201 results about "Alumina column" patented technology

A process for extracting ginkalide B and biobalide from gingko leaf includes such steps as baking gingko leaves, removing impurities, breaking, extracting in aqueous solution of alcohol, purifying by adsorptive column, extracting gingkalide purifying by alumina column, step crystallizing and recrystallizing.

The invention discloses a production technique of andrographolide and neoandrographolide, dehydroanddrographolide and oxyandrographolide; the technique comprises the following steps of: firstly preparing stem and leaf extract of andrographis paniculata, removing fat-soluble impurities such as chlorophyll and the like with petroleum ether, and then hot-melting the extract in lower alcohol or aqueous lower alcohol, conducting reflux and decolorization with active carbon, separating out a majority of andrographolide crystals, then removing flavonoid through an alumina column or alkali cleaning, obtaining the andrographolide, cold-melting the andrographolide with trichloromethane or dichloromethane for 2 to 4 times, filtering and obtaining two parts of filtrate and insoluble substances, concentrating the filtrate, then conducting solvent crystallization and recrystallization or column chromatography for separation, and finally, respectively obtaining dehydroanddrographolide and pure product of andrographolide; the insoluble substances go through solvent crystallization and recrystallization or column chromatography for separation to obtain the neoandrographolide and pure product of andrographolide. The technique has simple production equipment, simplified routes and easy operation, can realize industrialized batch production; and the proportion of neoandrographolide, dehydroanddrographolide and oxyandrographolide in the obtained andrographolide is high, while the content of impurities is low. The obtained neoandrographolide, dehydroanddrographolide and oxyandrographolide all have monomer purity of higher than 98 percent, thus being capable of being used as chemical reference substance of the traditional Chinese medicine, or being applied as raw materials of medicine and chemical industry.

A composition of paeoniflorin and albiflorin is prepared from peony through extracting in water to obtain aqueous solution, resin adsorption, alcohol eluting, concentrating, and chromatography by alumina column and silica gel column. It can be used to prepare to medicines in different forms.

A process for producing technetium-99m from a molybdenum-100 metal powder, comprising the steps of:(i) irradiating in a substantially oxygen-free environment, a hardened sintered target plate coated with a Mo-100 metal, with protons produced by a cyclotron;(ii) dissolving molybdenum ions and technetium ions from the irradiated target plate with an H2O2 solution to form an oxide solution;(iv) raising the pH of the oxide solution to about 14;(v) flowing the pH-adjusted oxide solution through a resin column to immobilize K[TcO4] ions thereon and to elute K2[MoO4] ions therefrom;(vi) eluting the bound K[TcO4] ions from the resin column;(vii) flowing the eluted K[TcO4] ions through an alumina column to immobilize K[TcO4] ions thereon;(viii) washing the immobilized K[TcO4] ions with water;(ix) eluting the immobilized K[TcO4] ions with a saline solution; and(x) recovering the eluted Na[TcO4] ions.

The invention discloses a method for preparing pneumocandin B0. The method comprises the following steps of: a) centrifuging the fermentation liquid of echinocandin B0, taking mycelium, leaching the echinocandin B0 in the mycelium with a first solvent and filtering and removing the mycelium; b) distilling the solvent in the first solvent leaching solution of echinocandin B0 to dryness, soaking with a second solvent and then filtering and removing the insoluble substances; c) distilling the second solvent soak solution of echinocandin B0 to dryness and then dissolving in the first solvent, andcollecting effluent liquid through overly acidic alumina column; d) distilling the collected solution of echinocandin B0 to dryness and then dissolving in the first solvent, utilizing adsorbent resin,performing eluting with the first solvent and then collecting the part with higher purity; e) distilling the collected solution of echinocandin B0 to dryness and then dissolving in the first solvent,utilizing inverse resin, performing eluting with the first solvent and collecting the part with higher purity; and f) distilling the collected solution of echinocandin B0 to dryness and then dissolving in the first solvent, adding in a small amount of water by dripping to achieve the purpose of separation by crystallization after supersaturation, and then preparing the echinocandin B0. The methodfor preparing the echinocandin B0 not only can well remove the pigment, but also leads the purity of the echinocandin B0 to be improved by more than 96 percent.

