CN102836280A - Folium Lycii total flavone extract and preparation method thereof - Google Patents
Folium Lycii total flavone extract and preparation method thereof Download PDFInfo
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- CN102836280A CN102836280A CN2012103419520A CN201210341952A CN102836280A CN 102836280 A CN102836280 A CN 102836280A CN 2012103419520 A CN2012103419520 A CN 2012103419520A CN 201210341952 A CN201210341952 A CN 201210341952A CN 102836280 A CN102836280 A CN 102836280A
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Abstract
The invention belongs to the field of folium lycii total flavone extraction technology, particularly relates to a folium lycii total flavone extract and a preparation method thereof. The preparation method includes mixing folium lycii or folium lycii powder with extraction solvent (one or more of water, aqueous or anhydrous methanol, ethanol, acetone, ethyl acetate, n-butanol or other liquid organic compound) at weight ratio of 1:(5-30); soaking; decocting or reflux-extracting; filtering to remove residue; concentrating and recovering organic reagent to obtain extractum; and performing separation and purification on the extractum to obtain the folium Lycii total flavone extract. According to the invention, the preparation method is scientific and reasonable, and the folium lycii total flavone extract with significant economic benefits is obtained.
Description
One, technical field:The invention belongs to Folium Lycii total flavones extractive technique field, particularly a kind of is Folium Lycii extractive of general flavone of extracting of raw material and preparation method thereof with the Folium Lycii.
Two, technical background:Fructus Lycii (
Lycium chinense.) be the perennial plant of Solanaceae Lycium, be distributed in the NORTHWEST CHINA area.Folium Lycii is commonly called as day smart grass, in tradition, mainly has kidney-tonifying sperm-generating, nourishing the liver in (Tibetans) medicine, an effect such as calm the nerves that makes eye bright, and claims the effect of Folium Lycii " have relieving restlessness benefit will to mend five kinds of strain and seven kinds of impairment, high aspiration gas removes pyretic toxicity, and the skin ulcer of loosing is swollen, except that wind makes eye bright " in the Compendium of Material Medica.According to research, the active component of Folium Lycii and Chinese wolfberry fruit basically identical, and on some nutrient even above Chinese wolfberry fruit.
The report of the pharmacological properties of Folium Lycii extractive of general flavone is less.The pharmacologically active of the Folium Lycii extractive of general flavone of finding now only rests on the level of antioxidant activity.Zou Yaohong etc. have isolated 5 kinds of flavone compounds in the Folium Lycii, are respectively 5,7; 3 '-trihydroxy-6,4 ', 5 '-trimethoxy flavone, acacetin (4 '-methoxyl group-5; The 7-dihydroxyflavone), acacetin-7-O-α-L-rhamanopyranosyl (1 → 6)-β-D-glucoside, luteolin (5,7,3 '; 4 '-kaempferol) and rutin, luteolin antioxidative activity is stronger in these 5 kinds of flavone compounds, is superior to a synthetic type antioxidant 3; 5-di-t-butyl-4-hydroxymethyl benzene (analytical test journal, 2002,21 (1): 76-78).Folium Lycii only is used for the Fructus Lycii tea use at present, and finding to adopt Folium Lycii as yet is the relevant report that raw material extracts Folium Lycii total flavones technology.
Three, summary of the invention:
The purpose of this invention is to provide a kind of is that raw material extracts Folium Lycii extractive of general flavone and method for preparing with the Folium Lycii; Extract the Folium Lycii extractive of general flavone that economy and medical value are arranged most in the Folium Lycii; Folium Lycii that the past is ignored by people even that abandon is turned waste into wealth, bring into play the economic and social benefit of Folium Lycii widely.
Technical scheme is: Folium Lycii 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 to make raw material with Folium Lycii, adopts water, moisture or water-free methanol, ethanol, acetone, ethyl acetate, n-butyl alcohol or other liquid organic compound to make to extract solvent and extracts.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 Folium Lycii or its powder: the weight ratio of extracting solvent and be 1:5-30 is carried out proportioning; Mix the Folium Lycii after the proportioning or its powder with the 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 the Folium Lycii extractive of general flavone again.
Isolation and purification method has three kinds; They are respectively: 1. adopt other the mixture as solvent a kind of or several kinds of liquid organic compound of acetone, ethyl acetate, n-butyl alcohol or its that extractum is extracted; After reclaiming organic solvent, remove remaining water and solvent again through vacuum drying, spray drying or lyophilization and get the Folium Lycii 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 is carried out vacuum drying, spray drying or lyophilization remove remaining water and solvent and get the Folium Lycii 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 solvent and are got the Folium Lycii extractive of general flavone.
