CN107353270A - A kind of method that aureusidin is extracted in the skin from water chestnut - Google Patents
A kind of method that aureusidin is extracted in the skin from water chestnut Download PDFInfo
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- CN107353270A CN107353270A CN201710557378.5A CN201710557378A CN107353270A CN 107353270 A CN107353270 A CN 107353270A CN 201710557378 A CN201710557378 A CN 201710557378A CN 107353270 A CN107353270 A CN 107353270A
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- water chestnut
- aureusidin
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- extracted
- water
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D307/00—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
- C07D307/77—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D307/78—Benzo [b] furans; Hydrogenated benzo [b] furans
- C07D307/82—Benzo [b] furans; Hydrogenated benzo [b] furans with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to carbon atoms of the hetero ring
- C07D307/83—Oxygen atoms
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- Medicines Containing Plant Substances (AREA)
Abstract
The invention belongs to Nature inorganic bone technical field, the method for extraction aureusidin in more particularly to a kind of skin from water chestnut, including following preparation process：1) water chestnut skin is dried, crushes, obtain water chestnut skin powder；2) ethanol solution of 15 20 times of water chestnut skin powder weight is added, the HIGH PRESSURE TREATMENT under 30 42MPa, obtains water chestnut latex liquid；3) water chestnut latex liquid is subjected to refluxing extraction once again, adds the deionized water of 6 10 times of water chestnut skin powder weight, refluxing extraction once, merges 2 filtrates；4) centrifuge, take supernatant；5) supernatant is recrystallized with absolute ethyl alcohol；6) wash, dry, obtain finished product.It can be extracted using the inventive method from water chestnut skin, obtain the aureusidin of ultra-high purity.
Description
Technical field
The invention belongs to Nature inorganic bone technical field, the side of aureusidin is extracted in more particularly to a kind of skin from water chestnut
Method.
Background technology
Water chestnut (scientific name：Heleocharis dulcis (Burm.f.) Trin.), also known as horseshoe, Shui Li, black taro, Bodhisattva's shepherd's purse
Deng monocot genus Cyperaceae, being perennial root herbaceous plant.There is elongated root-like stock of crawling, on the top for crawling root-like stock
Hold tuberization, popular leaf water chestnut.Stalk is most, grows thickly, uprightly, cylindric, there is most diaphragms, the existing section in stalk surface after doing, but not
Substantially, celadon, Glabrous.Leaf lacks such as, only has 2-3 leaf sheath in the base portion of stalk；The nearly film quality of sheath, green-yellow, aubergine or
Brown.Small ear basidixed, it is cylindric, there is the hollow no flower of two panels scale in small ear base portion, embrace small ear base portion one week；Remaining scale has entirely
Flower；Compared with the long half as much again of pyrene, there is hangnail；Column cap 3.The wide obovate of pyrene, biconvex shape, top are not hung contracting；Style base is leniently
The hurried stenosis of base portion become flat and triangular in shape.The flowering fruit bearing stage 5-10 months.India is originated in, is widely distributed in the whole world, the China whole nation is each
There is cultivation on ground, is more using subtropical and tropical zones.Water chestnut color of the leather purple is black, and meat is pure white, sweet succulence, clear and melodious tasty, both
Fruit can be done to eat it raw, vegetables can be done again and eaten.Bulb richness starch, eat raw, prepared food or extraction starch, sweet U.S.；Also hyoscine,
Appetizing removing toxic substances, eliminate dyspepsia, is good for stomach.Studies have found that water chestnut skin contains abundant aureusidin.
Aureusidin (Aureusidin), chemistry entitled 4,6,3 ', 4 '-tetrahydroxy aurones, is foremost aurones class
Compound, there are the multiple biological activities such as anti-oxidant, antibacterial, antitumor.Aureusidin structure is special, is distributed in natural plant
It is less, and the content in plant is low, it is difficult to fairly large acquisition.For the ease of studying its pharmacological activity, scholar generally makes
Aureusidin is obtained with the method for synthesis.Changzhou University Hu Kun just reports the total synthesis method of aureusidin, the method with 2,4,
6- trihydroxy-acetophenones and 3,4- 4-dihydroxy benzaldehyde are raw material, react synthesis aureusidin through five steps, its shortcoming is to synthesize
Journey easily entrains the opposite aureusidin isomers of configuration.Compared with synthesizing aureusidin, natural aureusidin avoids synthesis
During the isomers that brings, be considered as more security.People are more biased towards in the natural toad's-mouth of use in actual applications
Element.
