CN109053666A - A kind of extracting method of dihydromyricetin - Google Patents
A kind of extracting method of dihydromyricetin Download PDFInfo
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- CN109053666A CN109053666A CN201811032757.3A CN201811032757A CN109053666A CN 109053666 A CN109053666 A CN 109053666A CN 201811032757 A CN201811032757 A CN 201811032757A CN 109053666 A CN109053666 A CN 109053666A
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- graphene
- ethyl alcohol
- dihydromyricetin
- liquid
- extracting method
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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
- C07D311/32—2,3-Dihydro derivatives, e.g. flavanones
-
- 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
Abstract
The present invention relates to field of plant extraction, and in particular to a kind of extracting method of dihydromyricetin, comprising the following steps: S1. impregnates 3 ~ 5h of vine tea with deionized water, microwave radiation is used in soaking process, and maintain water temperature at 90 ~ 96 DEG C；S2. the liquid that step S1 is obtained is filtered while hot；S3. the obtained filtrate of step S2 is added to ethyl alcohol, after ethyl alcohol is added, the concentration of ethyl alcohol is 65% ~ 70%；S4. the obtained solution of step S3 is ultrasonically treated；S5. liquid step S4 obtained is by containing graphene filtering note；S6. the liquid that collection step S5 is obtained carries out condensation evaporation.The graphene restored using graphene oxide, since many oxygen-containing functional groups during graphene oxide restores are reduced, graphene surface will appear defect, and the further once big surface area of graphene increases the adsorption capacity of graphene.The dihydromyricetin that the method for the present invention obtains has higher purity.
Description
Technical field
The present invention relates to field of plant extraction, and in particular to a kind of extracting method of dihydromyricetin.
Background technique
Dihydromyricetin (3,5,7,3',4',5'-hexahydroxy-2,3-dihydroflavonol, dihydromyricetin,
DMY) DMY) it is a kind of polyphenol hydroxyl flavanonol, also known as ampelopsin, belong to flavone compound.Data shows dihydro poplar
Syphilis is largely present in Vitaceae ampelopsis, such as vine tea, that is, ampelopsis grossdentata, ampelopsis cantoniensis), leatherleaf porcelain ampelopsis (A
.chaffanjonii), porcelain ampelopsis, Northeastern Caulis seu folium ampelopsis brevipedunculatae, Ampelopsis (A .sinciavar .hancei) etc., wherein vine tea
Especially especially.Ampelopsis grossdentata in provinces and regions such as Guangdong, Guangxi, Yunnan, Hunan, Hubei, the Jiangxi for being distributed widely in China is planted
In the young young stem and leaf of object, it is found that the content of dihydromyricetin in its spring and summer children's young stem and leaf reaches 20 % or more of sample dry weight,
Lobus cardiacus in spire up to 40 % with.
Dihydromyricetin has anti-inflammatory, cough-relieving, eliminating the phlegm, analgesia, antibacterial, anti-hypertension, lipid-loweringing, antitumor, liver protecting
Etc. many physiological activity, great exploitation potential.Therefore, the recovery rate for how improving dihydromyricetin is increasingly subject to the pass of people
Note.
Graphene is the star's material being concerned in recent years, has unique structure and property.In structure, graphene
It can be considered as the graphite of single layer, by sp2The carbon atom composition hexatomic ring of hydridization is its basic structural unit.Graphene
It is considered and constitutes other sp2 The basis of carbon material, such as fullerene, carbon nanotube (CNTs) and graphite.The unique texture of graphene
So that it has how peculiar performance and application, huge potentiality have been illustrated in many fields.Research shows that graphene exists
The related fieldss such as electronics, the energy, advanced material, catalysis, biomedicine and environmental science have great application value.Such as
Graphene has excellent electric property, can be used for field-effect tube, integrated circuit, transparent conductive film, flexible lithium battery
Deng.Graphene excellent in mechanical performance, intensity are 100 times of steel or more, can be used for manufacturing the high-strength material of lightweight.
Graphene has photoelectric conversion performance, photoelectric conversion device is had been used to manufacture, such as solar battery and display.Graphite
Alkene material has good biocompatibility, can be used for drug carrier band, living imaging, biochemical analysis and biological tissue's work
Journey etc..In addition there are also the specific surface areas of super large to have good suction-operated for graphene, is generally used to carry out water process.