The method of above-mentioned separation and purification can use separately the Folium Lycii extractive of general flavone, but also combination in any use the Folium Lycii extractive of general flavone.The quality sum of flavone compound can be the 1-100% of extract gross mass in the Folium Lycii 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 Folium Lycii of the present invention or its powder are clean dried wolfberry leaves, or clean dried wolfberry leaf powder after crushed, are referred to as Folium Lycii or its powder.In the organic solvent because of its soluble in water, moisture or water-free methanol of Folium Lycii 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 Folium Lycii total flavonoid chemical compound first; It adopts scientific and reasonable method for distilling to obtain to have the very Folium Lycii 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 the Folium Lycii 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, Folium Lycii 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: Folium Lycii extractive of general flavone employing of the present invention is prepared as follows method and makes; Its preparation method is to use water as the extraction solvent; With Folium Lycii: the weight ratio of extracting aqueous solvent and be 1:5 is carried out proportioning, the Folium Lycii after the proportioning with extract aqueous solvent and mix, again through soaking, decoct Folium Lycii extractive of general flavone to the Folium Lycii all after the extractions; Filter and remove residue, concentrated extracting solution get extractum, then to extractum
Adopt acetone to make solvent extractum is extracted, behind extract recovery organic solvent, remove remaining water and solvent through vacuum drying and get Folium Lycii extractive of general flavone product.
Embodiment 2: Folium Lycii extractive of general flavone employing of the present invention is prepared as follows method and makes; Its preparation method is to make to extract solvent with moisture 35% methanol; With Folium Lycii: the weight ratio of extracting solvent and be 1:10 is carried out proportioning, the Folium Lycii after the proportioning with extract solvent and mix, after the Folium Lycii extractive of general flavone in immersion, reflux, extract, to Folium Lycii all extracts again, filter and remove residue; Concentrate the recovery solvent to extracting solution and get extractum; Adopt ethyl acetate to make solvent to extractum then extractum is extracted, behind extract recovery solvent, remove remaining water and solvent again through spray drying and get Folium Lycii extractive of general flavone product.
Embodiment 3: Folium Lycii extractive of general flavone employing of the present invention is prepared as follows method and makes; Its preparation method is that the use moisture content is 75% ethyl acetate do extraction solvent; With the Folium Lycii powder: the weight ratio of extracting solvent and be 1:30 is carried out proportioning; Mix Folium Lycii powder after the proportioning and extraction solvent; Again through soak, Folium Lycii extractive of general flavone in reflux, extract, to the Folium Lycii powder 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 and solvent again through lyophilization and get Folium Lycii extractive of general flavone product.
Embodiment 4: Folium Lycii extractive of general flavone of the present invention is to make raw material with the Folium Lycii powder; 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 the Folium Lycii powder: the weight ratio of extracting solvent and be 1:20 is carried out proportioning; Folium Lycii powder after the proportioning and extraction solvent; Again through soak, Folium Lycii extractive of general flavone in reflux, extract, to the Folium Lycii powder 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 solvent and get the Folium Lycii extractive of general flavone.
Embodiment 5: Folium Lycii extractive of general flavone of the present invention is that employing is prepared as follows method preparation and next; Its preparation method is that the mixture with Folium Lycii and Folium Lycii powder is a raw material; Make to extract solvent with water-free methanol, acetone with the mixture of 4:6 volume ratio proportioning; With Folium Lycii and Folium Lycii powder: the weight ratio of extracting solvent and be 1:10 is carried out proportioning; The Folium Lycii after the proportioning and Folium Lycii powder and extraction solvent; Again through soak, whether Folium Lycii extractive of general flavone in reflux, extract, to the Folium Lycii powder 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 solvent and get the Folium Lycii extractive of general flavone.
Embodiment 6: Folium Lycii extractive of general flavone employing of the present invention is prepared as follows method and makes; Its preparation method is to make to extract solvent with moisture 35% methanol; With Folium Lycii: the weight ratio of extracting solvent and be 1:10 is carried out proportioning, the Folium Lycii after the proportioning with extract solvent and mix, after the Folium Lycii extractive of general flavone in immersion, reflux, extract, to Folium Lycii all extracts again, filter and remove residue; Concentrate the recovery solvent to extracting solution and get extractum; With the mineral acid of hydrochloric acid the pH value of extractum is transferred to 0.1 then, under 0 ℃, leave standstill, sediment separate out and dry sediment are removed remaining water and solvent and are got the Folium Lycii extractive of general flavone again.
