsaturated bond and a tetraphenyl ethylene derivative are subjected to a coupling reaction. The coupling reaction is carried out in an inert atmosphere, the temperature is 90-150 DEG C, and the time is 6-24 hours. And purifying the product by silica gel column chromatography to obtain the target compound. Unsaturated bonds are introduced into a tetraphenyl ethylene structure, so that the adjustability of the photochromic wavelength is realized, the performance of the compound is remarkably improved, the application range of the compound is remarkably widened, and a new thought and a new method are provided for development of photochromic materials.

The application discloses a kind of acanthopanax acid polysaccharides with intestinal protection function and its preparation method and application, belong to the field of functional food and biotechnology.The acanthopanax acid polysaccharide is by water extraction alcohol precipitation, after impurity removal, through DEAE-52 anion exchange column elution and collection 0.2 mol / L NaCl elution peak, and the uniform component obtained by Sephadex G-100 gel column chromatography purification.Its uronic acid content is 30%-40%, weight average relative molecular weight is 50-100kDa, mainly by glucose, galactose, galacturonic acid and arabinose, infrared spectrum has carboxyl characteristic absorption peak at 1736 cm-1 and 1615 cm-1.Experiments prove that the acanthopanax acid polysaccharide has antioxidant activity and hypoglycemic activity.The acid polysaccharide has protective effect on LPS-induced Caco-2 cell damage, can effectively reduce the secretion of pro-inflammatory factors TNF-α, IL-1β, IL-6, and improve the level of anti-inflammatory factor IL-10.The acanthopanax acid polysaccharide can be prepared into oral liquid, tablet candy, solid beverage and other functional food forms.

The invention discloses an anthraquinone compound with anti-MTV activity and a preparation method and application thereof.The anthraquinone compound with the anti-MTV activity is prepared from stems and leaves of desmodium caudatum through the steps of pretreatment, extract extraction, silica gel column chromatography and separation and purification, the molecular formula of the anthraquinone compound with the anti-MTV activity is C18H17O7, and the structural formula of the anthraquinone compound with the anti-MTV activity is shown in the description. The preparation method comprises the following steps: 1, 6-dihydroxy-2, 7, 8-trimethoxy-3-methyl anthracene-9, 10-diketone is used as a raw material, and is named as 1, 6-dihydroxy-2, 7, 8-trimethoxy-3-methyl According to the invention, the English name is 1, 6-dihydroxy-2, 7, 8-trimesoxy-3-methylanthracene-9, 10-dione, and the English name is 1, 6-dihydroxy-2, 7, 8-trimesoxy-3-methylanthracene-9, 10-dione. The present invention has the following structure. Activity tests show that the compound has a certain inhibition effect on MTV. The novel compound disclosed by the invention is novel in structure, has certain anti-MTV activity, can be used as an anti-MTV lead compound, and can be used for research and development of anti-MTV prevention and treatment drugs.

The invention belongs to the technical field of natural pharmaceutical chemistry, and particularly relates to a novel iridoid compound, namely, uncarcinin, separated from wingceltis, a pharmaceutically acceptable isomer of the novel iridoid compound, a wingceltis extract containing the novel iridoid compound, and a preparation method and application of the novel iridoid compound. The chemical structure of the utazonine is shown as a formula I, and the absolute configuration of the utazonine is (1S, 3S, 3aR, 4R, 7aS). The invention also provides a method for extracting the compound or the extract from the stem of the wingceltis, and purifying by combining pH gradient extraction with silica gel column chromatography, semi-preparative high performance liquid chromatography and gel chromatography to obtain the compound or the extract. The wingceltis cycline, the isomer of the wingceltis cycline, the wingceltis extract containing the wingceltis cycline or the pharmaceutical composition show remarkable gastric mucosa protection activity in an in-vitro cell model, particularly, the protection rate of the wingceltis cycline to ethanol-induced human gastric mucosa epithelial cell (GES-1) injury at the concentration of 50 mu M can reach 5.21%, and the wingceltis cycline, the isomer of the wingceltis cycline, the wingceltis extract containing the wingceltis cycline or the pharmaceutical composition show definite gastric mucosa protection activity.

