CN108047184A - A kind of method that dihydromyricetin is extracted from ampelopsis grossdentata - Google Patents
A kind of method that dihydromyricetin is extracted from ampelopsis grossdentata Download PDFInfo
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- CN108047184A CN108047184A CN201810074897.0A CN201810074897A CN108047184A CN 108047184 A CN108047184 A CN 108047184A CN 201810074897 A CN201810074897 A CN 201810074897A CN 108047184 A CN108047184 A CN 108047184A
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- dihydromyricetin
- extracted
- water
- molecular sieve
- ampelopsis grossdentata
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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
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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
- C07D311/40—Separation, e.g. from natural material; Purification
Abstract
A kind of method that dihydromyricetin is extracted from ampelopsis grossdentata, comprises the following steps：(1) using ampelopsis grossdentata leaf, stem as raw material, extracted with water or ethanol water, repeat extraction 23 times, obtain crude extract；Crude extract is concentrated, is cooled to 0 20 DEG C, stands, pours out solution, lower floor's solid is cleaned with normal-temperature water, and solid is dissolved with ethanol water, obtains solution；(2) isolate and purify：The pH value of regulating step (1) acquired solution is 57, upper molecular sieve chromatography, it is adsorbed with 0.5 1.0mL/min flow velocitys, it is first eluted with water and removes water-solubility impurities and the macromolecular components such as carbohydrate, molecular sieve chromatography is eluted with ethanol water again, the high eluent of dihydromyricetin cellulose content is collected, is concentrated to give dihydromyricetin, purity is 85 93%.This method isolates and purifies dihydromyricetin using molecular sieve, and material can be recycled, cost-effective, simple for process, be easy to industrialized production and application.
Description
Technical field
The present invention relates to a kind of methods that dihydromyricetin is extracted from ampelopsis grossdentata.
Background technology
Dihydromyricetin traditional extraction technology mainly has decocting method, extraction, soxhlet extraction method etc., and efficiency is low, high energy consumption
And time-consuming；Emerging extractive technique has ultrasonic wave assisted extraction, microwave abstracting etc., and extraction efficiency is high, it is few to take.It is currently used
Isolation technics has solvent extraction, resin separation etc..
Ampelopsis grossdentata also known as vine tea, Maoyanmei tea, are a kind of wild bejucoes, and wherein main active is
Dihydromyricetin.It is among the people drink practice and scientific research the result shows that, ampelopsis grossdentata have clearing heat and detoxicating, antibacterial anti-inflammatory, subtract
Lipoid and reducing blood pressure, relieving alcoholism and protecting liver and other effects；Flavones ingredient content is up to 9.37% in ampelopsis grossdentata, and dihydromyricetin is wherein
One of main component, prevention alcoholic liver, fatty liver, inhibit incidence, anti-hypertension that liver cell deteriorates, reduces liver cancer,
Inhibit the formation of extracorporeal platelet aggregation and internal thrombus, reduce blood fat and blood glucose level, improve superoxide dismutase activity
And liver protecting etc. has special efficacy.It is mostly extracted at present in document and patent using hot water or alcohol water, with zygostyle layer
The techniques removal of impurities such as analysis, crystallization, and soluble impurity such as polysaccharide, protein, amino acid etc. are more in dihydromyricetin crude extract, remove
General labourer's skill is cumbersome, and solvent-oil ratio is big, of high cost and environmental pollution is serious.
Zeolite molecular sieve is a kind of with regular pore passage structure, silicon aluminate crystal of the inner surface with very big gap.
Hole in crystal is connected by the identical duct of many diameters, can be by the Molecular Adsorption smaller than its aperture, point bigger than aperture
Sub- exclusion, thus with good ion-exchange performance and adsorption selectivity, play the role of screening molecule.Zeolite point
Son sieve because of its special pore passage structure, the characteristics such as high-specific surface area, high hydrothermal stability and be widely used in ion exchange, gas
Body is adsorbed with separating, and is especially widely used in fields such as catalysis.
So far, it yet there are no the correlative study report using molecular sieve as carrier separating dihydromyricetin.
The content of the invention
The technical problem to be solved by the invention is to provide a kind of molecular sieves as being extracted in the slave ampelopsis grossdentata of carrier
The method of dihydromyricetin.
