CN106831354A - A kind of method that Chinese cassia tree slag prepares polyphenol - Google Patents
A kind of method that Chinese cassia tree slag prepares polyphenol Download PDFInfo
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- CN106831354A CN106831354A CN201510881175.2A CN201510881175A CN106831354A CN 106831354 A CN106831354 A CN 106831354A CN 201510881175 A CN201510881175 A CN 201510881175A CN 106831354 A CN106831354 A CN 106831354A
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- chinese cassia
- cassia tree
- polyphenol
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- tree slag
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C37/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
- C07C37/004—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring by obtaining phenols from plant material or from animal material
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Abstract
The invention discloses a kind of method that Chinese cassia tree slag prepares polyphenol, comprise the following steps：（1）Chinese cassia tree slag dry powder is mixed with ethanol, is stirred, extraction stands, filters, extraction, combining extraction liquid, evaporation drying；（2）By step（1）The product of acquisition mixes with petroleum ether, and extraction, supernatant simultaneously reclaims petroleum ether；Extract is added into ethyl acetate, is extracted, merged supernatant and evaporate ethyl acetate, freeze-drying obtains Chinese cassia tree slag polyphenol crude extract after solid frozen.The cinnamon polyphenol extract is extracted from Chinese cassia tree slag, and preparation method is simple, and extraction efficiency is high, low production cost, safe, is suitable to industrialized production.
Description
Technical field
The invention belongs to the preparing technical field of polyphenol, and in particular to be a kind of method that Chinese cassia tree slag prepares polyphenol.
Background technology
Polyphenols refers to the vegetable phenol with multiple phenolic hydroxyl groups in molecule.There is very high content in Chinese cassia tree slag fruit
Natural polyphenol class compound, plant polyphenol has very strong oxidation resistance, is the anti-of vitamin C under same dose
20 times of oxidability, therefore the oxygen radical in human body can be effectively removed, so as to reduce oxygen radical to normal cell
Destruction, play a protective role.Polyphenol compound can also prevent formation of the potential carcinogenicity material in human body simultaneously
And aggregation, improving metabolism, protective effect on cancer risk is notable.In addition the polyphenols of some special constructions has in Chinese cassia tree slag fruit
Some special effects.
Application of the polyphenol in food industry is of increasing concern, therefore to the research and development of this natural materials of polyphenol
It is more and more eager just to seem.Although polyphenols is widely present in plant derived foods, but its containing in different food products
Amount and structure have very big difference.And the content of polyphenol can be affected by various factors in plant, such as fruit and vegetables into
Temperature of ripe degree, storage condition and food processing process etc..Want to supplement polyphenol at present, can only be obtained by way of diet.
Plant polyphenol is water-soluble and methyl alcohol, ethanol, ethyl acetate, acetone and other organic solvent, insoluble in chloroform, in acidity
Stabilization, the oxidizable brown stain in alkaline medium in medium.The method of the extraction of current state's polyphenol crude product mainly has water and organic molten
Agent extraction method, supercritical fluid extraction, ultrasonic-leaching method, microwave digestion method ion catch electron microscopy, resin adsorption partition method,
The methods such as cryogenic purincation enzyme process.The advantage of solvent extraction method is easy to operate, it is not necessary to complicated instrument and equipment.Extracted with water
Compare, organic solvent extraction energy consumption is smaller, extraction rate is higher, and can effectively reduce the denaturation of polyphenol in leaching process, but
The residual of organic solvent and the stress problems to environment govern the extensive use of the method always.Various organic solvents are had at present
Be used for the extraction of plant polyphenol, wherein using it is most be ethanol.Using this kind of extractant, polyphenol oxidase can be delayed,
The preparation rate of polyphenol is improve to a certain extent, and it is safer compared to other organic solvents cheap.
At present, isolating and purifying for Chinese cassia tree polyphenol components studies disclosed data seldom, without suitable industrialized production
Data.
The content of the invention
The purpose of the present invention is to overcome the deficiencies in the prior art, there is provided a kind of method that Chinese cassia tree slag prepares polyphenol.
