CN102824473A - Lycium ruthenicum murr total flavonoid extract and preparation method thereof - Google Patents
Lycium ruthenicum murr total flavonoid extract and preparation method thereof Download PDFInfo
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- CN102824473A CN102824473A CN2012103419554A CN201210341955A CN102824473A CN 102824473 A CN102824473 A CN 102824473A CN 2012103419554 A CN2012103419554 A CN 2012103419554A CN 201210341955 A CN201210341955 A CN 201210341955A CN 102824473 A CN102824473 A CN 102824473A
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- fructus lycii
- black fructus
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- general flavone
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Abstract
The invention belongs to the technical field of lycium ruthenicum murr total flavonoid extraction, and particularly relates to a lycium ruthenicum murr total flavonoid extract and a preparation method thereof. The lycium ruthenicum murr total flavonoid extract is prepared by the following steps of: providing one or the mixture of several of water, methanol containing water or not, ethanol, acetone, ethyl acetate, n-butyl alcohol and other liquid organic compounds as an extraction solvent, and proportioning the lycium ruthenicum murr and the extraction solvent at a weight ratio of 1:(5-30); mixing the proportioned lycium ruthenicum murr and extraction solvent; soaking, decocting or reflux-extracting, filtering and removing slag, and concentrating and recycling the organic reagent to obtain extract; and separating and purifying the extract to obtain the lycium ruthenicum murr total flavonoid extract. Through the invention, the total flavonoid compound is discovered in lycium ruthenicum murr for the first time, and the lycium ruthenicum murr total flavonoid extract with remarkable economic benefits is obtained by a scientific and reasonable extraction method.
Description
One, technical field:The invention belongs to the extractive technique field of black Fructus Lycii fruit total flavones and extract, particularly a kind of really is the black Fructus Lycii fruit total flavones that extracts of raw material and extract and preparation method thereof with black Fructus Lycii.
Two, technical background:
Black Fructus Lycii (
Lycium ruthenicum Murr.) be perennial salt tolerant, the drought-resistant plant of Solanaceae Lycium, be distributed in the NORTHWEST CHINA area, be the medicinal herbs most in use in the national medicine.Mainly acting as in tradition in (Tibetan) medicine treated heart-heat syndrome, heart disease, menoxenia, menolipsis, and hypertension also is used as strengthening by means of tonics and makes eye bright medicine among the people.The fruit of black Fructus Lycii abbreviates the black Fructus Lycii fruit as.
The report of the pharmacological properties of black Fructus Lycii fruit extractive of general flavone is less.Bai Hong advances etc. to measure the removing ability of black Fructus Lycii blade methanolic extract to DPPH free radical, hydroxy radical (OH) and ultra-oxygen anion free radical (O2-), and black Fructus Lycii blade methanolic extract is to DPPH, OH and O2
-Free radical all have scavenging action preferably (time precious traditional Chinese medical science traditional Chinese medicines, 2008,19 (2): 326-327).If discoveries such as Tao Dayong are added black Fructus Lycii fruit anthocyanin class material in the vegetable oil to, can strengthen oxidation resistance (Chinese veterinarian's medical magazine, 2007,26 (4): 15-17) of these vegetable oil.
The black Fructus Lycii fruit only is used for using as medical material at present, does not find to adopt black Fructus Lycii really to extract the relevant report of black Fructus Lycii fruit total flavones and extract technology for raw material as yet.
Three, summary of the invention:
The purpose of this invention is to provide a kind of really is that raw material extracts black Fructus Lycii fruit extractive of general flavone and method for preparing with black Fructus Lycii; Extract the black Fructus Lycii fruit extractive of general flavone that economy and medical value are arranged most in the black Fructus Lycii fruit, bring into play the economic and social benefit of black Fructus Lycii fruit widely.Extraction process of the present invention is simple, and cost is low, and extraction ratio is high, can make full use of black Fructus Lycii fruit raw material.
Technical scheme is: black Fructus Lycii fruit extractive of general flavone of the present invention is to adopt the method that is prepared as follows to prepare to come; Its preparation method is really to make raw material with black Fructus Lycii, adopts the solvent do extraction solvent of water, moisture or water-free methanol, ethanol, acetone, ethyl acetate, n-butyl alcohol or other liquid organic compound to extract.Extracting the preparation process comprises: the mixture a kind of or several kinds of water, moisture or water-free methanol, ethanol, acetone, ethyl acetate, n-butyl alcohol or other liquid organic compound make to extract solvent; With black Fructus Lycii really: the extraction solvent is that the weight ratio of 1:5-30 is carried out proportioning; Mix fruit of the black Fructus Lycii after the proportioning and extraction solvent; Through soaking, decoct or reflux, extract,, filter and remove residue, concentrating and reclaim organic reagent and get extractum, then extractum is carried out separation and purification and get black Fructus Lycii fruit extractive of general flavone again.
