CN101862371A - Method for preparing flavone and alkaloid from mulberry leaves - Google Patents
Method for preparing flavone and alkaloid from mulberry leaves Download PDFInfo
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- CN101862371A CN101862371A CN201010130263A CN201010130263A CN101862371A CN 101862371 A CN101862371 A CN 101862371A CN 201010130263 A CN201010130263 A CN 201010130263A CN 201010130263 A CN201010130263 A CN 201010130263A CN 101862371 A CN101862371 A CN 101862371A
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- folium mori
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Abstract
The invention relates to a method for preparing flavone and alkaloid from mulberry leaves. The processing steps are as follows: alkaline water is heated to extract the flavone, 90 to 95 percent of ethanol and active carbon are then used for extracting the alkaloid, the flavone extract passes through a macroporous resin column after the pH of the flavone extract is regulated, acidification is carried out for crystallization, 70 to 80 percent of ethanol is used for dissolution and recrystallization, the alkaloid extract is concentrated and dissolved in acetone, and passes through a short wide alumina column, ammonification is carried out for crystallization, and 85 to 90 percent of ethanol is used for dissolution and recrystallization. When the method is adopted to produce flavone and alkaloid from mulberry leaves, the technique is simple and can be easily industrialized, the utilization rate of material is high, and the purity of the obtain products is high, and accords with the requirement of food and medicines.
Description
Technical field:
The present invention relates to a kind of flavone, the alkaloidal method of from Folium Mori, preparing, particularly a kind of employing potass extraction flavone and the alkaloidal technology of ethanol extraction.
Background technology:
China plants Sang Yangcan country the earliest in the world, also is that the Chinese nation one of contributes the greatness of human civilization.The history in existing more than 7,000 year of the cultivation of mulberry.Cultivate in extensive rangely, northeast is on the south Harbin; The northwest is from south, the Inner Mongol to Xinjiang, Qinghai; Reach Guangdong and Guangxi Provinces in the south, to the east of Taiwan; To Sichuan, Yunnan; The cultivation of various places, the middle and lower reach of Yangtze River at most.
Folium Mori are the leaf of Moraceae (Moraceae) Morus plant Mulberry (Morns dba L.), and bitter in the mouth, sweet is cold in nature, returns lung, Liver Channel, have that dispelling wind and heat pathogens, clearing away lung-heat and moistening for dryness, suppressing the hyperactive liver make eye bright, the effect of cooling blood for hemostasis.The Compendium of Material Medica record: Folium Mori are hands, the bright medicine of foot sun, control the consumptive fever cough, and the long hair that makes eye bright is only quenched one's thirst.
Folium Mori contain inokosterone, ecdysterone, β-Bao sterol, globulariacitrin, Mulberry glycoside, Isoquercitrin, umbelliferone, scopolin, trigonelline (trigonelline, choline etc.Flavones ingredient content is abundant in the Folium Mori, content account for cured leaf heavy 1.0%～3.0%, be higher a kind of of flavonoid content in the plant stem-leaf.Flavone compound has caused the extensive attention of Chinese scholars because of its physiologically active is varied, and progress is very fast.It has good free radical, antioxidation, defying age, blood fat reducing, immunomodulating, physiologically active such as antibiotic, has broad application prospects.Folium Mori alkaloid has hypoglycemic activity.
Mostly existing extraction flavones in mulberry leaves and alkaloid are that ethanol extraction or decocting boil, again through macroporous resin adsorption, extraction or ion column.As patent 200810236144 " a kind of coproduction of mulberry tea flavone, polysaccharide and alkaloid ", disclosed method adopts water heating lixiviate, macroporous resin adsorption.Also have patent 03101988 " a kind of method that contains its preparation of preparation of Folium Mori total alkali extractum " disclosed method to adopt hot water dissolving, ion-exchange resin purification.Ethanol and hot water extraction, two kinds of compositions of stripping simultaneously, separation and purification is difficult.
Summary of the invention:
The objective of the invention is in order to overcome with above-mentioned existing defective workmanship and deficiency, the inventor is according to flavones in mulberry leaves and alkaloidal nature difference, repetition test, and the spy provides a kind of flavone, alkaloidal method of preparing from Folium Mori.