Summary of the invention
It is an object of the invention to overcome the problems of the prior art, a kind of extracting method of dihydromyricetin is provided.
The purpose of the present invention is achieved by the following technical programs:
A kind of extracting method of dihydromyricetin, comprising the following steps:
S1. 3 ~ 5h of vine tea is impregnated with deionized water, microwave radiation is used in soaking process, and maintain water temperature at 90 ~ 96 DEG C；
S2. the liquid that step S1 is obtained is filtered while hot；
S3. the obtained filtrate of step S2 is added to ethyl alcohol, after ethyl alcohol is added, the concentration of ethyl alcohol is 65% ~ 70%；
S4. the obtained solution of step S3 is ultrasonically treated；
S5. liquid step S4 obtained is by containing graphene filtering note；
S6. the liquid that collection step S5 is obtained carries out condensation evaporation.
The dissolution of dihydromyricetin in water is promoted using the method for microwave during the extraction process, is filtered while hot, removal is not
It is dissolved in the impurity of water, is then further extracted using ethyl alcohol, promotes the dissolution of dihydromyricetin using ultrasound, then uses stone
Black alkene is adsorbed.Since graphene has very big specific surface area, there is stronger suction-operated, it can be in adsorbent solution
Impurity.
Preferably, the time that water impregnates in the step S1 is 4h, and the water temperature is 95 DEG C
Preferably, the concentration of ethyl alcohol is 68% in the step S3.
Preferably, the time being ultrasonically treated in the step S4 is 27 ~ 29 min.
Preferably, graphene described in the step S5 is to be obtained using the method for redox graphene.
The graphene restored using graphene oxide, due to many oxygen-containing during graphene oxide restores
Functional group is reduced, and graphene surface will appear defect, and the further once big surface area of graphene increases the suction of graphene
Attached ability.
The present invention has following technical effect that compared with prior art
A kind of extracting method of dihydromyricetin promotes dihydromyricetin in water using the method for microwave during the extraction process
Dissolution, filters while hot, removes impurity not soluble in water, is then further extracted using ethyl alcohol, promotes dihydro poplar using ultrasound
Then the dissolution of syphilis is adsorbed using graphene.Since graphene has very big specific surface area, there is stronger absorption
Effect, can be with the impurity in adsorbent solution.The graphene restored using graphene oxide, due to being restored in graphene oxide
During many oxygen-containing functional group be reduced, graphene surface will appear defect, the further once big surface of graphene
Product, increases the adsorption capacity of graphene.The dihydromyricetin that the method for the present invention obtains has higher purity.
Specific embodiment
The present invention can be explained further and illustrate in conjunction with following specific embodiments and comparative example, but specific embodiment is not
There is any type of restriction to the present invention.Test method without specific conditions in lower example embodiment, usually according to this field
Normal condition or the condition suggested according to manufacturer.Those skilled in the art is done any non-on the basis of the present invention
Substantive variation and replacement belongs to scope of the present invention.
Embodiment 1
A kind of extracting method of dihydromyricetin, comprising the following steps:
S1. the lobus cardiacus of spire of 5g vine tea is impregnated with deionized water, 3h uses microwave radiation in soaking process, and keeps
Water temperature is at 90 DEG C；
S2. the liquid that step S1 is obtained is filtered while hot；
S3. the obtained filtrate of step S2 is added to ethyl alcohol, after ethyl alcohol is added, the concentration of ethyl alcohol is 65%；
S4. the obtained solution of step S3 is ultrasonically treated；
S5. liquid step S4 obtained is by containing graphene filtering note；
S6. the liquid that collection step S5 is obtained carries out condensation evaporation.
Further, the time that water impregnates in step S1 is 4h, and the water temperature is 95 DEG C
Further, the concentration of ethyl alcohol is 68% in step S3.
Further, the time being ultrasonically treated in step S4 is 27 min.
Further, graphene described in step S5 is to be obtained using the method for redox graphene.
The dihydromyricetin finally obtained is 1.76g.