The application discloses a synthesis method of 2'-OMe adenosine, comprising the following steps: S1. dissolving adenosine in DMF, and reacting with a methylation reagent in the presence of a base to obtain a mixture of 2'-OMe adenosine and 3'-OMe adenosine; S2. reacting the mixture of 2'-OMe adenosine and 3'-OMe adenosine with acetic anhydride in a solvent to obtain an acetylated mixture; S3. deacetylating the acetylated mixture under the action of ammonia, and crystallizing to obtain 2'-OMe adenosine; the application uses cheap and easily available raw materials and a safe alkylating reagent, synthesizes 2'-OMe adenosine through a shorter route, avoids column chromatography operation, and provides a new synthesis method of 2'-OMe adenosine which is easy to process.

The application discloses a Dendrobium nobile Lindl polysaccharide component group, a preparation method thereof and application of the Dendrobium nobile Lindl polysaccharide component group in immunoregulation. Four polysaccharide components with definite structures, namely DNP-0-1 (>100 kDa), DNP-0-2 (30-100 kDa), DNP-0-3 (<30 kDa) and DNP-1-1 (<50 kDa), are synchronously separated from Dendrobium nobile Lindl by combining ultrasonic extraction process optimized by a response surface method with DEAE-cellulose column chromatography and ultrafiltration membrane series grading technology. After structure characterization and in-vitro immunological activity evaluation, the four components all have immunoregulatory activity, and the activity of DNP-0-1 is optimal. Pearson correlation analysis shows that the content of galactose and the molecular weight are extremely significantly positively correlated with the immunological activity, and the content of glucose and mannose is significantly negatively correlated with the activity. The application establishes an integrated research system of 'preparation by grading-structure characterization-activity screening-structure-activity analysis', and provides a material basis and evaluation basis for the development of immunoregulatory drugs or functional foods.

The invention provides a preparation method of pitch-based porous carbon for high-performance silicon carbon. The pitch-based porous carbon is prepared by an integrated process of component separation, structure regulation and surface modification, is dissolved by an alkane solvent, and is filtered to separate an insoluble substance A, and the remainder is a mixture B of oil and wax; dissolving the oil component and the wax mixture B in acetone, freezing to crystallize wax in the mixture B, filtering and separating wax crystals, and distilling filtrate to recover the acetone to obtain the oil component; the insoluble substance A and an organic solvent are mixed, subjected to reflux extraction and filtered and separated, free carbon is obtained, and filtrate is an aromatic and resin mixed solution C; separating aromatic and resin components in the aromatic and resin mixed solution C by adopting column chromatography; heating and uniformly mixing the separated aromatic substances, resin, free carbon, oil and wax in proportion to obtain blended asphalt D; the surface-modified asphalt-based porous carbon material is obtained through carbonization activation treatment and then modification treatment, and the application requirements of batteries in different application scenes can be met.

The invention discloses a method for synthesizing a polysubstituted trifluoromethyl olefin compound from gem-difluoroallyl alcohol. The preparation method comprises the following steps: in a nitrogen (N2) atmosphere, sequentially adding a gem-difluoroallyl alcohol (R1R2OHCR3C = CF2) compound, acetic anhydride (Ac2O), a solvent dichloromethane (DCM) and a fluorine source pyridine hydrofluoride (Py.9HF) reagent into a 10mL Schlenk tube to obtain a mixture, stirring the mixture at room temperature (rt) until the reaction is finished, filtering, washing and drying to obtain the compound. A crude product obtained by the reaction is subjected to silica gel column chromatography separation to obtain the high-selectivity polysubstituted trifluoromethyl olefin compound. The preparation method disclosed by the invention can be carried out under mild conditions and is simple and convenient to operate, most of the adopted raw materials are simple and easily available or commercialized reagents, the reaction raw materials are easily available, the yield of the target product is high, the functional group compatibility of the product is good, and the application range of a substrate is relatively wide; the obtained polysubstituted trifluoromethyl olefin compound contains a plurality of functional groups such as trifluoromethyl, olefin and the like. The method provides a more efficient and safer new strategy for synthesizing the polysubstituted trifluoromethyl olefin under mild conditions, particularly, metal participation is avoided, a new opportunity is provided for green medicine synthesis, and the method is predicted to have wide application prospects in the fields of medicine research and development, natural product derivative synthesis, life science and the like.