The object of the present invention is achieved like this:
A kind of flavone, alkaloidal method of preparing from Folium Mori is characterized in that comprising following step:
1) Folium Mori are pulverized, doubly measured 30-50 ℃ of dynamic extraction 1-3 of ph9-12 aqueous alkali hour with 6-10, extracts 2-3 time, merging aqueous extract, medicinal residues add 4-6 again and doubly measure 85-95% ethanol and active carbon reflux, extract, 2-3 time, the merging alcohol extract;
2) the step 1) aqueous extract is transferred ph5-7 add macroporous resin column absorption, water-pure eluting is collected the flavones in mulberry leaves flow point, and behind the adding active carbon reflux decolour, concentrating under reduced pressure ph1-3 leaves standstill crystallization;
3) leach the dissolving of coarse crystallization thing alkali alcohol and transfer the ph2-4 crystallization, it is dissolving crystallized to leach reuse 70-80% alcohol reflux, leaches crystal and is drying to obtain Folium Mori total flavonoids;
4) the step 1) alcohol extract is transferred to neutrality, reclaim ethanol, add acetone solution and filter to paste, add the aluminium oxide short wide column, collect lower column liquid and reclaim acetone, add the ammonia crystallization, it is dissolving crystallized to leach crystallization reuse 85-90% alcohol reflux, is drying to obtain the Folium Mori biology total alkali.
Optional sodium hydroxide of alkali in the step 1) or calcium hydroxide.Preferably calcium hydroxide.
Step 2), optional hydrochloric acid, sulphuric acid or the phosphoric acid of the accent ph 3), 4) a kind of.
Step 2) optional D101 of macroporous resin or SPD100 in, water-pure eluting is for washing neutrality 5-6BV50-70% ethanol elution flavones in mulberry leaves again.
Step 1), 2) active carbon is an injection class medicinal activity charcoal in, and the 1-3% of addition liquid, bleaching time are 1-2 hour.
Alkali alcohol in the step 3) is the 90-95% ethanol sodium hydroxide solution of ph9-12.
Aluminium oxide in the step 4) is a 120-200 order neutral alumina.
In sum, there is following advantage in the present invention: aqueous alkali extract at low temperature, the easy stripping of flavone and alkaloid does not have stripping; Extract alkaloid after the alkalization again, impurity is few; Acid-alkali treatment flavones content height, simple to operate; It is short that alumina is handled the alkaloid cycle.
Further specify the present invention below in conjunction with the specific embodiment, but the scope of protection of present invention is not limited to following embodiment.
The specific embodiment:
Embodiment 1:
Get the dry Folium Mori of 1kg, pulverize, the aqua calcis that adds 10Lph10, be heated to 50 ℃ of dynamic extraction 2 hours, extract twice, merge extractive liquid, filters hydrochloric acid and transfers ph to 5 to add the absorption of 500mlD101 resin column, washing is neutral, 3L65% ethanol elution flavones in mulberry leaves is collected flow point and is added 25g injection class medical activated carbon reflux decolour, and hydrochloric acid is regulated ph to 1 and left standstill crystallization, the 85% ethanol sodium hydroxide solution dissolving that leaches reuse ph9 filters transfers ph to 3 crystallization, it is dissolving crystallized to leach reuse 75% alcohol reflux, leaches the dry flavones in mulberry leaves 21g of getting, content 91%.
Above-mentioned Folium Mori residue adding 6L90% ethanol and 60g active carbon reflux, extract, 2 hours, extract 2 times, merging filtrate hydrochloric acid transfers to the neutral ethanol that reclaims, paste adds acetone solution, filter and add the neutral alumina short wide column, collection lower column liquid recovery acetone, the crystallization of adding ammonia, it is dissolving crystallized to leach coarse crystallization reuse 90% alcohol reflux, the dry Folium Mori alkaloid 90% that gets of filtering for crystallizing thing.
Embodiment 2:
Get the dry Folium Mori of 1kg, pulverize, the aqua calcis that adds 6Lph12, be heated to 30 ℃ of dynamic extraction 3 hours, extract 3 times, merge extractive liquid, filters hydrochloric acid and transfers ph to 7 to add the absorption of 500mlD101 resin column, washing is neutral, 2.5L70% ethanol elution flavones in mulberry leaves is collected flow point and is added 50g injection class medical activated carbon reflux decolour, and hydrochloric acid is regulated ph to 3 and left standstill crystallization, the 90% ethanol sodium hydroxide solution dissolving that leaches reuse ph10 filters transfers ph to 2 crystallization, it is dissolving crystallized to leach reuse 80% alcohol reflux, leaches the dry flavones in mulberry leaves 24g of getting, content 90%.