Natural aureusidin is present among composite family, Scrophulariaceae, Cyperaceae, Marchantiaceae plant, mainly from sedge
With it is isolated in Marchantiaceae marchantia, natural toad's-mouth in the market is usually from the extract of marchantia.Publication number
Aureusidin in marchantia is purified for CN103030615A Introduction To Cn Patent application superhigh pressure technique and macroporous resin enrichment
Method.This method has that extraction rate is fast, and macroporous resin adsorption is selectively good, and adsorption capacity is big, and separating effect substantially waits spy
Point.But requirement of the superhigh pressure technique that the invention uses to equipment is high, the silica gel used in column chromatography purge process can not repeat profit
With it is too high to result in the cost of production, and raw material marchantia, it is not easy to obtains, hinders the production-scale expansion of aureusidin.Shen
Number it please disclose a kind of water chestnut skin for CN201410834970.1 a patent of invention and extract the method for aureusidin, but be prepared into
The aureusidin purity arrived is also closest to hjolomorphism.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of method that aureusidin is extracted in skin from water chestnut, this method
The aureusidin of ultra-high purity can be prepared.
To achieve the above object, the present invention adopts the following technical scheme that：
The present invention provides a kind of method that aureusidin is extracted in skin from water chestnut, including following preparation process：
1) water chestnut skin is dried, crushes, obtain water chestnut skin powder；
2) ethanol solution of 15-20 times of water chestnut skin powder weight is added, the HIGH PRESSURE TREATMENT under 30-42MPa, obtains water chestnut latex
Liquid；
3) water chestnut latex liquid is subjected to refluxing extraction once again, adds the deionized water of 6-10 times of water chestnut skin powder weight,
Refluxing extraction once, merges 2 filtrates；
4) centrifuge, take supernatant；
5) supernatant is recrystallized with absolute ethyl alcohol；
6) wash, dry, obtain finished product.
Preferably, in step 1) of the present invention, it is crushed to 100-180 mesh.
Preferably, in step 2) of the present invention, the volumetric concentration of ethanol solution is 50-75%.
Preferably, in step 2) of the present invention, HIGH PRESSURE TREATMENT 8-16min.
Preferably, in step 3) of the present invention, the time of each refluxing extraction is all 1-2h.
Preferably, in step 3) of the present invention, the temperature of each refluxing extraction is all 40-60 DEG C.
Preferably, it is of the invention：In the step 4), 10-15min is centrifuged under 4500-6000r/min rotating speeds.
Preferably, in step 5) of the present invention, the volume ratio of supernatant and absolute ethyl alcohol is 1:3-5.
Preferably, in step 6) of the present invention, washed with deionized water.
Compared with prior art, the beneficial effects of the present invention are：
1st, invention is easy to get by the use of the water chestnut skin largely to go out of use as raw material, raw material, aboundresources, is produced into
This is low, turns waste into wealth, lifting water chestnut skin value.
2nd, aureusidin is extracted from water chestnut skin using the inventive method, break-through skill bottleneck, ultra-high purity is prepared
Aureusidin.
3rd, the inventive method operates, simple easily to realize.
Embodiment
The invention will be further described with reference to embodiments, but the invention is not limited in these embodiments.