Isolation and purification method has three kinds; They are respectively: 1. adopt the mixture as solvent a kind of or several kinds of acetone, ethyl acetate, n-butyl alcohol or other liquid organic compound that extractum is extracted; After reclaiming organic solvent, water and the solvent of removing remnants through vacuum drying, spray drying or lyophilization again get black Fructus Lycii fruit extractive of general flavone; 2. adopt adsorbent resin that extractum is carried out column chromatography; Select the flavonoid developer to detect effluent in the upper prop process arbitrarily to confirm whether resin adsorbs saturated; Before and after respectively use for twice the ethanol volumetric concentration of water, the 0.5-5 times column volume of 1-5 times of column volume to be the ethanol water washing of 1-99%; Reuse 3-10 times of resin column volume of ethanol volumetric concentration is the ethanol water eluting of 1-99%; Concentrate, and concentrated solution carried out remaining water is removed in vacuum drying, spray drying or lyophilization and solvent gets black Fructus Lycii fruit extractive of general flavone; 3. with mineral acid the pH value of extractum is transferred to 0.1-3, under 0-42 ℃, leave standstill, sediment separate out and dry sediment are removed remaining water and are got really extractive of general flavone of black Fructus Lycii with solvent.
The method of above-mentioned separation and purification can use separately black Fructus Lycii fruit extractive of general flavone, but also combination in any is used and is made black Fructus Lycii fruit extractive of general flavone.Described flavone compound is meant that chemical constitution belongs to chemical compound and they and the monosaccharide of flavonoid, flavonols, flavanone, anthocyan, flavanol compound, two benzene pyrrones, osajin, chalcones, dihydrochalcone-type, aurones class, homoisoflavone class or the derivant that oligosaccharide forms.The quality sum of flavone compound can be the 1-100% of extract gross mass in the black Fructus Lycii fruit extractive of general flavone of said method gained; Other material is non-flavone compound; These total flavones chemical compounds; Can separate and obtain through being further purified technology, these purification process be self-explantory to one skilled in the art.
Raw material black Fructus Lycii of the present invention really is clean dry black Fructus Lycii fruit.In the organic solvent because of its soluble in water, moisture or water-free methanol of black Fructus Lycii fruit extractive of general flavone, ethanol, acetone, ethyl acetate, n-butyl alcohol or other liquid organic compound, extract so adopt above-mentioned these solvents to make to extract solvent.Mineral acid example hydrochloric acid, nitric acid, sulphuric acid, carbonic acid, silicic acid ..., and they two all can to multiple mixture.
The present invention has following advantage: 1, the present invention finds to contain in the black Fructus Lycii fruit black Fructus Lycii fruit total flavonoid chemical compound first; It adopts scientific and reasonable method for distilling to obtain to have the very black Fructus Lycii fruit extractive of general flavone with blood sugar lowering, blood fat reducing and hypotensive activity of distinct economic; Select can on the one hand the new treatment of patient that above disease is arranged, significant to deeply developing black Fructus Lycii fruit resource on the one hand; 2, to have operation few, easy and simple to handle for method for preparing provided by the invention, with short production cycle and can remove the residual heavy metal in the raw material; 3, black Fructus Lycii fruit extractive of general flavone provided by the invention has the diabetes of treating and/or preventing, hyperlipidemia and hypertensive function, and resource is efficiently made full use of, and economic and social benefit very significantly.
Four, specific embodiments:
Embodiment 1: black Fructus Lycii fruit extractive of general flavone of the present invention employing is prepared as follows method and makes; Its preparation method is to use water as the extraction solvent; With black Fructus Lycii fruit: the weight ratio of extracting aqueous solvent and be 1:5 is carried out proportioning, the fruit of the black Fructus Lycii after the proportioning with extract aqueous solvent and mix, again through soaking, decoct black Fructus Lycii fruit extractive of general flavone to the black Fructus Lycii fruit all after the extractions; Filter and remove residue, concentrated extracting solution get extractum; Adopt acetone to make solvent to extractum then extractum is extracted, behind extract recovery organic solvent, water and the solvent of removing remnants through vacuum drying get black Fructus Lycii fruit extractive of general flavone product.