Above-mentioned Folium Mori residue adding 4L85% ethanol and 80g active carbon reflux, extract, 1 hour, extract 3 times, merging filtrate hydrochloric acid transfers to the neutral ethanol that reclaims, paste adds acetone solution, filter and add the neutral alumina short wide column, collection lower column liquid recovery acetone, the crystallization of adding ammonia, it is dissolving crystallized to leach coarse crystallization reuse 85% alcohol reflux, the dry Folium Mori alkaloid 90% that gets of filtering for crystallizing thing.
Embodiment 3:
Get the dry Folium Mori of 1kg, pulverize, the sodium hydroxide solution that adds 10Lph10, be heated to 40 ℃ of dynamic extraction 2 hours, extract twice, merge extractive liquid, filters hydrochloric acid and transfers ph to 6 to add the absorption of 500mlSPD100 resin column, washing is neutral, 3L50% ethanol elution flavones in mulberry leaves is collected flow point and is added 60g injection class medical activated carbon reflux decolour, and hydrochloric acid is regulated ph to 2 and left standstill crystallization, the 95% ethanol sodium hydroxide solution dissolving that leaches reuse ph12 filters transfers ph to 3 crystallization, it is dissolving crystallized to leach reuse 75% alcohol reflux, leaches the dry flavones in mulberry leaves 22g of getting, content 90%.
Above-mentioned Folium Mori residue adding 5L95% ethanol and 50g active carbon reflux, extract, 2 hours, extract 2 times, merging filtrate sulphuric acid transfers to the neutral ethanol that reclaims, paste adds acetone solution, filter and add the neutral alumina short wide column, collection lower column liquid recovery acetone, the crystallization of adding ammonia, it is dissolving crystallized to leach coarse crystallization reuse 90% alcohol reflux, the dry Folium Mori alkaloid 90% that gets of filtering for crystallizing thing.
Embodiment 4:
Get the dry Folium Mori of 5kg, pulverize, the aqua calcis that adds 50Lph10, be heated to 30 ℃ of dynamic extraction 2 hours, extract twice, merge extractive liquid, filters sulphuric acid and transfers ph to 5 to add the absorption of 2.5LD101 resin column, washing is neutral, 15L60% ethanol elution flavones in mulberry leaves is collected flow point and is added 300g injection class medical activated carbon reflux decolour, and sulphuric acid is regulated ph to 1 and left standstill crystallization, the 90% ethanol sodium hydroxide solution dissolving that leaches reuse ph10 filters transfers ph to 2 crystallization, it is dissolving crystallized to leach reuse 75% alcohol reflux, leaches the dry flavones in mulberry leaves 120g of getting, content 90%.
Above-mentioned Folium Mori residue adding 25L90% ethanol and 500g active carbon reflux, extract, 2 hours, extract 2 times, merging filtrate hydrochloric acid transfers to the neutral ethanol that reclaims, paste adds acetone solution, filter and add the neutral alumina short wide column, collection lower column liquid recovery acetone, the crystallization of adding ammonia, it is dissolving crystallized to leach coarse crystallization reuse 90% alcohol reflux, the dry Folium Mori alkaloid 90% that gets of filtering for crystallizing thing.
Embodiment 5:
Get the dry Folium Mori of 10kg, pulverize, the aqua calcis that adds 100Lph10, be heated to 40 ℃ of dynamic extraction 2 hours, extract 2 times, merge extractive liquid, filters hydrochloric acid and transfers ph to 5 to add the absorption of 5LSPD100 resin column, washing is neutral, 25L65% ethanol elution flavones in mulberry leaves is collected flow point and is added 500g injection class medical activated carbon reflux decolour, and hydrochloric acid is regulated ph to 2 and left standstill crystallization, the 85% ethanol sodium hydroxide solution dissolving that leaches reuse ph9 filters transfers ph to 2 crystallization, it is dissolving crystallized to leach reuse 75% alcohol reflux, leaches the dry flavones in mulberry leaves 215g of getting, content 91%.