Embodiment 1
A kind of method that aureusidin is extracted in skin from water chestnut, including following preparation process：
1) water chestnut skin is dried, is crushed to 100 mesh, obtain water chestnut skin powder；
2) volumetric concentration of 17 times of water chestnut skin powder weight is added as 50% ethanol solution, the HIGH PRESSURE TREATMENT under 42MPa
8min, obtain water chestnut latex liquid；
3) water chestnut latex liquid is subjected to refluxing extraction once again, adds the deionized water of 10 times of water chestnut skin powder weight, returned
Stream extraction once, merges 2 filtrates, and time of each refluxing extraction is all that the temperature of 1h and each refluxing extraction is all 60 DEG C；
4) 15min is centrifuged under 4500r/min rotating speeds, takes supernatant；
5) supernatant is recrystallized with the absolute ethyl alcohol of 3-5 times of supernatant volume；
6) washed, dried with deionized water, obtain the aureusidin finished product that content is 99.2%.
Embodiment 2
A kind of method that aureusidin is extracted in skin from water chestnut, including following preparation process：
1) water chestnut skin is dried, is crushed to 120 mesh, obtain water chestnut skin powder；
2) volumetric concentration of 20 times of water chestnut skin powder weight is added as 55% ethanol solution, the HIGH PRESSURE TREATMENT under 39MPa
10min, obtain water chestnut latex liquid；
3) water chestnut latex liquid is subjected to refluxing extraction once again, adds the deionized water of 9 times of water chestnut skin powder weight, flowed back
Extraction once, merges 2 filtrates, and time of each refluxing extraction is all that the temperature of 2h and each refluxing extraction is all 55 DEG C；
4) 13min is centrifuged under 5000r/min rotating speeds, takes supernatant；
5) supernatant is recrystallized with the absolute ethyl alcohol of 5 times of supernatant volume；
6) washed, dried with deionized water, obtain the aureusidin finished product that content is 99.3%.
Embodiment 3
A kind of method that aureusidin is extracted in skin from water chestnut, including following preparation process：
1) water chestnut skin is dried, is crushed to 140 mesh, obtain water chestnut skin powder；
2) volumetric concentration of 18 times of water chestnut skin powder weight is added as 60% ethanol solution, the HIGH PRESSURE TREATMENT under 36MPa
12min, obtain water chestnut latex liquid；
3) water chestnut latex liquid is subjected to refluxing extraction once again, adds the deionized water of 8 times of water chestnut skin powder weight, flowed back
Extraction once, merges 2 filtrates, and time of each refluxing extraction is all that the temperature of 1.5h and each refluxing extraction is all 50 DEG C；
4) 12min is centrifuged under 5500r/min rotating speeds, takes supernatant；
5) supernatant is recrystallized with the absolute ethyl alcohol of 4 times of supernatant volume；
6) washed, dried with deionized water, obtain the aureusidin finished product that content is 99.5%.
Embodiment 4
A kind of method that aureusidin is extracted in skin from water chestnut, including following preparation process：
1) water chestnut skin is dried, is crushed to 100 mesh, obtain water chestnut skin powder；
2) volumetric concentration of 16 times of water chestnut skin powder weight is added as 70% ethanol solution, the HIGH PRESSURE TREATMENT under 33MPa
14min, obtain water chestnut latex liquid；
3) water chestnut latex liquid is subjected to refluxing extraction once again, adds the deionized water of 7 times of water chestnut skin powder weight, flowed back
Extraction once, merges 2 filtrates, and time of each refluxing extraction is all that the temperature of 1h and each refluxing extraction is all 45 DEG C；
4) 11min is centrifuged under 6000r/min rotating speeds, takes supernatant；
5) supernatant is recrystallized with the absolute ethyl alcohol of 3 times of supernatant volume；
6) washed, dried with deionized water, obtain the aureusidin finished product that content is 99.2%.
Embodiment 5
A kind of method that aureusidin is extracted in skin from water chestnut, including following preparation process：
1) water chestnut skin is dried, is crushed to 150 mesh, obtain water chestnut skin powder；
2) volumetric concentration of 15 times of water chestnut skin powder weight is added as 75% ethanol solution, the HIGH PRESSURE TREATMENT under 30MPa
16min, obtain water chestnut latex liquid；
3) water chestnut latex liquid is subjected to refluxing extraction once again, adds the deionized water of 6 times of water chestnut skin powder weight, flowed back
Extraction once, merges 2 filtrates, and time of each refluxing extraction is all that the temperature of 2h and each refluxing extraction is all 40 DEG C；
4) 10min is centrifuged under 4500r/min rotating speeds, takes supernatant；
5) supernatant is recrystallized with the absolute ethyl alcohol of 5 times of supernatant volume；
6) washed, dried with deionized water, obtain the aureusidin finished product that content is 99.3%.