The present invention discloses a Rhizoma Corydalis Decumbentis total alkaloids extract, its preparation method, pharmaceutical composition containing same. The total alkaloids mainly comprise : macleyine, tetrahydropalmatine, bicucalline, palmatine hydrochloride, 'xiawuning' alkaloid, corydaline harmine, other alkaloid and extract. The preparation method is : using Rhizoma Corydalis Decumbentis as material, adding right amount of polar solvent for leaching, merging the leachate, carrying out large pore adsorption resin chromatography, eluting impurity with diluted acid and alkaline aqueous solution orderly, eluting using polar organic solvent, collecting elution liquor, eliminating impurity further by alumina column adsorption, Collecting after-column liquid, concentrating liquor to obtain the Rhizoma Corydalis Decumbentis total alkaloids extract. The present invention also discloses a pharmaceutical composition containing the total alkaloids extract and uses of the pharmaceutical composition in preparing tablet, capsule, soft capsule, suppository, granula, transdermal absorption agent, drop pills, oral disintegrating agent, slow release agent, freeze-drying powder injection etc.

The invention discloses a method for extracting high-purity sulforaphane from broccoli seeds; and the method comprises the following steps of: (1) after crushing dry broccoli seeds, adding water to the dry broccoli seeds to hydrolyze the broccoli seeds, so as to obtain a solid-liquid mixture; (2) adding anhydrous ethanol to the mixture; ultrasonically extracting the mixture; and carrying out suction filtration or double-layer gauze filtering on the mixture; (3) concentrating and evaporating ethanol from a filter liquor in a vacuum state; (4) carrying out chromatography on a material liquor by using a macroporous resin column and eluting the material liquor by using an ethanol solution in a gradient way; (5) collecting an eluting solution containing sulforaphane; carrying out chromatography on the eluting solution by using an alumina column; and concentrating a sulforaphane chromatography solution to form an extract so as to obtain a crude sulforaphane product; (6) adding water to the obtained crude product so as to dissolve the crude product; and extracting the dissolved crude product by using a polar solvent; and (7) collecting an organic layer; and concentrating the organic layer in a vacuum state so as to obtain an oily extract, so that the high-purity sulforaphane is obtained. As the high-purity sulforaphane can be directly extracted from the broccoli seeds and broccoli related materials, the method for extracting the high-purity sulforaphane from the broccoli seeds, disclosed by the invention, has the advantages of simple process, stable product, simple equipment and safety in production and is suitable for enterprises for industrially extracting the sulforaphane.

The invention relates to the plant extraction field and concretely relates to a new plant source for paeoniflorin extraction, and a paeoniflorin extraction method. The method for extracting paeoniflorin from peony seed meal is characterized in that the method comprises the steps of crushing, enzymatic hydrolysis, ultrasonic extraction with ethanol, microwave extraction with ethanol, macro-porous resin adsorption, alumina column adsorption, titanium rod filtration, membrane ultrafiltration, nanofiltration, concentration, and drying to obtain a paeoniflorin extract. According to the invention, waste peony seed meal which is treated as a raw material undergoes enzymatic hydrolysis, is added with the organic solvent ethanol for paeoniflorin extraction, and is extracted through a macro-porous adsorption resin, an alumina column, a titanium rod and membrane filtration, so the paeoniflorin extraction rate reaches 61.6%.

The invention relates to the natural medicine preparation field, and in particular, relates to a bulleyaconitine A preparation method; the preparation method comprises four steps: extraction, extraction separation, column chromatography separation purification, and crystallization purification. According to the bulleyaconitine A preparation method provided by the invention, alumina column chromatography is used for replacing silica gel column chromatography, so that the production cost is saved; a petroleum ether-diethylamine binary system is used as an eluent and is easy to recycle and reuse, so as to reduce environmental pollution.