The technical solution adopted by the present invention to solve the technical problems is：One kind extracts dihydromyricetin from ampelopsis grossdentata
The method of element, comprises the following steps：
(1) using ampelopsis grossdentata leaf, stem as raw material, extracted with water or ethanol water, 50-90 DEG C of Extracting temperature, while hot
Filtering repeats extraction 2-3 times, obtains crude extract；
Crude extract is concentrated into 3-8 times of raw material weight, is cooled to 0-20 DEG C, stands, pours out solution, lower floor's solid is with normal
Warm water cleans 2-3 times, and solid is dissolved with ethanol water, obtains solution；
(2) isolate and purify：The pH value of regulating step (1) acquired solution be 5-7, upper molecular sieve chromatography, with 0.5-
1.0mL/min flow velocitys adsorb, and are first eluted with water and remove water-solubility impurities and the macromolecular components such as carbohydrate, then with ethanol water pair
Molecular sieve chromatography is eluted, and is collected the high eluent of dihydromyricetin cellulose content, is concentrated to give dihydromyricetin, purity 85-
93%.
Further, in step (1), the volume fraction of ethanol water used in extraction is 30-80%.
Further, in step (1), the solid-liquid ratio 1 of extraction:6-15, unit kg/L.
Further, in step (1), the time of standing is 10-20h, preferably 12h.
Further, in step (1), the volume fraction of ethanol water used in dissolving is 30-60%.
Further, in step (2), it is water-soluble miscellaneous to remove carbohydrate etc. with 2.5-4.0 times of column volume (preferably 3 times) amount water elution
Matter and macromolecular components.
Further, in step (2), ethanol water is measured to molecular sieve chromatography with 2.5-4.0 times of column volume (preferably 3 times)
It is eluted.
Further, in step (2), the volume fraction of ethanol water used in elution is 90-95%.
Further, in step (2), the molecular sieve is any one in Y types, ZSM types, A types equimolecular sieve.
Further, in step (2), molecular sieve used carries out pre-treatment：Molecular sieve is placed in Muffle furnace, 600 ± 50 DEG C of height
Temperature 4 ± 1h of calcining, removal of impurities.
This method isolates and purifies dihydromyricetin using molecular sieve, and material can be recycled, cost-effective, work
Skill is simple, is easy to industrialized production and application.
Specific embodiment
The invention will be further described with reference to embodiments.
Embodiment 1
A kind of method that dihydromyricetin is extracted from ampelopsis grossdentata, comprises the following steps：
(1) using ampelopsis grossdentata leaf, stem as raw material, being extracted with ethanol water, 80-90 DEG C of Extracting temperature filters while hot,
Extraction 2 times is repeated, obtains crude extract；
Crude extract is concentrated into 5 times of raw material weight, is cooled to 20 DEG C, stands, pours out solution, lower floor's solid is steamed with room temperature
Distilled water is cleaned 3 times, and solid is dissolved with ethanol water, obtains solution；
(2) isolate and purify：The pH value of regulating step (1) acquired solution is 6, and upper molecular sieve chromatography is flowed with 0.8mL/min
Speed absorption first removes water-solubility impurities and the macromolecular components such as carbohydrates with 3 times of column volume amount water elutions, then with 3 times of amounts of column volume
Ethanol water elutes molecular sieve chromatography, collects the high eluent of dihydromyricetin cellulose content, is concentrated to give dihydromyricetin,
Purity is 93%.
In step (1), the volume fraction of ethanol water used in extraction is 60%.
In step (1), the solid-liquid ratio 1 of extraction:10, unit kg/L.
In step (1), the time of standing is 12h.
In step (1), the volume fraction of ethanol water used in dissolving is 60%.
In step (2), the volume fraction of ethanol water used in elution is 95%.
In step (2), the molecular sieve is ZSM type molecular sieves.
In step (2), molecular sieve used carries out pre-treatment：ZSM type molecular sieves are placed in Muffle furnace, 600 DEG C of high-temperature calcinations
4h, removal of impurities.