Technical scheme is summarized as follows：
A kind of method that Chinese cassia tree slag prepares polyphenol, comprises the following steps：
（1）The Chinese cassia tree slag dry powder of 150g is mixed with the ethanol of 700-800mL in proportion, is stirred, extract 3-5h, stand,
Filtering, extracts 1-3 times, combining extraction liquid, by the extract in 35-45 DEG C of evaporation drying；
（2）It is in proportion 1g：The ratio of 4-6mL, by step（1）The product of acquisition mixes with petroleum ether, extracts 2-4 times,
Merge supernatant and reclaim petroleum ether；It is in proportion 1g：Extract is added ethyl acetate by the ratio of 4-6mL, extracts 2-
4 times, merge supernatant in 35-45 DEG C of evaporation, evaporate ethyl acetate, to obtain Chinese cassia tree slag polyphenol thick for freeze-drying after solid frozen
Extract.
Method of the present invention process is simple, energy consumption is low, and separation condition is gentle, sample recovery rate is high, experimental result reappearance
High, simple equipments economy.
Specific embodiment
Embodiments of the invention be in order that those skilled in the art better understood when the present invention, can not be to this
Invention is imposed any restrictions.
With reference to specific embodiment, the present invention is further illustrated.
Embodiment 1
A kind of method that Chinese cassia tree slag prepares polyphenol, comprises the following steps：
（1）The Chinese cassia tree slag dry powder of 150g is mixed with the ethanol of 750mL in proportion, is stirred, extract 4h, stood, filter,
Extraction 2 times, combining extraction liquid, by extract in 40 DEG C of evaporation dryings；The ethanol is that volume ratio is 99.0：1.0 first
Alcohol and concentrated hydrochloric acid mixed liquor；
（2）It is in proportion 1g：The ratio of 5mL, by step（1）The product of acquisition mixes with petroleum ether, extracts 3 times, in merging
Clear liquid simultaneously reclaims petroleum ether；It is in proportion 1g：Extract is added ethyl acetate by the ratio of 5mL, is extracted 3 times, is merged
Supernatant evaporates ethyl acetate in 40 DEG C of evaporations, and freeze-drying obtains Chinese cassia tree slag polyphenol crude extract after solid frozen.Recovery rate
91.2%。
Chinese cassia tree slag polyphenol crude extract can be purified using various known methods, and method below is not made to the present invention
To limit：
（1）In proportion, 100mg Chinese cassia tree slag polyphenol crude extracts are dissolved in 50mL ethanol, with 45 μm of organic membrane filtrations
；
（2）Filtrate is pumped into constant flow pump to be anticipated and in populated AB-8 macroporous absorbent resins, thing solution to be extracted
Termination of pumping 15min during full of resin bed, 35min is rinsed with acidifying distilled water, uses ethanol desorption, when collector exists
Start to occur at 280nm to start to collect eluent during absworption peak until absworption peak terminates；
（3）Repeat step（2）2 times, merge eluent；Eluent in 40 DEG C of evaporations, be evaporated to be unable to re-evaporation and go out methyl alcohol be
Only, freeze at a temperature of -30 DEG C, freeze-drying 24h, obtain purifying Chinese cassia tree slag polyphenol.
Acidifying distilled water is that volume ratio is 99.5：0.5 distilled water and concentrated hydrochloric acid mixed liquor.
Embodiment 2
（1）The Chinese cassia tree slag dry powder of 150g is mixed with the ethanol of 700mL in proportion, is stirred, extract 5h, stood, filter,
Extraction 1 time, by extract in 35 DEG C of evaporation dryings；
（2）It is in proportion 1g：The ratio of 4mL, by step（1）The product of acquisition mixes with petroleum ether, extracts 4 times, merges
Supernatant simultaneously reclaims petroleum ether；It is in proportion 1g：Extract is added ethyl acetate by the ratio of 4mL, is extracted 4 times, is closed
And supernatant evaporates ethyl acetate in 35 DEG C of evaporations, freeze-drying obtains Chinese cassia tree slag polyphenol crude extract after solid frozen.Extract
Rate 89.9%.
Chinese cassia tree slag polyphenol crude extract can be purified using various known methods, and method below is not made to the present invention
To limit：
（1）In proportion, 100mg Chinese cassia tree slag polyphenol crude extracts are dissolved in 45mL ethanol, with 45 μm of organic membrane filtrations
；
（2）Filtrate is pumped into constant flow pump to be anticipated and in populated AB-8 macroporous absorbent resins, thing solution to be extracted
Termination of pumping 10min during full of resin bed, 35min is rinsed with acidifying distilled water, uses ethanol desorption, when collector exists
Start to occur at 280nm to start to collect eluent during absworption peak until absworption peak terminates；
（3）Repeat step（2）2 times, merge eluent；Eluent is evaporated to and is unable to re-evaporation and goes out methyl alcohol in 40 DEG C of evaporations
Untill, freeze at a temperature of -25 DEG C, freeze-drying 28h, obtain purifying Chinese cassia tree slag polyphenol.