The invention discloses a method for detecting dioxin and dioxin polychlorinated biphenyl in poultry eggs. The method comprises the following steps: (1) preparing a sample; (2) preparing a to-be-detected object; (3) purifying by virtue of an acid silica gel, (4) purifying by virtue of a multi-section silica gel column; (5) purifying by virtue of a gel chromatographic column; (6) purifying by virtue of an alkaline alumina column and a Florisil column or an activated carbon chromatographic column; and (7) carrying out machine testing. The method has the beneficial effects that the pretreatment is rapid and safe, and the matrix interference is slight; and by utilizing a high-resolution gas chromatography / double focusing magnetic mass spectrometer HRGC / HRMS in detection, the contents of dioxinand dioxin polychlorinated biphenyl in the poultry eggs can be relatively accurately acquired.

A process for preparing ginsenoside monomer from ginseng leaf includes such steps as preparing general ginsenoside from ginseng leaf, chromatography with alumina column to obtain several groups of ginsenosides, and chromatography by column to obtain different ginsenoside monomers.

The invention provides an analytical method of polycyclic aromatic hydrocarbon content and application thereof. The method includes the steps of: dissolving a to-be-tested sample and an internal standard substance in n-hexane, using n-hexane to perform elution on a silica gel column to obtain saturate fraction; connecting the silica gel column to the upper end of an alumina column in series, flushing the silica gel column and the alumina column with a mixed solution of n-hexane and dichloromethane to obtain aromatic fraction 1; separating the silica gel column from the alumina column, using a mixed solution of dichloromethane and n-hexane to flush the alumina column to obtain aromatic fraction 2; then using a mixed solution of dichloromethane and anhydrous ethanol to flush the alumina column to obtain aromatic fraction 3; concentrating the aromatic fraction 3, then employing toluene to bring the substance to a constant volume, and performing GC / MS analysis, thus obtaining the polycyclic aromatic hydrocarbon content of the to-be-tested sample. The method provided by the invention can perform quantitative analysis on the polycyclic aromatic hydrocarbon contained in environment friendly rubber filling oil and raw oil thereof.

The invention discloses a fritillaria medicinal material identification and content determination method comprising the steps: after extracting with ethanol, passing through a neutral alumina column, determining by high performance liquid chromatography, combining with specific chromatograms of medicinal materials, effectively identifying thunberg fritillary bulb, bulbus fritillariae cirrhosae and bulbus fritillariae ussuriensis, and determining the contents of peimine and peiminine. The method not only can effectively identify authenticity of the three fritillaria medicinal materials, but also can accurately determine for the contents of peimine and peiminine, achieves multiple evaluations through one-time determination, and is safe, environmentally friendly, convenient and quick.

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.

The invention discloses a method for synthesizing sweet saponin with bitter and fallen grosvenor momordica fruit as a raw material. The method comprises the following steps: 1) weighing and crushing bitter or fallen grosvenor momordica fruit, adding water or ethanol with a volume of 45 to 55% for extraction and subjecting obtained extract to macroporous resin column chromatography so as to obtain bitter grosvenor momordica fruit saponin, wherein the content of mogroside II and / or III is no less than 50%; 2) dissolving bitter grosvenor momordica fruit saponin in water, adding starch and cyclodextrin glucosyltransferase, carrying out an enzymic catalytic reaction at 60 to 65 DEG C until the reaction is completely finished, killing enzyme activity, carrying out filtering and collecting filtrate; and 3) subjecting the filtrate to macroporous resin or silica gel column chromatography, carrying out rinsing and collecting ethanol eluate with a volume of 30 to 40%, or directly allowing the filtrate to pass through an alumina column or active carbon column and collecting effluent, and concentrating and drying the collected ethanol eluate with the volume of 30 to 40% or the collected effluent. The method provided by the invention fundamentally overcomes the problem of bitter and fallen fruit in growth of grosvenor momordica fruit.