Embodiment 2: black Fructus Lycii fruit extractive of general flavone of the present invention employing is prepared as follows method and makes; Its preparation method is to make to extract solvent with moisture 35% methanol; With black Fructus Lycii really: the extraction solvent is that the weight ratio of 1:10 is carried out proportioning; Mix fruit of the black Fructus Lycii after the proportioning and extraction solvent; Again through soak, black Fructus Lycii fruit extractive of general flavone in reflux, extract, to the black Fructus Lycii fruit all extracts back, filter and remove residue, concentrates the recovery solvent to extracting solution and gets extractum, then extractum employing ethyl acetate is made solvent extractum is extracted; Behind extract recovery solvent, water and the solvent of removing remnants through spray drying again get black Fructus Lycii fruit extractive of general flavone product.
Embodiment 3: black Fructus Lycii fruit extractive of general flavone of the present invention employing is prepared as follows method and makes; Its preparation method is that the use moisture content is 75% ethyl acetate do extraction solvent; With black Fructus Lycii really: the extraction solvent is that the weight ratio of 1:30 is carried out proportioning; Mix fruit of the black Fructus Lycii after the proportioning and extraction solvent; Again through soak, black Fructus Lycii fruit extractive of general flavone in reflux, extract, to the black Fructus Lycii fruit all extracts back, filter and remove residue, concentrate the recovery solvent to extracting solution gets extractum; Then extractum being adopted acetone, ethyl acetate, n-butyl alcohol respectively is that 1/3rd mixture as solvent extracts extractum, extract is reclaimed solvent after, remove remaining water again through lyophilization and get really extractive of general flavone product of black Fructus Lycii with solvent.
Embodiment 4: black Fructus Lycii fruit extractive of general flavone of the present invention is really to make raw material with black Fructus Lycii; Adopt the ethanol of moisture content 45%, the n-butyl alcohol of moisture content 15% to mix do extraction solvent with the volume ratio proportioning of 8:2; With black Fructus Lycii really: the extraction solvent is that the weight ratio of 1:20 is carried out proportioning; Fruit of the black Fructus Lycii after the proportioning and extraction solvent; Again through soak, black Fructus Lycii fruit extractive of general flavone in reflux, extract, to the black Fructus Lycii fruit extracts clean back, filter and remove residue, concentrate the recovery organic reagent to extracting solution gets extractum; Adopt adsorbent resin to carry out column chromatography to extractum then; It is saturated to confirm whether resin adsorbs to select arbitrarily the flavonoid developer to detect effluent in the upper prop process, and it is 1% ethanol water washing that front and back are respectively used the ethanol volumetric concentration of the water of 1 times of column volume, 5 times of column volumes for twice, and 3 times of resin column volume of ethanol of reuse volumetric concentration is 99% ethanol water eluting; Concentrate, and concentrated solution is carried out vacuum drying remove remaining water and get really extractive of general flavone of black Fructus Lycii with solvent.
Embodiment 5: black Fructus Lycii fruit extractive of general flavone of the present invention is that employing is prepared as follows method preparation and next; Its preparation method is really to be raw material with black Fructus Lycii; Make to extract solvent with water-free methanol, acetone with the mixture of 4:6 volume ratio proportioning; With black Fructus Lycii really: the extraction solvent is that the weight ratio of 1:10 is carried out proportioning; Fruit of the black Fructus Lycii after the proportioning and extraction solvent; Again through soak, whether the black Fructus Lycii fruit extractive of general flavone of reflux, extract, to black Fructus Lycii fruit extracts clean back, filter and remove residue, concentrate extracting solution and reclaim organic solvent and get extractum, adopts adsorbent resin to carry out column chromatography to extractum then, select flavonoid developer detection effluent to adsorb saturated with definite resin in the upper prop process arbitrarily; Before and after respectively to use the ethanol volumetric concentration of the water of 5 times of column volumes, 0.5 times of column volume for twice be 99% ethanol water washing; 10 times of resin column volume of ethanol of reuse volumetric concentration is 1% ethanol water eluting, concentrates, and concentrated solution is carried out spray drying remove remaining water and get really extractive of general flavone of black Fructus Lycii with solvent.
