323 results about "Chloroform methanol" patented technology

A process for preparing high-purity momordicoside from fructus momordicae includes such steps as pulverizing, reflux extracting in alcohol, filtering to obtain extract A, suspending it in water, extracting in ethyl acetate 1-3 times, recovering ethyl acetate mother liquid, extracting in n-butanol 1-3 times, recovering n-butanol to obtain extract B, passing it through polyamide column, water washing, concentrating to obtain coarse saponin, chromatography by silica gel column, eluting with chloroform-methanol-water, collecting coarse momordicoside V, chromatography, water washing, eluting with alcohol, and collecting product.

The invention provides a wool-fabric protease anti-felting method based on weak oxidation and cutinase pretreatment, which belongs to the technical field of dyeing and finishing of wool fabric in the wool-spinning industry. The method aims to overcome the defects that the chlorination-process for wool-felting prevention seriously pollutes environment and the single protease-method treatment is poor in fabric wettability and high in felting rate in order to achieve the aim of optimizing the protease treatment effect of the wool fabric. All-wool grey fabric is extracted in a chloroform-methanol or carbon tetrachloride-methanol solution to remove free oily impurities, is pretreated with hydrogen peroxide and cutinase in turn to improve the hydrophilicity of the fiber surface, and then is subjected to reduction processing in a protease solution so as to realize biological processing combined with wool enzyme reduction. The method makes the prior chlorination-process felting prevention replaced with a biological-method wool-felting prevention process, and the method not only can effectively improve the reduction rate and anti-felting effect of the wool fabric, and promote the improvement of fabric wettability, but also can effectively increase the dyeing depth of fabric, and reduce fiber damage in reduction processing, and is favorable for protecting ecological environment.

Belonging to the technical field of medicine extraction, the invention discloses a method for extraction of paclitaxel from taxus chinensis. The extraction method provided in the invention consists of: using a methanol solution to conduct warm soaking extraction of taxus chinensis bark or branch and leaf powder, then carrying out chloroform extraction, performing silica gel column chromatography twice, implementing elution with a chloroform-methanol gradient solution and an n-hexane-acetic acid gradient elution respectively, and removing polar impurities so as to obtain a paclitaxel crude product; and further, carrying out third normal phase column chromatography, taking chemically treated silica gel as a stationary phase to effectively separate paclitaxel, recrystallizing the paclitaxel obtained from the column chromatography, thus obtaining a paclitaxel pure product with purity of over 98% pure product, with a process transfer rate being more than 80%. All the reagents used in the extraction method belong to the industrial grade, and the method provided in the invention has the advantages of wide applicability, strong innovation, simple process, low separation cost, high product yield, thus having innovative production value for industrial separation and production of paclitaxel.

The present invention discloses a technique for separating out and purifying triptolide monomer from common threewingnut root. The technique is carried out according to the following technical steps: (A) heating and extraction: after ethanol or methanol is warmly soaked, dregs are removed; (B) solvent extraction: organic solvent is adopted to extract concentrated solution in order to enrich the product; (C) chromatographic column chromatography: with neutral alumina or silica gel as filler, dichloromethane-methanol or chloroform-methanol is used to carry out gradient elution, and cut fraction is collected by stages; (D) high-efficiency preparation and liquid phase separation; (E) crystallization: two-phase solvent crystallization is adopted to use petroleum ether-ethyl acetate, dichloromethane-methanol or methylene dichloride-ethyl acetate to crystallize the cut fraction collected by stages, so that the colorless spiculate crystal product of triptolide, the purity of which reaches over 99.5 percent, can be obtained. The technique, which has the advantages of simplicity, rapidness, little solvent consumption, economy, environment-friendliness and high yield, can prepare a large amount of the product for one time, thus having high economic and academic values.

The invention relates to a method for purifying huperzine A, which is easy for industrialized production. The method comprises the following production steps of: crushing of raw materials, acid water heating and extraction, membrane filtration, impurity removal and condensation, aminated chloroform extraction and condensation, medium-pressure alumina column chromatography, chloroform methanol recrystallization, and drying of a finished product. The method for producing the huperzine A has low energy consumption and short period.