Embodiment 2
A kind of extracting method of dihydromyricetin, comprising the following steps:
S1. the lobus cardiacus of spire of 5g vine tea is impregnated with deionized water, 5h uses microwave radiation in soaking process, and protects
Water holding temperature is at 96 DEG C；
S2. the liquid that step S1 is obtained is filtered while hot；
S3. the obtained filtrate of step S2 is added to ethyl alcohol, after ethyl alcohol is added, the concentration of ethyl alcohol is 70%；
S4. the obtained solution of step S3 is ultrasonically treated；
S5. liquid step S4 obtained is by containing graphene filtering note；
S6. the liquid that collection step S5 is obtained carries out condensation evaporation.
Further, the time that water impregnates in step S1 is 4h, and the water temperature is 95 DEG C
Further, the concentration of ethyl alcohol is 68% in step S3.
Further, the time being ultrasonically treated in step S4 is 29 min.
Further, graphene described in step S5 is to be obtained using the method for redox graphene.
The dihydromyricetin finally obtained is 1.72g.
Comparative example 1
A kind of extracting method of dihydromyricetin, comprising the following steps:
S1. the lobus cardiacus of spire of 5g vine tea is impregnated with deionized water, 3h uses microwave radiation in soaking process, and keeps
Water temperature is at 90 DEG C；
S2. the liquid that step S1 is obtained is filtered while hot；
S3. the obtained filtrate of step S2 is added to ethyl alcohol, after ethyl alcohol is added, the concentration of ethyl alcohol is 65%；
S4. the obtained solution of step S3 is ultrasonically treated；
S5. the liquid that collection step S4 is obtained carries out condensation evaporation.
Further, the time that water impregnates in step S1 is 4h, and the water temperature is 95 DEG C
Further, the concentration of ethyl alcohol is 68% in step S3.
Further, the time being ultrasonically treated in step S4 is 27 min.
The dihydromyricetin finally obtained is 1.18g.
Comparative example 2
A kind of extracting method of dihydromyricetin, comprising the following steps:
S1. the lobus cardiacus of spire of 5g vine tea is impregnated with deionized water, 3h uses microwave radiation in soaking process, and keeps
Water temperature is at 90 DEG C；
S2. the liquid that step S1 is obtained is filtered while hot；
S3. the obtained filtrate of step S2 is added to ethyl alcohol, after ethyl alcohol is added, the concentration of ethyl alcohol is 65%；
S4. the obtained solution of step S3 is ultrasonically treated；
S5. liquid step S4 obtained is by containing D101 macroreticular resin filtering note；
S6. the liquid that collection step S5 is obtained carries out condensation evaporation.
Further, the time that water impregnates in step S1 is 4h, and the water temperature is 95 DEG C
Further, the concentration of ethyl alcohol is 68% in step S3.
Further, the time being ultrasonically treated in step S4 is 27 min.
The dihydromyricetin finally obtained is 1.32g.
Comparative example 3
A kind of extracting method of dihydromyricetin, comprising the following steps:
S1. the lobus cardiacus of spire of 5g vine tea is impregnated with deionized water, 3h uses microwave radiation in soaking process, and keeps
Water temperature is at 90 DEG C；
S2. the liquid that step S1 is obtained is filtered while hot；
S3. the obtained filtrate of step S2 is added to ethyl alcohol, after ethyl alcohol is added, the concentration of ethyl alcohol is 65%；
S4. the obtained solution of step S3 is ultrasonically treated；
S5. liquid step S4 obtained is by containing H-103 macroreticular resin filtering note；
S6. the liquid that collection step S5 is obtained carries out condensation evaporation.
Further, the time that water impregnates in step S1 is 4h, and the water temperature is 95 DEG C
Further, the concentration of ethyl alcohol is 68% in step S3.
Further, the time being ultrasonically treated in step S4 is 27 min.
The dihydromyricetin finally obtained is 1.35g.
A kind of extracting method of dihydromyricetin, comprising the following steps:
S1. the lobus cardiacus of spire of 5g vine tea is impregnated with deionized water, 3h uses microwave radiation in soaking process, and keeps
Water temperature is at 90 DEG C；
S2. the liquid that step S1 is obtained is filtered while hot；
S3. the obtained filtrate of step S2 is added to ethyl alcohol, after ethyl alcohol is added, the concentration of ethyl alcohol is 65%；
S4. the obtained solution of step S3 is ultrasonically treated；
S5. liquid step S4 obtained is by containing graphene filtering note；
S6. the liquid that collection step S5 is obtained carries out condensation evaporation.