Embodiment 6: black Fructus Lycii fruit extractive of general flavone of the present invention employing is prepared as follows method and makes; Its preparation method is to make to extract solvent with moisture 35% methanol; With black Fructus Lycii really: the extraction solvent is that the weight ratio of 1:10 is carried out proportioning; Mix fruit of the black Fructus Lycii after the proportioning and extraction solvent; Again through soak, black Fructus Lycii fruit extractive of general flavone in reflux, extract, to the black Fructus Lycii fruit all extracts back, filter and remove residue, concentrates the recovery solvent to extracting solution and gets extractum, with the mineral acid of hydrochloric acid the pH value of extractum transferred to 0.1 then; Under 0 ℃, leave standstill, remaining water and the solvent of sediment separate out and dry sediment removal gets black Fructus Lycii fruit extractive of general flavone again.
Embodiment 7: black Fructus Lycii fruit extractive of general flavone of the present invention is really to make raw material with black Fructus Lycii; Adopt the ethanol of moisture content 45%, the n-butyl alcohol of moisture content 15% to mix do extraction solvent with the volume ratio proportioning of 8:2; With black Fructus Lycii really: the extraction solvent is that the weight ratio of 1:20 is carried out proportioning; Fruit of the black Fructus Lycii after the proportioning and extraction solvent; Again through soak, black Fructus Lycii fruit extractive of general flavone in reflux, extract, to the black Fructus Lycii fruit extracts clean back, filter and remove residue, concentrate the recovery organic reagent to extracting solution gets extractum; Then extractum is transferred to 3 with the mixing mineral acid of 1:1 volume ratio proportioning with the pH value of extractum with nitric acid and sulphuric acid, under 42 ℃, leave standstill, sediment separate out and dry sediment are removed remaining water and are got really extractive of general flavone of black Fructus Lycii with solvent.
Embodiment 8: black Fructus Lycii fruit extractive of general flavone of the present invention is that employing is prepared as follows method preparation and next; Its preparation method is really to be raw material with black Fructus Lycii; Make to extract solvent with water-free methanol, acetone with the mixture of 4:6 volume ratio proportioning; With black Fructus Lycii really: the extraction solvent is that the weight ratio of 1:10 is carried out proportioning; The black Fructus Lycii after proportioning fruit with extract solvent, again through soak, black Fructus Lycii fruit extractive of general flavone in reflux, extract, to the black Fructus Lycii fruit extract clean after, filter and remove residue, concentrate the recovery organic solvent to extracting solution and get extractum, with the mineral acid of carbonic acid the pH value of extractum is transferred to 1.3 then; Under 25 ℃, leave standstill, sediment separate out and dry sediment remove remaining water and solvent gets black Fructus Lycii fruit extractive of general flavone.
Claims (8)
1. the method for preparing of black Fructus Lycii fruit extractive of general flavone; It is characterized in that really making raw material with black Fructus Lycii; The mixture a kind of or several kinds of water, moisture or water-free methanol, ethanol, acetone, ethyl acetate, n-butyl alcohol or other liquid organic compound make to extract solvent; With black Fructus Lycii really: the extraction solvent is that the weight ratio of 1:5-30 is carried out proportioning; The black Fructus Lycii after proportioning fruit with extract solvent and mix, through soaking, decoct or reflux, extract,, filter and remove residue, concentrating and reclaim organic reagent and get extractum, then extractum is carried out separation and purification and gets black Fructus Lycii fruit extractive of general flavone again.
2. the method for preparing of black Fructus Lycii fruit extractive of general flavone according to claim 1; It is characterized in that to the method that extractum carries out separation and purification it being to adopt the mixture as solvent a kind of or several kinds of acetone, ethyl acetate, n-butyl alcohol or other liquid organic compound that extractum is extracted; After reclaiming organic solvent, water and the solvent of removing remnants through vacuum drying, spray drying or lyophilization again get black Fructus Lycii fruit extractive of general flavone.
3. the method for preparing of black Fructus Lycii fruit extractive of general flavone according to claim 1; It is characterized in that to the method that extractum carries out separation and purification it being to adopt adsorbent resin that extractum is carried out column chromatography; Select the flavonoid developer to detect effluent in the upper prop process arbitrarily to confirm whether resin adsorbs saturated; Before and after respectively use for twice the ethanol volumetric concentration of water, the 0.5-5 times column volume of 1-5 times of column volume to be the ethanol water washing of 1-99%; Reuse 3-10 times of resin column volume of ethanol volumetric concentration is the ethanol water eluting of 1-99%; Concentrate, and concentrated solution carried out remaining water is removed in vacuum drying, spray drying or lyophilization and solvent gets black Fructus Lycii fruit extractive of general flavone.
