CN103145783A - Method of extracting isoquercitrin, senecio cannabifolius less glycoside and senecio cannabifolius less polysaccharide from senecio cannabifolius less - Google Patents
Method of extracting isoquercitrin, senecio cannabifolius less glycoside and senecio cannabifolius less polysaccharide from senecio cannabifolius less Download PDFInfo
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- CN103145783A CN103145783A CN2013100993537A CN201310099353A CN103145783A CN 103145783 A CN103145783 A CN 103145783A CN 2013100993537 A CN2013100993537 A CN 2013100993537A CN 201310099353 A CN201310099353 A CN 201310099353A CN 103145783 A CN103145783 A CN 103145783A
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- herba senecionis
- isoquercitrin
- senecionis cannabifolii
- senecio cannabifolius
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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Abstract
The invention relates to a method of extracting isoquercitrin, senecio cannabifolius less glycoside and senecio cannabifolius less polysaccharide from senecio cannabifolius less, wherein the isoquercitrin has the effects of stopping bleeding and reducing blood pressure, resisting inflammation and killing virus; the senecio cannabifolius less glycoside has the effects of relieving a cough and diminishing inflammation, and resisting tumors and lung cancer; and senecio cannabifolius less polysaccharide has the effect of enhancing the immunity. The conventional senecio cannabifolius less extract production technique still has more limits and deficiencies, different substances in the extracting product can not be effectively separated, and only one product is obtained. Three effective products can be obtained by adopting methods of supercritical CO2 extraction, normal-temperature ethanol digestion, macroporous resin adsorption and the like through one production technique. The method is simple in flow process and convenient to operate, hardly causes environment pollution, the content of active ingredients in the products is high, so that the method is a production technique for industrial production.
Description
Technical field
The present invention relates to a kind of Traditional Chinese medicine extraction method, particularly the extracting method of isoquercitrin, Herba Senecionis cannabifolii glucoside, Herba Senecionis cannabifolii polysaccharide in a kind of Chinese medicine Herba Senecionis cannabifolii.
Background technology
Herba Senecionis cannabifolii is composite family Senecio per nnial herb, mainly is distributed in the Changbaishan area in Jilin Province.This plant all herbal medicine, it is warm in nature, and flavor is hot, bitter, and moistening lung to lower QI has that heat-clearing is eliminated the phlegm, the effect of cough-relieving.The Herba Senecionis cannabifolii main active ingredient is isoquercitrin, Herba Senecionis cannabifolii glucoside, Herba Senecionis cannabifolii polysaccharide, and wherein isoquercitrin has the effect of hemostasis step-down, anti-inflammatory virus killing; The Herba Senecionis cannabifolii glucoside has the effect of relieving cough and diminishing inflammation, antitumor, anti-lung cancer; The Herba Senecionis cannabifolii polysaccharide has the effect of strengthening immunity.
Still there are many limitations and deficiency in conventional Herba Senecionis cannabifolii extract production technique, heterogeneity in the extraction product is not effectively separated, products therefrom only has a kind of, it is the general Herba Senecionis cannabifolii extract that obtained, products therefrom effective constituent can not be kept to greatest extent, and invalid components can not be removed to greatest extent, has directly affected quality product and clinical efficacy.
Summary of the invention
The object of the invention is to overcome the weak point of existing technique, provides a kind of flow process simple, easy to operate, low in the pollution of the environment, and in product, active constituent content is high, is fit to the production technique that industrialization is extracted.
The technical solution used in the present invention is: the hempleaf groundsel herb rhizome is pulverized oven dry → supercritical carbon dioxide extracting → microwave vacuum cryogenic temperature freezing drying and is processed → obtain waste residue → concentrated extracting solution → polar macroporous resin chromatography → wash-out → concentrate eluant → microwave ultravacuum frozen drying after isoquercitrin → alcohol at normal temperature lixiviate supercritical carbon dioxide extracting and process → obtain extract → decolouring that hempleaf groundsel herb glucoside → polar macroporous resin adsorption crosses → filtration → deproteinized → microwave vacuum cryogenic temperature freezing drying processing → hempleaf groundsel herb polysaccharide.
The present invention comprises the following steps with the method that Herba Senecionis cannabifolii extracts isoquercitrin, Herba Senecionis cannabifolii glucoside, Herba Senecionis cannabifolii polysaccharide:
The Herba Senecionis cannabifolii rhizome is pulverized and is dried the order to granularity 60-100, and bake out temperature is 55-65 ℃, dries 6-10 hour; Drop in extraction kettle after oven dry, extraction conditions is: supercritical carbon dioxide extraction pressure 34-40MPa, and temperature is 30-38 ℃; Separation condition is: flash trapping stage still pressure is 13-17MPa, and temperature is 30-40 ℃, and the second-order separation still pressure is 4MPa, and temperature is 30-40 ℃; 40-70% ethanol is done entrainment agent; After dynamic operation 4-8 hour, reclaim entrainment agent from flash trapping stage still, the second-order separation still, obtain solid-state isoquercitrin extract, the microwave vacuum cryogenic temperature freezing drying obtains isoquercitrin, and wherein the relative content of isoquercitrin can reach 30-80%.