Further, the time that water impregnates in step S1 is 4h, and the water temperature is 95 DEG C
Further, the concentration of ethyl alcohol is 68% in step S3.
Further, the time being ultrasonically treated in step S4 is 27 min.
Further, graphene described in step S5 is to be obtained using the method for mechanical stripping.
The dihydromyricetin finally obtained is 1.68g.
By above embodiments and comparative example it can be found that the dihydro of higher purity can be obtained using method of the invention
Myricetin, the graphene obtained in particular by electronation are adsorbed, the dihydromyricetin of available higher purity.
Claims (5)
1. a kind of extracting method of dihydromyricetin, which comprises the following steps:
S1. 3 ~ 5h of vine tea is impregnated with deionized water, microwave radiation is used in soaking process, and maintain water temperature at 90 ~ 96 DEG C；
S2. the liquid that step S1 is obtained is filtered while hot；
S3. the obtained filtrate of step S2 is added to ethyl alcohol, after ethyl alcohol is added, the concentration of ethyl alcohol is 65% ~ 70%；
S4. the obtained solution of step S3 is ultrasonically treated；
S5. liquid step S4 obtained is by containing graphene filtering note；
S6. the liquid that collection step S5 is obtained carries out condensation evaporation.
2. the extracting method of dihydromyricetin according to claim 1, which is characterized in that in the step S1 water impregnate when
Between be 4h, the water temperature be 95 DEG C.
3. the extracting method of dihydromyricetin according to claim 1, which is characterized in that the concentration of ethyl alcohol in the step S3
It is 68%.
4. the extracting method of the second light industry bureau myricetin according to claim 1, which is characterized in that be ultrasonically treated in the step S4
Time is 27 ~ 29 min.
5. the extracting method of dihydromyricetin according to claim 1, which is characterized in that graphene described in the step S5
It is obtained for the method using redox graphene.
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| CN201811032757.3A CN109053666A (en) | 2018-09-05 | 2018-09-05 | A kind of extracting method of dihydromyricetin |
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| CN201811032757.3A CN109053666A (en) | 2018-09-05 | 2018-09-05 | A kind of extracting method of dihydromyricetin |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115386745A (en) * | 2022-08-23 | 2022-11-25 | 铜仁学院 | Method for comprehensively utilizing manganese anode slime resources |
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| CN103554076A (en) * | 2013-11-04 | 2014-02-05 | 贵州师范大学 | Method for rapidly extracting high-purity dihydromyricetin in ampelopsis grossedentata leaves |
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| CN106563004A (en) * | 2015-10-12 | 2017-04-19 | 中国药科大学 | Application of carbon nanomaterial to preparation of natural product |
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| US20180126367A1 (en) * | 2016-11-06 | 2018-05-10 | Massachusetts Institute Of Technology | Light-assisted photocatalyst regeneration and oxygen-resilient radical polymerization |
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2018
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| CN101805321A (en) * | 2010-04-16 | 2010-08-18 | 安徽省瑞森生物科技有限责任公司 | Method for extracting dihydromyricetin from vine tea |
| CN103554076A (en) * | 2013-11-04 | 2014-02-05 | 贵州师范大学 | Method for rapidly extracting high-purity dihydromyricetin in ampelopsis grossedentata leaves |
| CN104496956A (en) * | 2014-11-25 | 2015-04-08 | 程金生 | Extraction separation method of flavone component based on amination grapheme |
| US20160145229A1 (en) * | 2014-11-25 | 2016-05-26 | Shenzhen Violin Technology Co.,Ltd. | Extraction separation method of a flavone component based on graphene |
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| US20180126367A1 (en) * | 2016-11-06 | 2018-05-10 | Massachusetts Institute Of Technology | Light-assisted photocatalyst regeneration and oxygen-resilient radical polymerization |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115386745A (en) * | 2022-08-23 | 2022-11-25 | 铜仁学院 | Method for comprehensively utilizing manganese anode slime resources |
| CN115386745B (en) * | 2022-08-23 | 2024-02-13 | 铜仁学院 | Comprehensive utilization method of manganese anode slime resources |
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Application publication date: 20181221 |