CN104072463A - Method of extracting quercetin from myricaria - Google Patents
Method of extracting quercetin from myricaria Download PDFInfo
- Publication number
- CN104072463A CN104072463A CN201410266358.9A CN201410266358A CN104072463A CN 104072463 A CN104072463 A CN 104072463A CN 201410266358 A CN201410266358 A CN 201410266358A CN 104072463 A CN104072463 A CN 104072463A
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- CN
- China
- Prior art keywords
- falsetamarisk
- twig
- germany
- quercetin
- meal
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
- C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
- C07D311/22—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4
- C07D311/26—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3
- C07D311/28—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3 with aromatic rings attached in position 2 only
- C07D311/30—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3 with aromatic rings attached in position 2 only not hydrogenated in the hetero ring, e.g. flavones
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
- C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
- C07D311/22—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4
- C07D311/26—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3
- C07D311/40—Separation, e.g. from natural material; Purification
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Saccharide Compounds (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention relates to a method of extracting quercetin from myricaria and in particular relates to a method integrating enzymatic hydrolysis of enzyme with macroporous adsorption resin. The method comprises the steps of drying and crushing myricaria; carrying out enzymatic hydrolysis; adding an extraction solvent to carry out reflux extraction; carrying out pressure-reduced concentration; and purifying and concentrating. The method is simple in process, high in extraction efficiency, low in cost and suitable for large-scale industrial production.
Description
Technical field
The present invention relates to the extractive technique of activeconstituents in a kind of natural medicinal plant, be specifically related to a kind ofly utilize the method that biological enzyme zymolysis technique combines with macroporous adsorbent resin to extract the effective constituent in natural phant.
Background technology
Twig of Germany Falsetamarisk, its chemical composition mainly containing is: flavones, Quercitroside, Quercetin, kaempferol, gallic acid etc.Twig of Germany Falsetamarisk is a kind of Tibetan medicine, can be used for the promoting eruption of inducing sweat, and dispellings wind and arresting itching, and cures mainly measles without adequate eruption, rheumatic arthralgia, ringworm.Be distributed in Badong, Zigui and Wushan, Sichuan, be born in bank, the low mountains and rivers and roadside.
Quercetin, has another name called quercetin, Quercetin, molecular formula C
15h
10o
7, molecular weight 302.23.Be dissolved in Glacial acetic acid, it is yellow that alkaline aqueous solution is, hardly water-soluble, ethanolic soln; Taste is very bitter.Can be used as medicine, have preferably eliminate the phlegm, antitussive action, and have certain antiasthmatic effect.In addition reduce blood pressure in addition, strengthen capillary resistance, reduce capillary fragility, reducing blood-fat, coronary artery dilator, increase the effects such as coronary flow.Be used for the treatment of chronic bronchitis.Coronary heart disease and hyperpietic are also had to auxiliary therapeutic action.
The material source that at present Quercetin extracts is mainly to take Ginkgo Leaf and rutin as main, the invention provides the method for extracting Quercetin from another plant, thereby makes the plant origin of Quercetin more extensive.The present invention adopts is alcoholic solution reflux extraction, under the condition of biological enzymolysis, extract the Quercetin in Twig of Germany Falsetamarisk and adopt the purifying of macroporous adsorbent resin to Quercetin, make Quercetin go out rate and purity is all greatly improved.In the disclosed patent of application " a kind of method of extracting Quercetin from Folium Eucommiae " (patent No. 201210126236.0), a kind of method of extracting Quercetin is disclosed, its step is mainly and adopts alcoholic solution refluxing extraction, concentrates, purifying obtains Quercetin, wherein the process of material processing is insufficient, and the rate that goes out of material the inside effective constituent is greatly reduced.
Summary of the invention
The present invention be directed to the existing research of preparing the existing defect of method of Twig of Germany Falsetamarisk Quercetin and carrying out, be mainly for provide a kind of simple to operate, extraction efficiency is high, cost is low, extracting method that can realization of industrialization.
Step of the present invention is as follows:
A, by fresh Twig of Germany Falsetamarisk material, in temperature, be dry 1-3 hour in the baking oven of 60-70 ℃, pulverized 40-60 mesh sieve, collect meal standby;
B, take a certain amount of meal and be placed in extractor, add meal weight 0.5-1 water infiltration doubly, then add the biological enzyme reagent of meal weight 0.5%-3% to carry out enzyme digestion reaction, under the condition of 30-45 ℃, allow its enzyme digestion reaction 40-80min, collect enzymolysis raw material;
C, then in meal mixed solution, add extraction solvent, adopt alcoholic solution refluxing extraction method;
D, filtration, collect filtrate, and filter residue repeats to extract 2-4 time, and united extraction liquid is evaporated to the 1/4-1/2 of original volume;
E, by macroporous adsorbent resin on concentrated solution, use elutriant wash-out, collect ethanol eluate, be evaporated to the 1/4-1/2 of original volume.
Biological enzyme described in step b is a kind of in cellulase, amylase, hemicellulase and polygalacturonase.
The extraction solvent adding described in step c is the mixed solution of 30% hydrochloric acid and 75% methyl alcohol, and volume ratio is 1:1-4.
The starting material that add described in step c are 1:4-10 with the solid-liquid ratio that extracts solvent, and the time of each refluxing extraction is 60-120min.
Macroporous adsorbent resin described in step e is that a kind of in AB-8, D-101, D-101-I, DA-20, described elution process is: first use column volume 6-8 deionized water wash-out doubly, then the ethanol elution that is 75%-85% by 4-8 times of column volume, concentration.
