CN104193734A - Method for extracting isovitexin from ficus microcarpa - Google Patents
Method for extracting isovitexin from ficus microcarpa Download PDFInfo
- Publication number
- CN104193734A CN104193734A CN201410445690.1A CN201410445690A CN104193734A CN 104193734 A CN104193734 A CN 104193734A CN 201410445690 A CN201410445690 A CN 201410445690A CN 104193734 A CN104193734 A CN 104193734A
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- CN
- China
- Prior art keywords
- extraction
- extracting
- saponaretin
- isovitexin
- foliole banyan
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D407/00—Heterocyclic compounds containing two or more hetero rings, at least one ring having oxygen atoms as the only ring hetero atoms, not provided for by group C07D405/00
- C07D407/02—Heterocyclic compounds containing two or more hetero rings, at least one ring having oxygen atoms as the only ring hetero atoms, not provided for by group C07D405/00 containing two hetero rings
- C07D407/04—Heterocyclic compounds containing two or more hetero rings, at least one ring having oxygen atoms as the only ring hetero atoms, not provided for by group C07D405/00 containing two hetero rings directly linked by a ring-member-to-ring-member bond
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention relates to a method for extracting isovitexin from ficus microcarpa, and particularly relates to a method for extracting the isovitexin by combining an application flash extraction technology and enzymolysis-ultrasonic-assisted extraction. The method comprises the following treatment steps: placing fresh or dry ficus microcarpa into a container, adding 70%-80% ethanol, and carrying out smashing extraction on the ficus microcarpa on a traditional Chinese medicine extractor for 5-10 minutes; taking out, regulating a pH value to 4.0-5.5, and carrying out enzymolysis and ultrasonic-assisted extraction; filtering, alkalifying filter liquor for neutralization, purifying by adopting macroporous adsorption resin, and recrystallizing to obtain the high-purity isovitexin. The method disclosed by the invention is simple in process, has complementary advantages by combining two technologies, greatly shortens the extraction time and is low in cost, more favorable to environmental protection and suitable for industrialized production.
Description
Technical field
The present invention relates to a kind of method of extracting Saponaretin from Foliole banyan leaf, be specifically related to a kind of application and dodge combine with the enzymolysis-ultrasonic-assisted extraction method of extraction Saponaretin of the technology of putting forward, belong to Separation of Natural Products field.
Background technology
Foliole banyan leaf, has another name called little banyan leaf, the money that lands, and derives from the leaf of Moraceae ficus species banyan.Foliole banyan leaf is conventional herbal medicine among the people, and it is lightly seasoned, cool in nature, has that heat-clearing is delivered, effect of detoxify and promote the subsdence of swelling, the pain relieving of drying.Be used for the treatment of asthma and chronic bronchitis, also have significant effect at Cardiovarscular, anti-inflammatory, the aspect such as antibacterial.Wherein, mainly containing chemical compositions such as flavones, triterpenes and steroidal compounds, flavones ingredient is taking Saponaretin as main.Saponaretin, yellow shape dry powder, 228 DEG C of fusing points, water insoluble, be dissolved in the organic solvents such as ethanol, methyl alcohol, ethyl acetate, chloroform, belong to carbon glycosides flavones, Stability Analysis of Structures, is difficult for degraded, and has anti-oxidant, antibacterial isoreactivity.
Be at present mainly traditional pickling process, percolation, reflux extraction etc. about the method for extracting Saponaretin, all there is many deficiencies in these extraction methods, as many in impurity, and extraction time is long, and extraction yield is low, solvent consumption and residual greatly, high in cost of production.Patent CN1289470C " fast preparation method of several medicinal substances in high purity in Patrinia villosa Juss ", adopt extraction using alcohol, the steps such as organic solvent extraction, high performance countercurrent chromatography separation and purification, the method extraction time is long, consumption of organic solvent is large, and be subject to the restriction of plant and instrument, cost is high, is not suitable for scale operation.
Summary of the invention
The object of the present invention is to provide a kind of method of extracting fast and efficiently high purity Saponaretin, that the method has is simple to operate, reaction conditions is gentle, nontoxicity, environment amenable advantage, is easy to realize suitability for industrialized production.
The present invention includes following steps:
A. fresh or dry Foliole banyan leaf is put into container, add 70 ~ 80% the ethanol of 5 ~ 10 times, be placed on Chinese medicament extracting device the broken Foliole banyan leaf 5 ~ 10min of extraction;
B. take out, acetic acid/sodium-acetate is adjusted pH value to 4.0 ~ 5.5, adds 1 ~ 2% cellulase, is placed in ultrasonic unit, enzymolysis 40 ~ 60min at 250 ~ 400W, 40 ~ 60 DEG C;
C. filter, filtrate adds alkali and is neutralized to PH7.0, purification with macroreticular resin, and 40 ~ 50% the ethanol elution of 8 ~ 10BV, elutriant concentrating under reduced pressure, obtains crude product;
D. ethyl alcohol recrystallization 2 times, obtains highly purified Saponaretin.
Alkali described in step c is sodium hydroxide, potassium hydroxide or sodium carbonate.
Macroreticular resin described in step c is AB-8, D-140, ADS-5 etc.