Take out the waste residue in overcritical still, with 6-10 times of volume, the lixiviate of 30-60% alcohol at normal temperature, circulation 3-5 time, united extraction liquid, cross polar macroporous resin column and adsorb, the extracting solution that adsorbed is preserved and is continued to employ.With the mixed solution of ethanol and methylene dichloride as the polar macroporous resin of elutriant wash-out, wherein the volume ratio of ethanol and methylene dichloride is: ethanol/dichloromethane=1/1 ~ 1/2, elution flow rate per hour is 1-3 times of column volume, concentrate eluant, adopt microwave vacuum cryogenic temperature freezing drying method to obtain the Herba Senecionis cannabifolii glucoside, wherein the Herba Senecionis cannabifolii salidroside content can reach 30-80%.
With the extracting solution of above-mentioned preservation non-polar macroporous resin adsorption bleaching, filter.Filtrate is concentrated to 1/10 ~ 1/15 of original volume, and Deproteinization obtains the Herba Senecionis cannabifolii polysaccharide with the method for microwave vacuum cryogenic temperature freezing drying, and wherein the Herba Senecionis cannabifolii polysaccharide content can reach 40-80%.
The advantage of extraction process of the present invention is:
1, the technological process of production of the present invention is simple, and is easy to operate, low in the pollution of the environment, is fit to suitability for industrialized production.
2, adopt the method for microwave vacuum cryogenic temperature freezing drying, make the product structure composition not have in drying course destroyed, preserved to greatest extent the property of medicine effect of product, and time of drying is short, speed is fast.
3, product yield of the present invention is high, and purity is high, and the relative content that obtains the isoquercitrin in Herba Senecionis cannabifolii rhizome powder by extraction process of the present invention can reach 30-80%; Herba Senecionis cannabifolii glucoside relative content can reach 30-80%; Herba Senecionis cannabifolii polysaccharide relative content can reach 40-80%.
4, the present invention produces isoquercitrin, Herba Senecionis cannabifolii glucoside, Herba Senecionis cannabifolii polysaccharide with Herba Senecionis cannabifolii, and production efficiency is high, by a production technique, obtains three kinds of products, has realized taking full advantage of of Herba Senecionis cannabifolii resource.
Embodiment
The present invention is further described below in conjunction with specific embodiment
Embodiment 1:
The Herba Senecionis cannabifolii rhizome is pulverized and is dried to granularity 100 orders, takes 200 grams, and bake out temperature is 55 ℃, dries 10 hours.Drop in extraction kettle after oven dry, extraction conditions is: supercritical carbon dioxide extraction pressure 35MPa, and temperature is 38 ℃; Separation condition is: flash trapping stage still pressure is 13MPa, and temperature is 35 ℃, and the second-order separation still pressure is 4MPa, and temperature is 35 ℃; 50% ethanol is done entrainment agent; After dynamic operation 4 hours, reclaim entrainment agent from flash trapping stage still, the second-order separation still, obtain solid-state isoquercitrin extract, the microwave vacuum cryogenic temperature freezing drying obtains isoquercitrin, and wherein the isoquercitrin relative content is 76.64%.
Take out the waste residue in overcritical still, with 8 times of volumes, 50% alcohol at normal temperature lixiviate, circulate 5 times, united extraction liquid is crossed polar macroporous resin column and is adsorbed, and the extracting solution that adsorbed is preserved and continued to employ.With the mixed solution of ethanol and methylene dichloride as the polar macroporous resin of elutriant wash-out, wherein the volume ratio of ethanol and methylene dichloride is: ethanol/dichloromethane=1/2, elution flow rate per hour is 1 times of column volume, concentrate eluant, adopt microwave vacuum cryogenic temperature freezing drying method to obtain the Herba Senecionis cannabifolii glucoside, wherein the relative content of Herba Senecionis cannabifolii glucoside is 78.81%.
With the extracting solution of above-mentioned preservation non-polar macroporous resin adsorption bleaching, filter.Filtrate is concentrated to 1/15 of original volume, and Deproteinization obtains the Herba Senecionis cannabifolii polysaccharide with the method for microwave vacuum cryogenic temperature freezing drying, and wherein the relative content of Herba Senecionis cannabifolii polysaccharide is 60.87%.