A method for the preparing 20 (R)-ginseniside Rg3 includes dissolving panax notoginseng saponins (PNS) with water, adding acids (hydrochloric acid, phosphoric acid, sulfuric acid, acetic acid, glacial acetic acid, formic acid and the like) to adjust the pH to be 1 to 3, heating and returning the mixture for 30 minutes to 60 minutes, recycling an acid liquor and concentrating the acid liquor into paste, and drying the pasted liquor to obtain coarse converted products; and performing silica-gel column chromatography on the coarse converted products, performing gradient elution on chloroform-methanol-water, collecting an eluent, performing tracking detection through thin layer chromatography (TLC) compared with the ginseniside Rg3, merging flow parts mainly containing the ginseniside Rg3, recycling solvents with the amount two times of the amount of the pseudo-ginseng saponin before transformation, performing standing and filtration, and drying filter cakes to obtain the 20 (R)-ginseniside Rg3. Tested by high performance liquid chromatography (HPLC), the content of the 20 (R)-ginseniside Rg3 is larger than 90%. The method for preparing the 20 (R)-ginseniside Rg3 has the advantages of being simple, low in cost, high in product purity, and suitable for industrial production.

The invention relates to a method for preparing catalpol, which has simple operation, light pollution and less equipment investment. The method comprises the following processing steps of: taking fresh roots of rehmannia root; adding methanol of which the volume is 5 to 10 times weight of the fresh roots; refluxing for 2 to 4 times, and taking 0.5 to 2 hours for each refluxing; merging backflow liquid; filtering the liquid; recovering the methanol at reduced pressure and condensing the liquid; adding isopyknic water saturation butarol to extract for 3 to 8 times; merging a butarol layer; recovering the butarol at reduced pressure until the butarol is exhausted; adsorbing the butarol with a macroporous adsorbent resin column; carrying out water washing to remove impurities; carrying out elution with 5 to 30 percent ethanol; collecting eluent of which the volume is 3 to 8 times volume of the column; concentrating and drying the eluent; adding the eluent to a silica gel chromatographic column by a dry method; carrying out elution with chloroform-methanol-water (6:4:1); making the eluent in each column volume as one fluid part; collecting 3rd to 6th fluid parts; merging the fluid parts; recovering the solvent and concentrating the fluid parts; and adding anhydrous ethanol to crystallize. The catalpol prepared by the method has high product purity and is easy to realize industrialization expansion.

This invention discloses a method for separating vitexin derivatives, vitexin-4'-O-glucoside and vitexin-2''-O-glucoside. The method comprises: (1) pulverizing hawthorn leaves into coarse powder, extracting by refluxing in alcohol aqueous solution, filtering, incorporating the filtrates, vacuum-concentrating to no alcohol odor, removing impurities with macroporous adsorption resin AB-8 or D101, eluting with 30-80% ethanol, vacuum-concentrating to no alcohol odor, decolorizing with petroleum ether, extracting with n-butanol, vacuum-recovering n-butanol, separating the extract by silica gel column chromatography, eluting with chloroform-methanol at a ratio of (4-3):1, vacuum-concentrating the eluate, separating by silica gel column chromatography,, eluting with ethyl acetate-butanone-methanoic acid-water or ethyl acetate-acetone-methanoic acid-water, and standing at 0-15 deg.C to obtain vitexin-4'-O-glucoside and vitexin-2''-O-glucoside. The method has such advantages as high yield, high purity, simple process and low toxicity, and is environmentally friendly.

The invention is a method to separate main monomer components in soy isoflavone, using the mixture with not less than 40% soy isoflavone content as raw material, silica gel as sorbent, and chloroform-methanol solution as eluting system, its technical steps: preparing sample solution; processing sorbent and placing in column; applying sample, where the added quantity of sample solution is 5-15% of effective volume of separating column; eluting, where the eluent flow velocity is controlled at 0.5-1.5% of effective volume of separating column each minute, and collecting the eluent in sections; qualitatively detecting the collected eluents, respectively and compared with the contrast product; obtaining monomer components, combining the eluents with the same component, and respectively vacuum condensing and drying to obtain four main monomer components: genistein, daidzein, genistin and daidzin. It is detected by high efficiency liquid phase chromatography that each monomer component's content can reach above 90%.

Production of medicinal component snow bile pigment and its usage for preparing medicines in treatment of cancers are disclosed. The process is carried out by taking snow bile plant tuber, crushing, taking acetone 18-26 proportion as solvent, extracting by diacolation method, recovering extract in water-bath kettle at 60-75 degree to obtain extractive, adding extractive into silica gel 1-2 proportion, drying to obtain silica-gel column, gradient eluting by ethanol or chloroform with volume concentration 2-10%, recovering eluent to obtain coarse product, heating while dissolving for ethanol or alcohol in water bath, filtering, lowering to room temperature, re-crystallizing to obtain prism crystal with purity above 98%. It can be used to prepare medicines in treatment of hepatocarcinoma, lung cancer, gastric carcinoma, laryngeal cancer and leukemia.