Claims (9)
1. the method for aureusidin is extracted in a kind of skin from water chestnut, it is characterised in that including following preparation process：
1) water chestnut skin is dried, crushes, obtain water chestnut skin powder；
2) ethanol solution of 15-20 times of water chestnut skin powder weight is added, the HIGH PRESSURE TREATMENT under 30-42MPa, obtains water chestnut latex liquid；
3) water chestnut latex liquid is subjected to refluxing extraction once again, adds the deionized water of 6-10 times of water chestnut skin powder weight, flowed back
Extraction once, merges 2 filtrates；
4) centrifuge, take supernatant；
5) supernatant is recrystallized with absolute ethyl alcohol；
6) wash, dry, obtain finished product.
2. the method for aureusidin is extracted in the skin according to claim 1 from water chestnut, it is characterised in that：The step 1)
In, it is crushed to 100-180 mesh.
3. the method for aureusidin is extracted in the skin according to claim 1 from water chestnut, it is characterised in that：The step 2)
In, the volumetric concentration of ethanol solution is 50-75%.
4. the method for aureusidin is extracted in the skin according to claim 3 from water chestnut, it is characterised in that：The step 2)
In, HIGH PRESSURE TREATMENT 8-16min.
5. the method for aureusidin is extracted in the skin according to claim 1 from water chestnut, it is characterised in that：The step 3)
In, the time of each refluxing extraction is all 1-2h.
6. the method for aureusidin is extracted in the skin according to claim 5 from water chestnut, it is characterised in that：The step 3)
In, the temperature of each refluxing extraction is all 40-60 DEG C.
7. the method for aureusidin is extracted in the skin according to claim 1 from water chestnut, it is characterised in that：The step 4)
In, centrifuge 10-15min under 4500-6000r/min rotating speeds.
8. the method for aureusidin is extracted in the skin according to claim 1 from water chestnut, it is characterised in that：The step 5)
In, the volume ratio of supernatant and absolute ethyl alcohol is 1:3-5.
9. the method for aureusidin is extracted in the skin according to claim 1 from water chestnut, it is characterised in that：The step 6)
In, washed with deionized water.
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| CN201710557378.5A CN107353270A (en) | 2017-07-10 | 2017-07-10 | A kind of method that aureusidin is extracted in the skin from water chestnut |
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| CN201710557378.5A CN107353270A (en) | 2017-07-10 | 2017-07-10 | A kind of method that aureusidin is extracted in the skin from water chestnut |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103030615A (en) * | 2012-12-13 | 2013-04-10 | 大兴安岭林格贝有机食品有限责任公司 | Method for preparing aureusidin in liverwort by superhigh pressure technique |
| CN104557824A (en) * | 2014-12-29 | 2015-04-29 | 贺州学院 | Method for extracting aureusidin from eleocharis tuberosa peels |
| CN104592180A (en) * | 2014-12-29 | 2015-05-06 | 贺州学院 | Method for extracting 5-methyl aureusidin from eleocharis tuberosa peels |
-
2017
- 2017-07-10 CN CN201710557378.5A patent/CN107353270A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103030615A (en) * | 2012-12-13 | 2013-04-10 | 大兴安岭林格贝有机食品有限责任公司 | Method for preparing aureusidin in liverwort by superhigh pressure technique |
| CN104557824A (en) * | 2014-12-29 | 2015-04-29 | 贺州学院 | Method for extracting aureusidin from eleocharis tuberosa peels |
| CN104592180A (en) * | 2014-12-29 | 2015-05-06 | 贺州学院 | Method for extracting 5-methyl aureusidin from eleocharis tuberosa peels |
Non-Patent Citations (1)
| Title |
|---|
| 孔令义: "《天然药物化学 第2版》", 31 August 2015, 中国医药科技出版社 * |
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Application publication date: 20171117 |