41results about How to "Easy to prepare materials in batches" patented technology

The invention relates to novel process for preparing calycosin-7-O-beta-D-glucoside and ononin chemical reference products synchronously. The calycosin-7-O-beta-D-glucoside and ononin chemical reference products with a purity of over 98 percent can be obtained by purifying alcohol extract of astragalus by silica gel column chromatography, resin column impurity removal and preparation of high performance liquid chromatography. In the invention, the process steps are simple, the purity is high, the color and luster are desirable, and large-scale production is easy.

The invention relates to a preparation method for stearylglycerol in Lycium ruthenicum Murr. The method comprises the following steps: (1) impurity removal with microporous resin: a step of dissolving extract of Lycium ruthenicum Murr with an ethanol solution, separating the obtained solution by using a microporous resin column, carrying out step gradient elution and subjecting eluate to pressure-reduced drying so as to obtain a crude product of stearylglycerol; and (2) silica gel column chromatography separation: a step of subjecting the crude product of stearylglycerol to silica gel column chromatography separation, carrying out elution, collecting fraction, detecting and collecting fraction with an Rf value of 0.1 to 0.2 by using thin-layer chromatography and subjecting the collected fraction to pressure-reduced drying so as to obtain colorless oily 1-[(12E,16E)-12,16-eicosadienoyl]-2-[(E,E)-7,11-octadecadienoyl]-3-stearylglycerol with purity of greater than 95%. The preparation method is simple and has a high recovery rate; and the prepared 1-[(12E,16E)-12,16-eicosadienoyl]-2-[(E,E)-7,11-octadecadienoyl]-3-stearylglycerol has good blood fat-reducing effect.

The invention relates to a method for preparing a rosmarinic acid chemical reference substance from three types of high mountain salvias. The method comprises the following steps: (1) performing pore resin decontamination: dissolving an alcohol extract of one of salvia roborowskii, salvia przewalskii and salvia prattii with ethanol solution, filtering, separating on a pore resin column, eluting with water solution for decontaminating, then performing stepwise gradient elution with methanol solution, collecting 30% to 50% of methyl alcohol water eluate, and drying the methyl alcohol water eluate under reduced pressure to obtain a phenolic acid type component crude product; (2) performing silica gel column enrichment: performing silica gel column chromatography separation on the phenolic acid type component crude product, then eluting, and collecting a fraction with an Rf value of 0.18 to 0.22; drying the fraction under reduced pressure to obtain a faint yellow and powdery rosmarinic acid crude product; (3) performing preparative liquid chromatography purification: dissolving the rosmarinic acid crude product with methanol solution, filtering, performing preparative liquid chromatography separation, collecting a chromatography peak fraction, and drying the chromatography peak fraction under reduced pressure to obtain the white and powdery reference substance. The method is simple in process and easy for large scale.

The invention relates to a method for isolating and preparing rosmarinic acid from Dracocephalum heterophyllum, comprising the steps of (1) extracting, to be specific, soaking powder of Dracocephalum heterophyllum herb, and performing reflux extraction and vacuum concentration to obtain Dracocephalum heterophyllum extract; (2) cleaning by microporous resin, to be specific, dissolving the Dracocephalum heterophyllum extract, filtering, feeding to MCI microporous resin columns, eluting, collecting 50% ethanol solution eluent, and subjecting the 50% ethanol solution eluent to vacuum concentration to obtain rosmarinic acid crude extract; (3) isolating and purifying by hydrophilic liquid chromatography, to be specific, dissolving the rosmarinic acid crude extract, filtering with a microporous filter membrane, and isolating and purifying by using hydrophilic liquid chromatography to obtain rosmarinic acid having purity of higher than 98%. In addition, the invention also discloses application of the rosmarinic acid. The method is simple and is easy for large-scale production.