The invention relates to a notoginsen triterpenes purifying method using ultra-filtration and nano-filtration technology to extract trashes and purify the notoginsen triterpenes in notoginsen triterpenes production process using notoginseng as raw material. That is: notoginseng-> smashing-> enthanol eluting-> passing macroporous resin column-> passing alumina column->adding an amount of needle used active carbon, titanium rod filtering-> ultra-filtering-> nano-filtering-> refining and concentrating->drying->smashing-> notoginsen triterpenes. The process can also be used in Xuesaitong injection production process using notoginsen triterpenes as raw material. That is: adding water for injection into notoginsen triterpenes, mixing and boiling-> adding active carbon, filtering and fine-filtering->ultra-filtering->nano-filtering->adding an amount of sodium chloride, regulating pH value, diluting by an amount of water and obtaining the Xuesaitong injection. The invention achieves the advantages of simple production process, simple operation, good separation effect and no damage to bioactive substances, can eliminate macromolecular substance impurity and micromolecule substance impurity such as inorganic salt, thereby improving the purity of notoginsen triterpenes.

This invention discloses a method of extracting biao-gao-yi-chun from isatis root. The procedures include (a) ethanol water solution is back flow extracting solution and its weight is 30-95% of 6-12 times isatis root weight, then extracting solutions are combined. (b) Ethanol is recovered after filtration and then liquor is got. (c) The liquor flows through big holes resin adsorption column. (d) Scrubbing column is scrubbed by scrub solution until effluent liquid is leuko. (e) It is eluted by 30-95% weight percentage ethanol water solution, and eluent is collected. (f) The eluent is dried and solid substance is got. (g) Average particle diameter is -0.001-2mm powder is got after grinding. (h) The powder got from (g) is added to alumina column, (i) gradient elution is done by chloroform and ethanol component solvent, every 200-1000ml is one flow portion in order to add 0.1-2ml methanol after collecting every 50 portion. (j) The portions contain biao-gao-yi-chun are collected. (k) Solvent is discharged from the portion in (j), and then biao-gao-yi-chun extract product is got. This invention also provides the use of biao-gao-yi-chun in preparing antivirus medicine.

This invention relates to a hyperbranched polymer used as polythene processing assistant and its synthesis method, specifically the Polymer composed of higher alcohol of acrylic ester and styrene and the method of atom transfer radical polymerization. The invention synthesizes the hyperbranched polymer firstly through the following formula (weight): p-CMS 1, styrene 6.84~13.68, acrylic dodecyl alcohol ester 7.88~23.64, Bpy 0.21~ 0.63, CuCl 0.065~0.196. The above components conduct evacuation, filling argon or nitrogen for more than five times, closing tightly, and response under magnetic stirring for four to twelve hours and 100~130deg.C. The product is dissolved in acetone, filtered in alumina column, precipitated in ethanol, and dried in vacuum for a few hours under 25~40deg.C to obtain the hyperbranched polymers. The melt viscosity of this invention decreases significantly corresponding to pure HDPE, and its strength change is very small showed by the tensile performance test.

The invention relates to a method for extracting rubusoside from sweet tea leaves. The method comprises the following steps: (1) crushing sweet tea leaves, sieving the material, adding water, continuously performing countercurrent extraction, and filtering the material; (2) adding an enzyme preparation for enzymatic hydrolysis, and performing steps of inactivation, cooling, flocculation, filtration, and filter residue washing with water; (3) performing ultrafiltration and nanofiltration; (4) performing adsorption on macroporous adsorption resin chromatography column, washing the material withwater, discarding a washing solution, performing gradient elution with an organic solvent, and performing vacuum concentration; (5) performing adsorption on an alumina column, washing the material with water, and performing vacuum concentration; (6) adding activated carbon, stirring the material, filtering the material, and performing vacuum concentration and spray drying; and 7) dissolving the material with the organic solvent, and performing steps of filtering, crystallization, pumping filtration, vacuum drying, and crushing to obtain the rubusoside product. The extracted rubusoside productpresents pure white color, the purity is greater than or equal to 99%, and the yield is greater than or equal to 90.5%. The method of the invention has the advantages of simple operation process, short extraction time, low energy consumption and low cost, and can realize continuous large-scale production.