Above-mentioned Folium Mori residue adding 50L90% ethanol and 500g active carbon reflux, extract, 2 hours, extract 2 times, merging filtrate hydrochloric acid transfers to the neutral ethanol that reclaims, paste adds acetone solution, filter and add the neutral alumina short wide column, collection lower column liquid recovery acetone, the crystallization of adding ammonia, it is dissolving crystallized to leach coarse crystallization reuse 85% alcohol reflux, the dry Folium Mori alkaloid 90% that gets of filtering for crystallizing thing.
Claims (7)
1. one kind prepares flavone, alkaloidal method from Folium Mori, it is characterized in that comprising following step:
1) Folium Mori are pulverized, doubly measured 30-50 ℃ of dynamic extraction 1-3 of ph9-12 aqueous alkali hour with 6-10, extracts 2-3 time, merging aqueous extract, medicinal residues add 4-6 again and doubly measure 85-95% ethanol and active carbon reflux, extract, 2-3 time, the merging alcohol extract;
2) the step 1) aqueous extract is transferred ph5-7 add macroporous resin column absorption, water-pure eluting is collected the flavones in mulberry leaves flow point, and behind the adding active carbon reflux decolour, concentrating under reduced pressure ph1-3 leaves standstill crystallization;
3) leach the dissolving of coarse crystallization thing alkali alcohol and transfer the ph2-4 crystallization, it is dissolving crystallized to leach reuse 70-80% alcohol reflux, leaches crystal and is drying to obtain Folium Mori total flavonoids;
4) the step 1) alcohol extract is transferred to neutrality, reclaim ethanol, add acetone solution and filter to paste, add the aluminium oxide short wide column, collect lower column liquid and reclaim acetone, add the ammonia crystallization, it is dissolving crystallized to leach crystallization reuse 85-90% alcohol reflux, is drying to obtain the Folium Mori biology total alkali.
2. according to described flavone, the alkaloidal method of from Folium Mori, preparing of claim 1, it is characterized in that optional sodium hydroxide of alkali or calcium hydroxide in the step 1).
3. according to described flavone, the alkaloidal method of from Folium Mori, preparing of claim 1, it is characterized in that step 2), 3), 4) in optional hydrochloric acid, sulphuric acid or phosphoric acid a kind of of accent ph.
4. according to described flavone, the alkaloidal method of from Folium Mori, preparing of claim 1, it is characterized in that step 2) middle optional D101 of macroporous resin or SPD100, water-pure eluting is for washing neutrality 5-6BV50-70% ethanol elution flavones in mulberry leaves again.
5. according to described flavone, the alkaloidal method of from Folium Mori, preparing of claim 1, it is characterized in that step 1), 2) in active carbon be injection class medicinal activity charcoal, the 1-3% of addition liquid, bleaching time are 1-2 hour.
6. according to described flavone, the alkaloidal method of from Folium Mori, preparing of claim 1, it is characterized in that the alkali alcohol in the step 3) is the 90-95% ethanol sodium hydroxide solution of ph9-12.
7. according to described flavone, the alkaloidal method of from Folium Mori, preparing of claim 1, it is characterized in that the aluminium oxide in the step 4) is a 120-200 order neutral alumina.
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| CN201010130263A CN101862371A (en) | 2010-03-23 | 2010-03-23 | Method for preparing flavone and alkaloid from mulberry leaves |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102277009A (en) * | 2011-07-27 | 2011-12-14 | 晨光生物科技集团股份有限公司 | Method for extracting and purifying cottonseed brown pigment from cottonseed hulls |
| CN103641771A (en) * | 2013-12-23 | 2014-03-19 | 江苏省中国科学院植物研究所 | Method for preparing both amino sugar and flavone extractive from silkworm excrement |
-
2010
- 2010-03-23 CN CN201010130263A patent/CN101862371A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102277009A (en) * | 2011-07-27 | 2011-12-14 | 晨光生物科技集团股份有限公司 | Method for extracting and purifying cottonseed brown pigment from cottonseed hulls |
| CN103641771A (en) * | 2013-12-23 | 2014-03-19 | 江苏省中国科学院植物研究所 | Method for preparing both amino sugar and flavone extractive from silkworm excrement |
| CN103641771B (en) * | 2013-12-23 | 2016-05-11 | 江苏省中国科学院植物研究所 | A kind of method of simultaneously preparing iminosugar and chromocor extract from silkworm excrement |
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Application publication date: 20101020 |