Embodiment 2
A kind of method that dihydromyricetin is extracted from ampelopsis grossdentata, comprises the following steps：
(1) using ampelopsis grossdentata leaf, stem as raw material, being extracted with ethanol water, 70-80 DEG C of Extracting temperature filters while hot,
Extraction 2 times is repeated, obtains crude extract；
Crude extract is concentrated into 6 times of raw material weight, is cooled to 15 DEG C, stands, pours out solution, lower floor's solid is steamed with room temperature
Distilled water is cleaned 3 times, and solid is dissolved with ethanol water, obtains solution；
(2) isolate and purify：The pH value of regulating step (1) acquired solution is 5, and upper molecular sieve chromatography is flowed with 0.5mL/min
Speed absorption first removes water-solubility impurities and the macromolecular components such as carbohydrates with 3 times of column volume amount water elutions, then with 3 times of amounts of column volume
Ethanol water elutes molecular sieve chromatography, collects the high eluent of dihydromyricetin cellulose content, is concentrated to give dihydromyricetin,
Purity is 90%.
In step (1), the volume fraction of ethanol water used in extraction is 70%.
In step (1), the solid-liquid ratio 1 of extraction:9, unit kg/L.
In step (1), the time of standing is 12h.
In step (1), the volume fraction of ethanol water used in dissolving is 60%.
In step (2), the volume fraction of ethanol water used in elution is 90%.
In step (2), the molecular sieve is ZSM type molecular sieves.
In step (2), molecular sieve used carries out pre-treatment：ZSM type molecular sieves are placed in Muffle furnace, 600 DEG C of high-temperature calcinations
4h, removal of impurities.
Embodiment 3
A kind of method that dihydromyricetin is extracted from ampelopsis grossdentata, comprises the following steps：
(1) using ampelopsis grossdentata leaf, stem as raw material, extracted with water or ethanol water, 70-80 DEG C of Extracting temperature, while hot
Filtering repeats extraction 2 times, obtains crude extract；
Crude extract is concentrated into 4 times of raw material weight, is cooled to 10 DEG C, stands, pours out solution, lower floor's solid is steamed with room temperature
Distilled water is cleaned 3 times, and solid is dissolved with ethanol water, obtains solution；
(2) isolate and purify：The pH value of regulating step (1) acquired solution is 7, and upper molecular sieve chromatography is flowed with 1.0mL/min
Speed absorption first removes water-solubility impurities and the macromolecular components such as carbohydrates with 3 times of column volume amount water elutions, then with 3 times of amounts of column volume
Ethanol water elutes molecular sieve chromatography, collects the high eluent of dihydromyricetin cellulose content, is concentrated to give dihydromyricetin,
Purity is 88%.
In step (1), the volume fraction of ethanol water used in extraction is 80%.
In step (1), the solid-liquid ratio 1 of extraction:12, unit kg/L.
In step (1), the time of standing is 12h.
In step (1), the volume fraction of ethanol water used in dissolving is 60%.
In step (2), the volume fraction of ethanol water used in elution is 90%.
In step (2), the molecular sieve is ZSM type molecular sieves.
In step (2), molecular sieve used carries out pre-treatment：ZSM type molecular sieves are placed in Muffle furnace, 600 DEG C of high-temperature calcinations
4h, removal of impurities.
Claims (10)
- A kind of 1. method that dihydromyricetin is extracted from ampelopsis grossdentata, which is characterized in that comprise the following steps：(1) using ampelopsis grossdentata leaf, stem as raw material, being extracted with water or ethanol water, 50-90 DEG C of Extracting temperature filters while hot, Extraction 2-3 times is repeated, obtains crude extract；Crude extract is concentrated into 3-8 times of raw material weight, is cooled to 0-20 DEG C, stands, pours out solution, lower floor's solid is with normal-temperature water Cleaning 2-3 times, solid is dissolved with ethanol water, obtains solution；(2) isolate and purify：The pH value of regulating step (1) acquired solution be 5-7, upper molecular sieve chromatography, with 0.5-1.0mL/min Flow velocity adsorbs, and is first eluted with water and removes water-solubility impurities and the macromolecular components such as carbohydrate, then with ethanol water to molecular sieve layer Analysis column is eluted, and is collected the high eluent of dihydromyricetin cellulose content, is concentrated to give dihydromyricetin, purity 85-93%.
- 2. the method according to claim 1 that dihydromyricetin is extracted from ampelopsis grossdentata, which is characterized in that step (1) in, the volume fraction of ethanol water used in extraction is 30-80%.
- 3. the method according to claim 1 or 2 that dihydromyricetin is extracted from ampelopsis grossdentata, which is characterized in that step Suddenly in (1), the solid-liquid ratio 1 of extraction:6-15, unit kg/L.