The invention relates to a refined sweetsop total lactone for anticancer and a method for preparing the same. The method comprises that: Root, leaf and bark or seed of sweetsop are used as raw materials, are percolated and extracted by petroleum ether, chloroform, and acetic ether, or a mixed solution of the petroleum ether, the chloroform and acetic ether, or the raw materials are extracted by supercritical carbon dioxide; the raw materials adopts solvent method, namely the raw materials are heated and dissolved by the petroleum ether and are subjected to impurity removal to obtain sweetsop total lactone; and the sweetsop total lactone is subjected to silica gel column chromatography, is subjected to gradient elution by the petroleum ether-the acetic ether or the chloroform-methanol, and is separated and is refined to obtain the sweetsop total lactone taking Shikemoxin and valeric sweetsop as main compositions. The raw materials have rich sources, low price and availability; the obtained refined sweetsop total lactone has high content, clear compositions and controllable quality; and the preparation method has a simple process, low consumption and high yield, and can realize large industrialized production.

The invention discloses a method for producing microbial grease by fermenting inulin serving as a raw material. The method comprises the following steps of: hydrolyzing the inulin raw material by using inulase to prepare an inulin hydrolysate, adding yeast extract, peptone, potassium dihydrogen phosphate and MgSO4.7H2O into the inulin hydrolysate to obtain an inulin hydrolysate fermentation medium, inoculating trichosporon cutaneum seed liquid to the fermentation medium, performing fermentation culture, obtaining microbial grease bacteria by centrifuging after culture, drying the microbial grease bacteria, extracting the grease in the cells of the dried microbial grease bacteria by using an organic solvent chloroform-methanol method, and thus obtaining the microbial grease. By the method for producing the microbial grease by using the inulin, the grease raw material source of biodiesel is greatly expanded, the cost of the grease raw material for the biodiesel is remarkably lowered, and meanwhile, the problem of low value utilization of jerusalem artichoke tubers in the prior art is solved.

The invention provides an amino acid ionic liquid water-based additive and a preparation method and application thereof, belonging to the technical field of organic compounds of lubricating oil additives. The structural formula of the amino acid ionic liquid water-based additive provided by the invention is shown as a formula 1 which is described in the specification. The amino acid ionic liquid water-based additive provided by the invention is biodegradable, environment-friendly and pollution-free, and has good solubility. The prepared amino acid ionic liquid water-based additive can also befully dissolved in organic solvents with different polarities, such as chloroform, methanol and water, and has excellent anti-friction and anti-wear properties and high bearing capacity when used as alubricant of a steel/steel friction pair.

The invention provides a method for purifying arecoline, which comprises the steps: taking the arecoline material, removing the core, crushing, adding 5-10 times of alcohol or methanol solution with the concentration of 30-50%, refluxing and extracting for 2-3 times, recovering a reagent from an extracting solution, adjusting the pH of a concentrated solution by hydrochloric acid to be 3-5, adding macroporous resins for absorption, readjusting the pH of a lower column liquid to be 7-8, adding chloroform for extraction, using the extracting solution to recover the chloroform to obtain an oily betel nut extract, selecting a chloroform-methanol-water solvent system or a normal hexane ethyl acetate methanol-water solvent system, adopting a high-speed counter current chromatograph for separation, freezing, drying to obtain the high-content arecoline. The method adopted for producing the arecoline has the advantages of short production cycle and low cost.

The invention discloses an alkaloid dimer, a preparation method thereof and application of the alkaloid dimer as an antiviral agent. The method comprises the following steps: firstly, carrying out strain culture on fungus Pestalotiopsis sp.(ZJ-2009-7-6) during preparation, and carrying out fermental cultivation on the fungus; leaching the obtained mycelium with a chloroform-methanol mixed liquid (1 to 1) for three times, carrying out vacuum concentration, and extracting with ethyl acetate for three times, so as to obtain crude extractum; and sequentially carrying out positive slica column chromatography, Sephadex LH-20 gel column chromatography and HPLC (high-performance liquid chromatography) on ethyl acetate-phase crude extractum to obtain a compound shown in a formula I. The antiviral agent provided by the method has the characteristics that the compound shown in the formula I or a pharmaceutically acceptable salt is taken as an effective component for preventing and/or treating diseases caused by herpes simplex virus I (HSV-1) and/or enterovirus 71 (EV71).

The invention relates to a method for preparing a compound of 2, 4-dihydroxy-5-methyl-hypnone by separating the fermentation liquid of Polyporus picipes. In the method, a method of plate-to-flask liquid culture is adopted; firstly, peeled potato, glucose and distilled water with the pH of 7.2 approximately are sterilized and made into a culture medium; then the culture medium is cultured and fermented to obtain the fermentation liquid; the fermentation liquid is extracted by ethyl acetate to obtain extractum; the extractum is separated by column chromatography and is eluted by a chloroform-methanol system in a gradient way; and the pure compound of the 2, 4-dihydroxy-5-methyl-hypnone (II) is obtained after several times of silica gel column chromatography, reverse C18 column and Sephadex LH-20 gel column chromatography and separation by a recrystallization method. The invention can develop the 2, 4-dihydroxy-5-methyl-hypnone (II) into the original drug of antipathogen fungi antibiotic and solves the problem of the raw material source of the 2, 4-dihydroxy-5-methyl-hypnone, and the invention has the advantages of mild culture condition, being simple and easy for confecting the culture medium, and short fermentation time, etc.