The invention provides a method for extracting phillyrin from forsythia, which relates to a novel method for extracting phillyrin by the steps of soaking with ethyl alcohol solution, adding surfactant and heating by microwaves. The traditional product generally has the defects of low yield rate, poor stability, high production cost and the like. The method comprises the following steps of: crushing forsythia into 16 meshes; adding 58% ethyl alcohol solution for soaking; adding surfactant which accounts for 0.03-0.3% of the weight of the mixture; heating by microwaves, standing and filtering; adding 58% ethyl alcohol solution into residues for soaking; heating by microwaves, standing and filtering; combining filter liquors, evaporating solvent by using a rotary evaporator, adding a small amount of methyl alcohol solution, adding alumina and uniformly stirring, and evaporating. The operations are performed on the basis of official method, the phillyrin is put on a treated neutral alumina column to elute and evaporate, and then the phillyrin powder is prepared. The invention is used for extracting phillyrin.

The invention relates to a method for simultaneously determining three alkaloids in granules for eliminating the phlegm and stopping the cough for children. The method is characterized in that the HPLC (High Performance Liquid Chromatography) method is employed for the first time, an ordinary gradient elution and reversed-phase chromatographic column are adopted, and acetonitrile, methanol and 0.1% phosphoric acid in the volume ratio of (1.5-2.5) : (12.5-11) : (86-86.5) are taken as the mobile phase; the detection wavelength is 205 nm; and the contents of ephedrine hydrochloride, cephaeline hydrochloride and emetine hydrochloride in the granules for eliminating the phlegm and stopping the cough for children are determined simultaneously, so as to end the history of no HPLC determining method for emetine and no quantitative determining indexes for granules for eliminating the phlegm and stopping the cough for children. The method provided by the invention comprises the steps of performing an ultrasonic treatment to a sample with methanol, sucking a certain amount of subsequent filtrate, removing impurities with an alumina column, and determining. The method has the benefits that crest separation of the three alkaloids is excellent, the baseline is stable, and 30 min is required to finish the determining; the quality control aim of being simple, convenient, quick, scientific, standard and multi-component quantitive by one maker is realized; and safety and effectiveness of taking granules for eliminating the phlegm and stopping the cough for children are ensured.

The invention relates to a separation and purification method for lappaconitine, which is used for preparing high-purity lappaconitine by integrating a solvent extraction-ion resin column-alumina column-recrystallization method and comprises the following steps: ultrasonically extracting the lappaconitine by utilizing ethanol, dissolving the concentrated lappaconitine by utilizing 1% of hydrochloric acid, adding cation exchange resins in a countercurrent mode, carrying out acid elution, regulating the pH value to neutral and desalting, wherein a column chromatography adopts a short and thick column; a filler is alumina; a mobile phase is the ethanol; and a recrystallization solvent is acetone-ethanol (the ratio is 1 to 1). The separation and purification method has the advantages of obvious reduction of organic solvents, in particular to toxic solvents, low cost, high yield, short production period and easy industrialization.

The invention relates to a method for preparing indirubin with simple and convenient operation, small pollution and little equipment investment. The method comprises the following technological steps:adding methanol with the quantity of 5-10 times of raw materials into the raw materials, extracting by ultrasonic for 1-3 times, extracting for 0.2-1 hour each time, merging extracting liquid, recovering the methanol by depressurization, concentrating, filtering liquor by a macroporous resin column, eluting with water firstly, removing impurities, then eluting with ethyl acetate, concentrating eluent, adopting chromatographic separation by an alumina column, eluting with chloroform-ethyl acetate, concentrating eluent, recrystallizing with methanol-acetone, washing, drying to obtain the indirubin. By adopting the invention to prepare the indirubin, the product purity is high and industrialization amplification is easy to realize.

The invention relates to a method for preparing nuciferine from lotus leaf; the process takes lotus leaf medical material as raw material and includes the steps that: the lotus leaf medical material is shredded, and is soaked in acid and extracted for 2-3 times, ammonia water is used for adjusting pH, and then the steps of concentration, chloroform dissolving, active carbon column decoloration, alumina column separation and chloroform-ethanol-ammonia water mixed solution elution are conducted to collect nuciferine fractions and recover reagents, and then the end products are obtained after placement crystallization, chloroform and ethanol recrystallization. The process is suitable for scaling up.