The invention relates to a method for preparing rutin and quercetin chemical reference substances simultaneously from lycium barbarum leaves. The method comprises the following steps: (1) carrying out impurity removal with microporous resin: dissolving a lycium barbarum leaf alcohol extract with a methanol solution, filtrating the solution, loading the filtrate to a microporous resin column for separation, then, carrying out stepped gradient elution sequentially with water, a 20-35% methanol solution and a 70% methanol solution, collecting 70% methanol water eluate, and enabling the methanol water eluate to be subjected to reduced-pressure drying, thereby obtaining rutin and quercetin crude products; (2) enabling the rutin and quercetin crude products to be subjected to silicagel-column chromatographic separation, eluting, and combining fractions with the Rf value of 0.3-0.5; enabling the fractions to be subjected to reduced-pressure drying, thereby obtaining brown-yellow powdered rutin and quercetin components; and (3) refining with reversed phase liquid preparative chromatography: dissolving the rutin and quercetin components with a methanol solution, filtrating the solution, separating the filtrate with an efficient reversed phase liquid preparative chromatographic column, collecting two major chromatographic peak fractions from a preparative chromatogram, and enabling the chromatographic peak fractions to be subjected to reduced-pressure drying, thereby obtaining yellow powdered rutin and quercetin reference substances. The method is simple in process and facilitates large-scale production.

The present invention relates to a pretreatment method for the nucleoside components of Armillaria chrysanthemum fruiting bodies, the method comprising the following steps: (1) Extraction: After the Armillaria chrysanthemum fruiting bodies are crushed, analytical pure water is added for extraction, after filtration, decompression Dry to paste to obtain Armillaria chrysanthemum fruiting body aqueous extract; (2) Alcohol precipitation: Add water to the aqueous extract of Armillaria chrysanthemum fruiting body to dissolve, then carry out alcohol precipitation, filter, and dry under reduced pressure to obtain a brown-yellow extract (3) Resin column chromatography enrichment: add ethanol solution to the brownish yellow extract to dissolve, and separate through resin column, carry out gradient elution with aqueous solution and ethanol solution respectively, and each eluate obtains 20% ethanol solution respectively after drying under reduced pressure The eluate, 50% ethanol solution eluate, 75% ethanol solution eluate and 95% ethanol solution eluate can obtain nucleoside target components. The invention has the advantages of simple process, easy large-scale implementation, repeatability, stable and controllable quality.

The present invention relates to a method for preparing gentiopicroside chemical reference substance from Gentiana gentipicroside, the method comprising the following steps: (1) extraction with 95% ethanol solution: drying the whole herb of gentipicroside in the shade, crushing, carrying out alcohol extraction, filtering, and drying to paste , to obtain the alcoholic extract of Gentiana japonica; (2) Resin column enrichment: dissolving the alcoholic extract of Gentiana kinkanii with methanol solution and separating it through a resin column, first eluting with aqueous solution to remove large polar impurities, and then using 30% methanol solution, Step gradient elution with 50% methanol solution, collect 50% of the eluate, and dry the 50% of the eluate under reduced pressure to obtain the crude product of Gentiana japonica; (3) Refined by reverse-phase liquid phase preparative chromatography: after the crude product of Gentiana genus twisted is dissolved in methanol solution , after filtration, reversed-phase liquid phase preparative chromatographic separation, the main chromatographic peak fraction in the preparative chromatogram was collected, and the chromatographic peak fraction was dried under reduced pressure to obtain a white powdery reference substance with a purity greater than 98%. The invention has short separation time, good separation effect and high product purity.

The invention relates to the technical field of natural medicinal chemistry, in particular to a method for separating and preparing lignan derivatives from cypress arborvitae. Its preparation method includes four steps: extraction, microporous resin enrichment, reversed-phase C18 liquid chromatography separation, and reversed-phase phenyl column liquid chromatography purification and separation. The technical means adopted in the present invention can carry out large-scale production: the raw materials are widely planted, the cost is low, and it is easy to prepare materials in batches; n-hexane room temperature percolation extraction is easy to operate; the separation adopts microporous resin rough separation, and the microporous resin separation material can be installed In the medium-pressure column chromatography system, it is easy to scale up; the reverse-phase high-pressure preparative liquid chromatography used in the separation and purification is a fast isocratic method and can ensure that the product purity is greater than 98%.