Embodiment 7: Folium Lycii extractive of general flavone of the present invention is to make raw material with the Folium Lycii powder; 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 the Folium Lycii powder: the weight ratio of extracting solvent and be 1:20 is carried out proportioning; Folium Lycii powder after the proportioning and extraction solvent; Again through soak, Folium Lycii extractive of general flavone in reflux, extract, to the Folium Lycii powder 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 solvent and are got the Folium Lycii extractive of general flavone.
Embodiment 8: Folium Lycii extractive of general flavone of the present invention is that employing is prepared as follows method preparation and next; Its preparation method is that the mixture with Folium Lycii and Folium Lycii powder is a raw material; Make to extract solvent with water-free methanol, acetone with the mixture of 4:6 volume ratio proportioning; With Folium Lycii and Folium Lycii powder: the weight ratio of extracting solvent and be 1:10 is carried out proportioning; The Folium Lycii after the proportioning and Folium Lycii powder with extract solvent, again through soak, Folium Lycii extractive of general flavone in reflux, extract, to the Folium Lycii powder 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 are removed remaining water and solvent and are got the Folium Lycii extractive of general flavone.
Claims (8)
1. the method for preparing of a Folium Lycii extractive of general flavone; It is characterized in that making raw material with Folium 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 Folium Lycii or its powder: the weight ratio of extracting solvent and be 1:5-30 is carried out proportioning; The Folium Lycii after the proportioning or its powder 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 the Folium Lycii extractive of general flavone again.
2. the method for preparing of Folium Lycii 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, remove remaining water and solvent again through vacuum drying, spray drying or lyophilization and get the Folium Lycii extractive of general flavone.
3. the method for preparing of Folium Lycii 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 is carried out vacuum drying, spray drying or lyophilization remove remaining water and solvent and get the Folium Lycii extractive of general flavone.
4. the method for preparing of Folium Lycii 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 are removed remaining water and solvent and are got the Folium Lycii extractive of general flavone.
5. Folium Lycii extractive of general flavone; It is characterized in that it is by being prepared as follows the method preparation; Its preparation method is to make raw material with Folium Lycii; The mixture of water, moisture or water-free methanol, ethanol, acetone, ethyl acetate, n-butyl alcohol or other liquid organic compound a kind of or several kinds make to extract solvent, and with Folium Lycii or its powder: the weight ratio of extracting solvent and be 1:5-30 is carried out proportioning, the Folium Lycii after the proportioning or its powder 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 get the Folium Lycii extractive of general flavone again.
6. Folium Lycii 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, remove remaining water and solvent again through vacuum drying, spray drying or lyophilization and get the Folium Lycii extractive of general flavone.
7. Folium Lycii 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 vacuum drying, spray drying or lyophilization remove remaining water and solvent and get the Folium Lycii extractive of general flavone.
8. Folium Lycii 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 are removed remaining water and solvent and are got the Folium Lycii extractive of general flavone.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105998358A (en) * | 2016-05-16 | 2016-10-12 | 南京农业大学 | Preparation method of lycium barbarum leaf polyphenol with antioxidant activity and alpha-glucosidase inhibitory activity |
| CN108159187A (en) * | 2018-01-22 | 2018-06-15 | 周学义 | A kind of method that flavones is extracted from wolfberry leaf |
| NL2028620B1 (en) * | 2021-07-02 | 2022-06-16 | Wolfberry Science Inst Ningxia Academy Of Agriculture And Forestry Sciences | Method for extracting total flavonoids from lycium chinese leaves |
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| CN102000208A (en) * | 2010-11-09 | 2011-04-06 | 中国科学院西北高原生物研究所 | Method for extracting and preparing medlar leaf flavone |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105998358A (en) * | 2016-05-16 | 2016-10-12 | 南京农业大学 | Preparation method of lycium barbarum leaf polyphenol with antioxidant activity and alpha-glucosidase inhibitory activity |
| CN108159187A (en) * | 2018-01-22 | 2018-06-15 | 周学义 | A kind of method that flavones is extracted from wolfberry leaf |
| NL2028620B1 (en) * | 2021-07-02 | 2022-06-16 | Wolfberry Science Inst Ningxia Academy Of Agriculture And Forestry Sciences | Method for extracting total flavonoids from lycium chinese leaves |
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Application publication date: 20121226 |