The invention relates to a method for extracting panax notoginseng saponins from fresh panax notoginsengs, which comprises the following steps: adopting the fresh panax notoginsengs as raw materials; crushing the panax notoginsengs; soaking the panax notoginsengs in ethanol and extracting the same for three times; recycling the ethanol from an extracting solution; adsorbing a concentrated solution with D101 macroporous adsorbent resin; washing off impurities first with water, and then performing elution with the ethanol; collecting an eluent and recycling the ethanol; and passing the concentrated solution through an alumina column. With the method, the extraction ratio of the panax notoginseng saponins can reach more than 14 percent, which is at least 2 percentage points higher than other extraction methods.

The invention discloses a method for extracting squalene from grease. The method comprises the following steps of using glycerin and lipase to perform glycerolysis on the grease; converting most of triglyceride in the grease into monoglyceride and diglyceride; utilizing a cyclodextrin inclusion technique to extract the squalene, so as to avoid the complicated operation of the one-step column chromatography or saponification extraction method, greatly reduce the usage amount of organic solvent, and avoid the defects of high cost and low efficiency in the supercritical extraction and high-efficiency counter-current chromatography. The method has the advantages that the amount of impurities is small, the squalene and residual sterol are adsorbed and separated by an alumina column, and the purpose of further purifying the squalene is realized.

The invention provides a preparation method of theophylline. The preparation method comprises the following steps: A, extracting theophylline, namely preparing a chlorine salt solution, and soaking tea leaf medicinal materials in the chlorine salt solution to extract theophylline; B, enriching theophylline, namely adsorbing extracting liquid by adopting non-polar polystyrene type macroporous adsorption resin column chromatography, after adsorbing, eluting, collecting eluting liquid, and performing reduced pressure concentration to obtain extract; C, purifying, namely performing alumina column chromatography on the extract, eluting, collecting eluting liquid, performing reduced pressure concentration, and refrigerating, crystallizing, filtering and drying concentrated liquid to obtain theophylline compounds. According to the method, a large quantity of high-quality theophylline compounds can be obtained through the four steps of extracting by the chlorine salt solution, enriching by macroporous adsorption resin, performing alumina column chromatography and crystallizing; the four steps are mild in condition and low in requirement, and the preparation cycle is short; the process is simple, the operation is simple and convenient, the requirement for the technical level of operators is low, and the industrialized popularization is facilitated.

The invention relates to a method for extracting cucurbitacin B. The method comprises the following steps of: crushing a raw material of muskmelon pedicel, and wetting the crushed muskmelon pedicel with acidic water; adding a biological enzyme for enzymolysis for 2-4 days at 30-40 DEG C; extracting zymolytic raw materials 2-3 times with 80-95% ethanol; enabling the extracting solution to flow by a short active carbon alumina column and then concentrating until the ethanol concentration is 30-50 percent; standing and crystallizing; carrying out the cold dissolution treatment with chloroform for secondary crystallization; and dissolving under the refluxing of 90-99% ethanol, decoloring with active carbon, removing impurities, recrystallizing, and the like. The method adopted for producing the cucurbitacin B has the advantages of high product yield, low cost and simple process and is easy to operate. The invention is suitable for industrial production.

The invention discloses a preparation method of refined egg oil. The preparation method comprises the steps of: supercritically extracting yolks to obtain crude egg oil; dissolving by using an organic solvent as a solvent (adding 1L of organic solvent to 1kg of crude egg oil to dissolve) and stirring; standing and precipitating, taking supernate to flow into an alumina column, adding the rest of precipitate into the alumina column, continuously eluting by using the organic solvent (eluting 1kg of alumina by using 2-6L of organic solvent), combining eluents, and concentrating to obtain egg oil; continuously adding hargil, reducing pressure and stirring at 100-150 DEG C, cooling and filtering to remove hargil to obtain the refined egg oil with low cholesterol, acid value and peroxide value. The preparation method has the characteristics of convenience for operation, low energy consumption and the like and meets the demands of industrial batch production.