The invention relates to a pretreatment method of phenolic components in three mountainous sage plants. The method comprises the following steps: (1) extracting: drying salvia roborowskii, salvia przewalskii or salvia prattii in shade, crushing, then extracting by alcohol, filtering and drying to obtain paste, i.e. deepred extract; (2) spectral enrichment by resin column: dissolving deepred extract into methanol solution, separating by virtue of the resin column, carrying out gradient elution for the deepred extract by adopting aqueous solution and methanol solution, and collecting 40% to 50% methanol elution substance; decompressing and drying the 70% to 80% methanol elution substance, and obtaining a phenolic acid component crude product; (3) spectrally removing impurities by adopting silicone column: separating and eluting the phenolic acid component crude product by virtue of silicone column spectrum, collecting a fraction with Rf value of 0.15 to 0.25, and decompressing and drying the fraction to obtain the light yellow powdered phenolic acid component. The process is simple, the mass implementation can be realized, the repeatability is good, and the quality is stable and controllable.

The invention relates to the technical field of natural medicine chemistry, in particular to a method for separating and preparing a chemical reference substance of petracenin in saxifrage. Its preparation method includes three steps: extraction, polyamide column enrichment and microporous resin column separation. The present invention has low cost and product purity greater than 98%; the technical means adopted in the present invention can be used for large-scale production: the requirements for raw materials are not high, the cost is low, and it is easy to prepare materials in batches; the methanol is extracted by cold soaking at room temperature, and it is easy to operate; the polyamide column is used for enrichment , the separation material can be installed in a medium-pressure column system and connected to the preparative liquid chromatography, which is easy to scale; the microporous resin column used in the separation is a rapid isocratic method.

The invention relates to a new technology for large-scale preparation of a wedelolactone chemical reference substance. Through wedelolactone stability and preparation process streamlining optimization, a self-made large medium-pressure or pressure reduced silica gel column is employed for chromatography purification to obtain the wedelolactone chemical reference substance with purity greater than 98% in batches, and the scale is up to the 10g grade.

The present invention relates to a method for large-scale preparation of adenosine chemical reference substance from Armillaria chrysanthemum fruiting bodies, the method comprising the following steps: (1) Alcohol precipitation and impurity removal: the aqueous extract of Armillaria chrysanthemum fruiting bodies is dissolved in water, then alcoholic precipitation, After filtering and drying under reduced pressure, a brownish-yellow extract is obtained; (2) microporous resin column enrichment: the brownish-yellow extract is dissolved in ethanol solution, filtered, and separated on a microporous resin column, followed by step gradient elution with water and ethanol solution , collect 50% ethanol water eluate, and dry the eluate under reduced pressure to obtain crude adenosine; (3) Reverse-phase liquid phase preparation chromatography purification: the crude adenosine is dissolved in methanol solution, filtered, and prepared by high-efficiency reverse-phase liquid phase The chromatographic column is separated, and the main chromatographic peak fraction in the preparation chromatogram is collected. The chromatographic peak fraction can be dried under reduced pressure to obtain the white powder adenosine reference substance. The process of the invention is simple and easy to scale.

The invention relates to a novel process for simultaneously preparing chemical reference substances of calycosin and formononetin, comprising two steps of purifying astragalus root alcohol extracts by utilizing silicagel column chromatography and recrystallizing to obtain the two types of chemical reference substances of the calycosin and the formononetin with purities greater than 98%. The method has the advantages of simple process steps and high purity of obtained products, and is easy for scale production.