The invention relates to a process for the isolation of compound scopoletin which is used as nitric oxide synthesis inhibitor from Artemisia annua and other plant families, said process comprising extraction of dried powdered material of different plant parts with an aqueous acetonitrite solvent in the ratio of 1:5 for 6 to 8 hrs., concentration of the extracted solvent upto 30% of its original extract under vacuum, partitioning the concentrated extract with halogenated solvent to transfer scopoletin in the non-polar halogenated solvent, drying halogenated solvent over anhydrous sodium sulphate and evaporating the solvent, crystallizing the residues in methanol and filtering the crystals, concentrating the filtrate and chromatographed on silica gel, eluting scopoletin in chloroform methanol mixture; and crystallization of the fractions containing the scopoletin to get the pure scopoletin compound.

The invention relates to a high-performance liquid chromatography of phosphatidylserine. The High-performance liquid chromatography comprises the steps of (1) preparing a phosphatidylserine standard solution, and using a chloroform-methanol solution to dissolve and fix the constant volume to be 80 to 400ug/ml; (2) preparing a phosphatidylserine sample solution, using the chloroform-methanol solution to dissolve and fix the volume, and diluting and preparing the sample solution of which the phosphatidylserine content is within the concentration range of standard serial solutions; (3) measuring the standard solution and the sample solution under the condition that the high-performance liquid chromatography cooperates with an evaporative light-scattering detector, performing logarithmetics on the peak area of the standard solution as a y-coordinate, performing logarithmetics on the concentration of the standard solution as an x-coordinate, drawing a double logarithmic standard curve, and finding the concentration of the sample solution from the double logarithmic standard curve according to the peak area. The high-performance liquid chromatography has the following beneficial effects: due to the fact that the high-performance liquid chromatography cooperates with the evaporative light-scattering detector, a simple and effective method is provided for the quality control during a phosphatidylserine production process through the entering of different mobile phase volume ratios.

Belonging to the technical field of natural polymers, the invention discloses an extraction method for ganoderma lucidum polysaccharide. The extraction method for ganoderma lucidum polysaccharide comprises the steps of: removing fat from ganoderma lucidum fruit body dry powder, adding the ganoderma lucidum fruit body dry powder into an extracting agent composed of water and glycerin to perform extraction, then carrying out filtration, and collecting the filtrate; re-extracting the filter residue by the extracting agent several times, carrying out filtration, and collecting the filtrate; combining the filtrate, and dissolving ganoderma lucidum polysaccharide in the obtained filtrate; then further performing ultrafiltration concentration to obtain a ganoderma lucidum polysaccharide solution; or conducting ultrafiltration to remove part of glycerin or water, thus obtaining a glycerin-containing ganoderma lucidum polysaccharide water solution. The glycerin-containing ganoderma lucidum polysaccharide water solution can be used as a functional additive of cosmetics or masks. The method provided by the invention makes use of the hydroxyl in the glycerin and polysaccharide to form strong hydrogen-bond interaction, is in favor of dissolution of polysaccharide, and enhances the extraction efficiency. Also the used extracting agent is safe, and environmental pollution caused by chloroform, methanol and other organic solvents or acid-base employed by traditional methods can be avoided.

The invention discloses an extraction method of dendrobine, which is simple and convenient to operate and small in pollution. The method comprises the technical steps of: 1) crushing a dendrobium stem raw material to 20-80 meshes, infiltrating by alkaline water, placing in a CO2 supercritical extraction tank to extract, wherein the CO2 flow is 1-5ml/min/g raw material, selecting 90% acetone as an entrainer, wherein the flow is 0.1-0.5ml/min/g raw material, the extraction temperature is 30-60 DEG C, the pressure is 20-30MPa and the extraction time is 1-4 hours, dissolving the extract by chloroform, filtrating and recovering chloroform to obtain a crude extract; and 2) separating and purifying by high speed counter current chromatography by using chloroform, methanol and water as a solvent system for the crude extract, and collecting the fraction according to the chromatogram and decompressing and drying the fraction to obtain dendrobine. With the adoption of the method for extracting dendrobine, the purity of the product is high, and the method is easy to realize industrial amplification.