- 4. the method according to claim 1 or 2 that dihydromyricetin is extracted from ampelopsis grossdentata, which is characterized in that step Suddenly in (1), the time of standing is 10-20h.
- 5. the method according to claim 1 or 2 that dihydromyricetin is extracted from ampelopsis grossdentata, which is characterized in that step Suddenly in (1), the volume fraction of ethanol water used in dissolving is 30-60%.
- 6. the method according to claim 1 or 2 that dihydromyricetin is extracted from ampelopsis grossdentata, which is characterized in that step Suddenly in (2), water elution removing water-solubility impurity and macromolecular components are measured for 2.5-4.0 times with column volume.
- 7. the method according to claim 1 or 2 that dihydromyricetin is extracted from ampelopsis grossdentata, which is characterized in that step Suddenly in (2), measure ethanol water with 2.5-4.0 times of column volume and molecular sieve chromatography is eluted.
- 8. the method according to claim 1 or 2 that dihydromyricetin is extracted from ampelopsis grossdentata, which is characterized in that step Suddenly in (2), the volume fraction of ethanol water used in elution is 90-95%.
- 9. the method according to claim 1 or 2 that dihydromyricetin is extracted from ampelopsis grossdentata, which is characterized in that step Suddenly in (2), the molecular sieve is any one in Y types, ZSM types, A type molecular sieve.
- 10. the method according to claim 1 or 2 that dihydromyricetin is extracted from ampelopsis grossdentata, which is characterized in that step Suddenly in (2), molecular sieve used carries out pre-treatment：Molecular sieve is placed in Muffle furnace, 600 ± 50 DEG C of 4 ± 1h of high-temperature calcination, removal of impurities.
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| CN201810074897.0A CN108047184A (en) | 2018-01-25 | 2018-01-25 | A kind of method that dihydromyricetin is extracted from ampelopsis grossdentata |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109305954A (en) * | 2018-11-21 | 2019-02-05 | 中南民族大学 | A method of isolating and purifying dihydromyricetin from vine tea |
| CN111072618A (en) * | 2019-12-17 | 2020-04-28 | 华南农业大学 | Method for conveniently and rapidly purifying dihydromyricetin from Ampelopsis grossedentata leaves |
| CN111892566A (en) * | 2019-05-05 | 2020-11-06 | 首都医科大学 | Ampelopsis grossedentata water extract, preparation method thereof and application of water extract as acetylcholinesterase inhibitor |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1393443A (en) * | 2001-06-29 | 2003-01-29 | 张友胜 | Process for preparing dihydromyricetin from porcelain ampelopsis |
| CN1477104A (en) * | 2003-07-11 | 2004-02-25 | 上海奥利实业有限公司 | Extraction and purification method of licoflavone |
| CN101824018A (en) * | 2010-04-30 | 2010-09-08 | 韩山师范学院 | Method for purifying dihydromyricetin |
| 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 |
-
2018
- 2018-01-25 CN CN201810074897.0A patent/CN108047184A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1393443A (en) * | 2001-06-29 | 2003-01-29 | 张友胜 | Process for preparing dihydromyricetin from porcelain ampelopsis |
| CN1477104A (en) * | 2003-07-11 | 2004-02-25 | 上海奥利实业有限公司 | Extraction and purification method of licoflavone |
| CN101824018A (en) * | 2010-04-30 | 2010-09-08 | 韩山师范学院 | Method for purifying dihydromyricetin |
| 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 |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109305954A (en) * | 2018-11-21 | 2019-02-05 | 中南民族大学 | A method of isolating and purifying dihydromyricetin from vine tea |
| CN111892566A (en) * | 2019-05-05 | 2020-11-06 | 首都医科大学 | Ampelopsis grossedentata water extract, preparation method thereof and application of water extract as acetylcholinesterase inhibitor |
| CN111072618A (en) * | 2019-12-17 | 2020-04-28 | 华南农业大学 | Method for conveniently and rapidly purifying dihydromyricetin from Ampelopsis grossedentata leaves |
| CN111072618B (en) * | 2019-12-17 | 2023-09-05 | 华南农业大学 | Method for conveniently and rapidly purifying dihydromyricetin from self-display ampelopsis grossedentata leaves |
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Application publication date: 20180518 |