The invention has the advantages that: application sudden strain of a muscle is put forward technology plant is carried out to fragmentation, makes material high-speed be crushed to suitable granularity, simultaneously with the external force such as high-speed stirring, vibration, has fully improved extraction efficiency; The cell walls of cellulose-binding enzyme enzymolysis of plants, makes cytoclasis again, under ultrasonication, accelerates the stripping of effective constituent, thereby has improved the speed and the productive rate that extract.That the present invention has advantages of is simple to operate, the cycle is short, product yield is high, purity is high, can realize large-scale industrialization and produce.
Below in conjunction with embodiment, the present invention is further elaborated, but the scope of protection of present invention is not limited to following embodiment.
Embodiment
Embodiment 1:
Foliole banyan leaf fresh or dry 1000g is put into container, add 80% the ethanol of 5 times, be placed on Chinese medicament extracting device the broken Foliole banyan leaf 5min of extraction, take out, acetic acid/sodium-acetate is adjusted pH value to 4.0, adds 1% cellulase, is placed in ultrasonic unit, enzymolysis 40min at 250W, 40 DEG C, filter, filtrate hydro-oxidation sodium is neutralized to PH7.0, AB-8 purification with macroreticular resin, 50% the ethanol elution of 8BV, elutriant concentrating under reduced pressure, recrystallizing methanol 2 times, obtains 5.3g Saponaretin, detect through HPLC, purity is 92.3%.
Embodiment 2:
Foliole banyan leaf fresh or dry 1000g is put into container, add 75% the ethanol of 8 times, be placed on Chinese medicament extracting device the broken Foliole banyan leaf 8min of extraction, take out, acetic acid/sodium-acetate is adjusted pH value to 5.0, adds 1.5% cellulase, is placed in ultrasonic unit, enzymolysis 50min at 300W, 50 DEG C, filter, filtrate hydro-oxidation sodium is neutralized to PH7.0, ADS-5 purification with macroreticular resin, 40% the ethanol elution of 10BV, elutriant concentrating under reduced pressure, recrystallizing methanol 2 times, obtains 6.2g Saponaretin, detect through HPLC, purity is 95.6%.
Embodiment 3:
Foliole banyan leaf fresh or dry 1000g is put into container, add 70% the ethanol of 10 times, be placed on Chinese medicament extracting device the broken Foliole banyan leaf 10min of extraction, take out, acetic acid/sodium-acetate is adjusted pH value to 5.5, adds 2% cellulase, is placed in ultrasonic unit, enzymolysis 60min at 400W, 60 DEG C, filter, filtrate hydro-oxidation sodium is neutralized to PH7.0, AB-8 purification with macroreticular resin, 45% the ethanol elution of 9BV, elutriant concentrating under reduced pressure, recrystallizing methanol 2 times, obtains 5.8g Saponaretin, detect through HPLC, purity is 93.8%.
Claims (3)
1. one kind is extracted the method for Saponaretin from Foliole banyan leaf, it is characterized in that, comprise the following steps: fresh or dry Foliole banyan leaf is put into container, add 70 ~ 80% the ethanol of 5 ~ 10 times, be placed on Chinese medicament extracting device the broken Foliole banyan leaf 5 ~ 10min of extraction, take out, acetic acid/sodium-acetate is adjusted pH value to 4.0 ~ 5.5, add 1 ~ 2% cellulase, be placed in ultrasonic unit, in 250 ~ 400W, enzymolysis 40 ~ 60min at 40 ~ 60 DEG C, filter, filtrate adds alkali and is neutralized to PH7.0, purification with macroreticular resin, 40 ~ 50% the ethanol elution of 8 ~ 10BV, elutriant concentrating under reduced pressure, recrystallizing methanol 2 times, obtain highly purified Saponaretin.
2. a kind of method of extracting Saponaretin from Foliole banyan leaf according to claim 1, is characterized in that, described alkali is sodium hydroxide, potassium hydroxide or sodium carbonate.
3. a kind of method of extracting Saponaretin from Foliole banyan leaf according to claim 1, is characterized in that, described macroreticular resin is AB-8, D-140, ADS-5 etc.
Priority Applications (1)
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CN201410445690.1A CN104193734A (en) | 2014-09-04 | 2014-09-04 | Method for extracting isovitexin from ficus microcarpa |
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CN201410445690.1A CN104193734A (en) | 2014-09-04 | 2014-09-04 | Method for extracting isovitexin from ficus microcarpa |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107456483A (en) * | 2017-08-31 | 2017-12-12 | 吉林修正药业新药开发有限公司 | A kind of pharmaceutical composition for being used for cough and asthma and chronic bronchitis and preparation method thereof |
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2014
- 2014-09-04 CN CN201410445690.1A patent/CN104193734A/en active Pending
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107456483A (en) * | 2017-08-31 | 2017-12-12 | 吉林修正药业新药开发有限公司 | A kind of pharmaceutical composition for being used for cough and asthma and chronic bronchitis and preparation method thereof |
CN107456483B (en) * | 2017-08-31 | 2020-05-19 | 吉林修正药业新药开发有限公司 | A pharmaceutical composition for treating cough and asthma and chronic bronchitis, and its preparation method |
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Application publication date: 20141210 |