The present invention first carries out enzymolysis processing to material, and the rate that goes out of effective constituent in Twig of Germany Falsetamarisk is greatly improved, and its operation steps is simple, environmentally safe; And the present invention adopts alcohol to follow sour mixed solution as extracting solvent, can improve to a great extent the extraction yield of Quercetin; The use of macroporous adsorbent resin, makes the purity of gained Quercetin higher, and macroporous adsorbent resin can reuse, thereby has reduced production cost, has industrialization meaning.
Below in conjunction with embodiment, further illustrate the present invention, but the scope of protection of present invention is not limited to following embodiment.
embodiment:
Embodiment 1:
It is in the baking oven of 70 ℃ dry 1 hour that fresh Twig of Germany Falsetamarisk is placed on to Temperature Setting, dry complete, pulverized and sieved 40 orders, collection meal is standby, take 100g Twig of Germany Falsetamarisk meal in extractor, add 50mL water, the cellulase enzymolysis 60min under the condition of 35 ℃ that simultaneously adds 2g, collect enzymolysis raw material, then add 400mL extraction solvent (extracting solvent is V30% hydrochloric acid: V75% methyl alcohol=1:3) refluxing extraction 60min, filter, collect filtrate, filter residue repeats refluxing extraction 2 times, and united extraction liquid is evaporated to 1/3 of original volume.By AB-8 macroporous adsorptive resins on concentrated solution, first use the deionized water wash-out of 6 times of column volumes, then the ethanol elution that is 75% by 5 times of column volumes, concentration, collect ethanol eluate, be evaporated to 1/4 of original volume, obtain Twig of Germany Falsetamarisk Quercetin sample.Through HPLC, detect, in gained starting material, the content of Quercetin is 89.5%, and the extraction yield of Quercetin is 60.41%.
Claims (7)
1. from Twig of Germany Falsetamarisk, extract a method for Quercetin, it is characterized in that adopting following operation steps:
A, by fresh Twig of Germany Falsetamarisk material, in temperature, be dry 1-3 hour in the baking oven of 60-70 ℃, pulverized 40-60 mesh sieve, collect meal standby;
B, take a certain amount of meal and be placed in extractor, add water infiltration and add biological enzyme reagent to carry out enzyme digestion reaction, collect enzymolysis raw material;
C, then in meal mixed solution, add extraction solvent, adopt refluxing extraction method;
D. filter, collect filtrate, filter residue repeats to extract 2-4 time, and united extraction liquid is evaporated to the 1/4-1/2 of original volume;
E, by macroporous adsorbent resin on concentrated solution, use elutriant wash-out, collect ethanol eluate, be evaporated to the 1/4-1/2 of original volume.
2. the method for extracting Quercetin from Twig of Germany Falsetamarisk according to claim 1, is characterized in that: the solid-liquid ratio of the meal described in step b and water is 1:0.5-1, and the amount that adds biological enzyme is the 0.5%-3% of meal weight.
3. the method for extracting Quercetin from Twig of Germany Falsetamarisk according to claim 1, it is characterized in that: the biological enzyme described in step b is a kind of in cellulase, amylase, hemicellulase and polygalacturonase, Temperature Setting during enzymolysis is at 30-45 ℃, and the time of enzyme digestion reaction is 40-80min.
4. the method for extracting Quercetin from Twig of Germany Falsetamarisk according to claim 1, it is characterized in that: the extraction solvent adding in step c is the mixed solution of 30% hydrochloric acid and 75% methyl alcohol, and volume ratio is 1:1-4.
5. the method for extracting Quercetin from Twig of Germany Falsetamarisk according to claim 1, is characterized in that: in step c, the solid-to-liquid ratio of refluxing extraction is 1:4-10, and the time of each refluxing extraction is 60-120min.
6. the method for extracting Quercetin from Twig of Germany Falsetamarisk according to claim 1, is characterized in that: the macroporous adsorbent resin described in step e is a kind of in AB-8, D-101, D-101-I, DA-20.
7. the method for extracting Quercetin from Twig of Germany Falsetamarisk according to claim 1, is characterized in that: the elution process described in step e is for first using column volume 6-8 deionized water wash-out doubly, then the ethanol elution that is 75%-85% by 4-8 times of column volume, concentration.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410266358.9A CN104072463A (en) | 2014-06-16 | 2014-06-16 | Method of extracting quercetin from myricaria |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410266358.9A CN104072463A (en) | 2014-06-16 | 2014-06-16 | Method of extracting quercetin from myricaria |
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| CN104072463A true CN104072463A (en) | 2014-10-01 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201410266358.9A Pending CN104072463A (en) | 2014-06-16 | 2014-06-16 | Method of extracting quercetin from myricaria |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108675977A (en) * | 2018-06-08 | 2018-10-19 | 滨州医学院 | One kind extracted from Chinese tamarisk separation kaempferide and Quercetin -3 ', the method for 4 '-dimethyl ether |
| CN115161367A (en) * | 2022-07-04 | 2022-10-11 | 云南西草资源开发有限公司 | Method for extracting quercetin from pyracantha fortuneana fruit by using stepped enzyme |
-
2014
- 2014-06-16 CN CN201410266358.9A patent/CN104072463A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108675977A (en) * | 2018-06-08 | 2018-10-19 | 滨州医学院 | One kind extracted from Chinese tamarisk separation kaempferide and Quercetin -3 ', the method for 4 '-dimethyl ether |
| CN115161367A (en) * | 2022-07-04 | 2022-10-11 | 云南西草资源开发有限公司 | Method for extracting quercetin from pyracantha fortuneana fruit by using stepped enzyme |
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Application publication date: 20141001 |
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| WD01 | Invention patent application deemed withdrawn after publication |