Acidifying distilled water is that volume ratio is 99.5：0.5 distilled water and concentrated hydrochloric acid mixed liquor.
Embodiment 3
A kind of method that Chinese cassia tree slag prepares polyphenol, comprises the following steps：
（1）The Chinese cassia tree slag dry powder of 150g is mixed with the ethanol of 800mL in proportion, is stirred, extract 3h, stood, filter,
Extraction 3 times, combining extraction liquid, by extract in 45 DEG C of evaporation dryings；
（2）It is in proportion 1g：The ratio of 6mL, by step（1）The product of acquisition mixes with petroleum ether, extracts 2 times, merges
Supernatant simultaneously reclaims petroleum ether；It is in proportion 1g：Extract is added ethyl acetate by the ratio of 6mL, is extracted 2 times, is closed
And supernatant evaporates ethyl acetate in 45 DEG C of evaporations, freeze-drying obtains Chinese cassia tree slag polyphenol crude extract after solid frozen.Extract
Rate 90.6%.
Chinese cassia tree slag polyphenol crude extract can be purified using various known methods, and method below is not made to the present invention
To limit：
（1）In proportion, 100mg Chinese cassia tree slag polyphenol crude extracts are dissolved in 55mL ethanol, with 45 μm of organic membrane filtrations
；
（2）Filtrate is pumped into constant flow pump to be anticipated and in populated AB-8 macroporous absorbent resins, thing solution to be extracted
Termination of pumping 15min during full of resin bed, 30min is rinsed with acidifying distilled water, uses ethanol desorption, when collector exists
Start to occur at 280nm to start to collect eluent during absworption peak until absworption peak terminates；
（3）Repeat step（2）1 time, merge eluent；Eluent is evaporated to and is unable to re-evaporation and goes out methyl alcohol in 40 DEG C of evaporations
Untill, freeze at a temperature of -35 DEG C, freeze-drying 20h, obtain purifying Chinese cassia tree slag polyphenol.
Acidifying distilled water is that volume ratio is 98.5：1.5 distilled water and concentrated hydrochloric acid mixed liquor.
Claims (1)
1. a kind of method that Chinese cassia tree slag prepares polyphenol, it is characterised in that comprise the following steps：
（1）The Chinese cassia tree slag dry powder of 150g is mixed with the ethanol of 700-800mL in proportion, is stirred, extract 3-5h, stand,
Filtering, extracts 1-3 times, combining extraction liquid, by the extract in 35-45 DEG C of evaporation drying；
（2）It is in proportion 1g：The ratio of 4-6mL, by step（1）The product of acquisition mixes with petroleum ether, extracts 2-4 times,
Merge supernatant and reclaim petroleum ether；It is in proportion 1g：Extract is added ethyl acetate by the ratio of 4-6mL, extracts 2-
4 times, merge supernatant in 35-45 DEG C of evaporation, evaporate ethyl acetate, to obtain Chinese cassia tree slag polyphenol thick for freeze-drying after solid frozen
Extract.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510881175.2A CN106831354A (en) | 2015-12-07 | 2015-12-07 | A kind of method that Chinese cassia tree slag prepares polyphenol |
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| CN201510881175.2A CN106831354A (en) | 2015-12-07 | 2015-12-07 | A kind of method that Chinese cassia tree slag prepares polyphenol |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110642824A (en) * | 2018-06-27 | 2020-01-03 | 鼎赫生物科技股份有限公司 | Method for preparing antioxidant ingredient kaempferol from cortex cinnamomi by hydrolysis technology |
| CN114405055A (en) * | 2021-12-24 | 2022-04-29 | 宁波杰顺生物科技有限公司 | Cinnamon polyphenol extract and preparation method thereof |
-
2015
- 2015-12-07 CN CN201510881175.2A patent/CN106831354A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110642824A (en) * | 2018-06-27 | 2020-01-03 | 鼎赫生物科技股份有限公司 | Method for preparing antioxidant ingredient kaempferol from cortex cinnamomi by hydrolysis technology |
| CN114405055A (en) * | 2021-12-24 | 2022-04-29 | 宁波杰顺生物科技有限公司 | Cinnamon polyphenol extract and preparation method thereof |
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| PB01 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20170613 |
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| WD01 | Invention patent application deemed withdrawn after publication |