4. the method for preparing of black Fructus Lycii fruit extractive of general flavone according to claim 1; It is characterized in that to the method that extractum carries out separation and purification it being the pH value of extractum to be transferred to 0.1-3 with mineral acid; Under 0-42 ℃, leave standstill, sediment separate out and dry sediment remove remaining water and solvent gets black Fructus Lycii fruit extractive of general flavone.
5. black Fructus Lycii fruit extractive of general flavone; It is characterized in that it is by being prepared as follows the method preparation; Its preparation method is really to make raw material with black Fructus Lycii; The mixture a kind of or several kinds of water, moisture or water-free methanol, ethanol, acetone, ethyl acetate, n-butyl alcohol or other liquid organic compound are made the extraction solvent, and with black Fructus Lycii really: the extraction solvent is that the weight ratio of 1:5-30 is carried out proportioning, mixes fruit of the black Fructus Lycii after the proportioning and extraction solvent; Through soaking, decoct or reflux, extract,, filter and remove residue, concentrating and reclaim organic reagent and get extractum, then extractum is carried out separation and purification and get black Fructus Lycii fruit extractive of general flavone again.
6. black Fructus Lycii fruit extractive of general flavone according to claim 5; It is characterized in that to the method that extractum carries out separation and purification it being to adopt the mixture as solvent a kind of or several kinds of acetone, ethyl acetate, n-butyl alcohol or other liquid organic compound that extractum is extracted; After reclaiming organic solvent, water and the solvent of removing remnants through vacuum drying, spray drying or lyophilization again get black Fructus Lycii fruit extractive of general flavone.
7. black Fructus Lycii fruit extractive of general flavone according to claim 5; It is characterized in that to the method that extractum carries out separation and purification it being to adopt adsorbent resin that extractum is carried out column chromatography; Select the flavonoid developer to detect effluent in the upper prop process arbitrarily to confirm whether resin adsorbs saturated; Before and after respectively use for twice the ethanol volumetric concentration of water, the 0.5-5 times column volume of 1-5 times of column volume to be the ethanol water washing of 1-99%; Reuse 3-10 times of resin column volume of ethanol volumetric concentration is the ethanol water eluting of 1-99%, concentrates, and concentrated solution carried out remaining water is removed in vacuum drying, spray drying or lyophilization and solvent gets black Fructus Lycii fruit extractive of general flavone.
8. black Fructus Lycii fruit extractive of general flavone according to claim 5; It is characterized in that to the method that extractum carries out separation and purification it being the pH value of extractum to be transferred to 0.1-3 with mineral acid; Under 0-42 ℃, leave standstill, sediment separate out and dry sediment remove remaining water and solvent gets black Fructus Lycii fruit extractive of general flavone.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103583760A (en) * | 2013-10-26 | 2014-02-19 | 张海凤 | Production formula of Lycium ruthenicum Murr coffee, and production technology of Lycium ruthenicum Murr coffee |
| CN108434248A (en) * | 2018-05-24 | 2018-08-24 | 湖南师范大学 | A kind of extracting method and purposes of matrimony vine active ingredient |
| CN111920722A (en) * | 2020-09-08 | 2020-11-13 | 邓守毅 | Production process of wolfberry facial mask |
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| CN1686421A (en) * | 2005-04-26 | 2005-10-26 | 陶燕铎 | Black fruit lycium plant fruit extract, its preparation method and application |
| CN101991709A (en) * | 2010-11-09 | 2011-03-30 | 中国科学院西北高原生物研究所 | Method for preparing antioxidant lycium ruthenicum extract |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1686421A (en) * | 2005-04-26 | 2005-10-26 | 陶燕铎 | Black fruit lycium plant fruit extract, its preparation method and application |
| CN101991709A (en) * | 2010-11-09 | 2011-03-30 | 中国科学院西北高原生物研究所 | Method for preparing antioxidant lycium ruthenicum extract |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103583760A (en) * | 2013-10-26 | 2014-02-19 | 张海凤 | Production formula of Lycium ruthenicum Murr coffee, and production technology of Lycium ruthenicum Murr coffee |
| CN108434248A (en) * | 2018-05-24 | 2018-08-24 | 湖南师范大学 | A kind of extracting method and purposes of matrimony vine active ingredient |
| CN108434248B (en) * | 2018-05-24 | 2021-02-02 | 湖南师范大学 | Extraction method and application of active ingredients of medlar |
| CN111920722A (en) * | 2020-09-08 | 2020-11-13 | 邓守毅 | Production process of wolfberry facial mask |
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Application publication date: 20121219 |