Embodiment 2:
The Herba Senecionis cannabifolii rhizome is pulverized and is dried to granularity 80 orders, takes 200 grams, and bake out temperature is 50 ℃, dries 8 hours.Drop in extraction kettle after oven dry, extraction conditions is: supercritical carbon dioxide extraction pressure 40MPa, and temperature is 35 ℃; Separation condition is: flash trapping stage still pressure is 17MPa, and temperature is 40 ℃, and the second-order separation still pressure is 4MPa, and temperature is 40 ℃; 70% ethanol is done entrainment agent; After dynamic operation 8 hours, reclaim entrainment agent from flash trapping stage still, the second-order separation still, obtain solid-state isoquercitrin extract, the microwave vacuum cryogenic temperature freezing drying obtains isoquercitrin, and wherein the relative content of isoquercitrin is 67.34%.
Take out the waste residue in overcritical still, with 10 times of volumes, 40% alcohol at normal temperature lixiviate, circulate 3 times, united extraction liquid is crossed polar macroporous resin column and is adsorbed, and the extracting solution that adsorbed is preserved and continued to employ.With the mixed solution of ethanol and methylene dichloride as the polar macroporous resin of elutriant wash-out, wherein the volume ratio of ethanol and methylene dichloride is: ethanol/dichloromethane=1/1, elution flow rate per hour is 3 times of column volumes, concentrate eluant, adopt microwave vacuum cryogenic temperature freezing drying method to obtain the Herba Senecionis cannabifolii glucoside, wherein the relative content of Herba Senecionis cannabifolii glucoside is 61.44%.
With the extracting solution of above-mentioned preservation non-polar macroporous resin adsorption bleaching, filter.Filtrate is concentrated to 1/10 of original volume, and Deproteinization obtains the Herba Senecionis cannabifolii polysaccharide with the method for microwave vacuum cryogenic temperature freezing drying, and wherein the relative content of Herba Senecionis cannabifolii polysaccharide is 67.17%.
Claims (1)
1. extract the method for isoquercitrin, Herba Senecionis cannabifolii glucoside, Herba Senecionis cannabifolii polysaccharide with Herba Senecionis cannabifolii, it is characterized in that comprising the following steps:
The Herba Senecionis cannabifolii rhizome is pulverized and is dried the order to granularity 60-100, and bake out temperature is 55-65 ℃, dries 6-10 hour; Drop in extraction kettle after oven dry, extraction conditions is: supercritical carbon dioxide extraction pressure 34-40MPa, and temperature is 30-38 ℃; Separation condition is: flash trapping stage still pressure is 13-17MPa, and temperature is 30-40 ℃, and the second-order separation still pressure is 4MPa, and temperature is 30-40 ℃; 40-70% ethanol is done entrainment agent; After dynamic operation 4-8 hour, reclaim entrainment agent from flash trapping stage still, the second-order separation still, obtain solid-state isoquercitrin extract, the microwave vacuum cryogenic temperature freezing drying obtains isoquercitrin;
Take out the waste residue in overcritical still, with 6-10 times of volume, the lixiviate of 30-60% alcohol at normal temperature, circulation 3-5 time, united extraction liquid, cross polar macroporous resin column and adsorb, the extracting solution that adsorbed is preserved and is continued to employ; With the mixed solution of ethanol and methylene dichloride as the polar macroporous resin of elutriant wash-out, wherein the volume ratio of ethanol and methylene dichloride is: ethanol/dichloromethane=1/1 ~ 1/2, elution flow rate per hour is 1-3 times of column volume, concentrate eluant, and the microwave vacuum cryogenic temperature freezing drying obtains the Herba Senecionis cannabifolii glucoside;
With the extracting solution of above-mentioned preservation non-polar macroporous resin adsorption bleaching, filter; Filtrate is concentrated to 1/10 ~ 1/15 of original volume, Deproteinization, and the microwave vacuum cryogenic temperature freezing drying obtains the Herba Senecionis cannabifolii polysaccharide.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107556354A (en) * | 2017-10-31 | 2018-01-09 | 桂林纽泰生物科技有限公司 | The method that isoquercitrin is extracted from beggar-ticks |
| CN108635391A (en) * | 2018-06-20 | 2018-10-12 | 吉林益民堂制药有限公司 | A kind of hempleaf groundsel herb phenolic acid components and the preparation method and application thereof |
| CN108752498A (en) * | 2018-06-20 | 2018-11-06 | 吉林益民堂制药有限公司 | One kind having the immunocompetent grass polysaccharide and the preparation method and application thereof of returning from the grave of enhancing |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107556354A (en) * | 2017-10-31 | 2018-01-09 | 桂林纽泰生物科技有限公司 | The method that isoquercitrin is extracted from beggar-ticks |
| CN108635391A (en) * | 2018-06-20 | 2018-10-12 | 吉林益民堂制药有限公司 | A kind of hempleaf groundsel herb phenolic acid components and the preparation method and application thereof |
| CN108752498A (en) * | 2018-06-20 | 2018-11-06 | 吉林益民堂制药有限公司 | One kind having the immunocompetent grass polysaccharide and the preparation method and application thereof of returning from the grave of enhancing |
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Application publication date: 20130612 |