CN108101924A - A kind of method that ellagic acid is extracted in the hair shell from Chinese chestnut - Google Patents
A kind of method that ellagic acid is extracted in the hair shell from Chinese chestnut Download PDFInfo
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- CN108101924A CN108101924A CN201810006407.3A CN201810006407A CN108101924A CN 108101924 A CN108101924 A CN 108101924A CN 201810006407 A CN201810006407 A CN 201810006407A CN 108101924 A CN108101924 A CN 108101924A
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- C07—ORGANIC CHEMISTRY
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- C07D493/00—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system
- C07D493/02—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system in which the condensed system contains two hetero rings
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Abstract
From Chinese chestnut hair shell with ethanol water or alkaline solution it is Extraction medium the present invention provides one kind, uses the method for microwave radiation exaraction ellagic acid.Under microwave radiation technology, with different Extraction mediums, within 16 minutes, the recovery rate of ellagic acid is extracted up to 2.644mg/g (ethanol water) and 3.794mg/g (buck) from Chinese chestnut hair shell.This method, which realizes, fast and efficiently extracts ellagic acid, provides a new process that ellagic acid is extracted from Chinese chestnut hair shell.
Description
Technical field
From Chinese chestnut hair shell with ethanol water or alkaline solution it is Extraction medium the present invention provides one kind, use is micro-
The method of ripple assisted extraction ellagic acid.Belong to field of natural compound extraction.
Background technology
Chinese chestnut, which plants oneself, the history of more than 3000 years, and the cultivated area of China Chinese chestnut and yield rapidly increase in recent years.From
Increased year by year with average annual 10% yield since 2006, by the end of 2016, China's Chinese chestnut gross annual output amount was accounted for up to 1,000,000 tons
The 65%-70% of world's Chinese chestnut total output.With the fast development of world chestnut industry, except Chinese chestnut Seed is largely used to varieties of food items
Outside, the utilization of other Chinese chestnut by-products is extremely limited, and most of Chinese chestnut hair shells and inner skin of Chinese chestnut are by as production rubbish
It discards or is burned off.Both the huge wasting of resources had been caused, also as serious environmental problem.
It is reported that in Chinese chestnut hair shell containing gallic acid, ellagic acid, shikimic acid, Quercetin, former catechin, oleanolic acid,
A variety of polyphenol components such as malol.Plant polyphenol proves by medical research as a kind of important bioactive ingredients,
Metabolic condition can be improved, reduce the incidence of cardiovascular and cerebrovascular disease, while in the side such as antitumor, antiviral, anti-aging
Face has good effect.And natural polyphenol also has extremely strong antioxidation activity, while preventing blood fat from raising, can increase
The content of high-density lipoprotein.Therefore, natural polyphenol class substance can be used as natural additive for foodstuff, improve food
Quality enhances the antioxygenic property of food.
Ellagic acid is a kind of native compound with polyphenol structure, is detected through analysis, it is found that ellagic acid is Chinese chestnut polyphenol
A kind of main component, therefore, the primary content for effectively utilizing chestnut be exactly from Chinese chestnut hair shell in extracting and developing it is high-purity
Spend ellagic acid.Carried out around extracting and purifying ellagic acid, the Qinling Mountains etc. in Chinese chestnut hair shell using the mode of ultrasonic wave assisted extraction
Extract related work (application of the castanea mollissima blume ellagitannin in antioxidant is prepared, CN103610212A [P] .2014), Shi En
Intelligent grade also uses ultrasonic wave assisted extraction method to carry out extraction as main extracting method and separated relevant work, is being separated
Amberlyst process (extraction, purifying and its antioxygenic property research [D] Beijing of the intelligent Chinese chestnut involucres polyphenol of stone grace is used during purifying
Agricultural college, 2013.).
But in the above-mentioned work carried out, except using common distillation extraction and macroporous resin purification, for
Ellagic acid to high-purity is still inefficient or complex process, and time-consuming in extraction process, and solvent-oil ratio is big.
The present invention devises a kind of significantly more efficient extracting method, by the use of alcohol water or buck as Extraction medium, uses Microwave-assisted Extraction
Ellagic acid is taken, obtains higher yield.
The content of the invention：
The purpose of the present invention is being soluble in polar solvent using polyphenols, using efficient microwave radiation technology, exploitation one
The method that kind efficiently, rapidly extracts ellagic acid from Chinese chestnut hair shell.
Using microwave radiation exaraction, the method for ellagic acid is extracted from Chinese chestnut hair shell to be included：
A. the Chinese chestnut hair shell of collection is crushed using pulverizer, sieving, the rice-chestnut powder for removing large particulate matter is placed in refrigerator
It refrigerates spare.
B. a certain amount of Chinese chestnut hair shell powder, ethanol water or certain density alkali using 50% -90% are weighed
Aqueous solution dissolves according to solid-liquid ratio 1/10-1/25 and impregnates 1-30hr.
C. above-mentioned soak is placed in microwave reactor to extract, 65 DEG C -80 DEG C of Extracting temperature, extraction time 4-
16min, the solution that extraction is finished cool down, and filter off filter residue, obtain Chinese chestnut hair shell extracting solution.
D. extracting solution is evaporated, is recrystallized with methanol, accurate quantification is carried out by high performance liquid chromatography (HPLC).
The Chinese chestnut hair extracting solution of shell and the test solution of ellagic acid sterling are prepared, is analyzed by HPLC, utilizes ellagic acid
Standard curve, is calculated the recovery rate of ellagic acid, and chromatogram is shown in attached drawing.The chromatographic condition used for： Waters 515-
717-996 high performance liquid chromatographs, chromatographic column are Agilent Eclipse Plus C18 (4.6mm × 250mm, 5 μm), are flowed
It is dynamic mutually for the formic acid solution of methanol -0.1% gradient elution (0min, 15:85 v/v；10min, 30:70v/v；15min, 45:55v/
v；18min, 65:35v/v；30min, 15:85 v/v；40min, 15:85v/v), flow velocity 1.0mL/min, Detection wavelength are
254nm, 10 μ L of sample size, column temperature is room temperature.
The present invention achieves following achievement：
1st, 3.794mg/g is reached using the amount of microwave radiation exaraction ellagic acid, extraction time was foreshortened within 20 minutes.
2nd, using alcohol water or buck, reduce the use of organic reagent, reduce cost.
3rd, it is a kind of environmental-friendly extracting method The method reduces the discharge of waste water and waste liquid.
Description of the drawings
Fig. 1 Chinese chestnuts hair shell alcohol water extract HPLC spectrograms.
Fig. 2 Chinese chestnuts hair shell buck extractive HPLC spectrogram.
Fig. 3 ellagic acid standard curves
Specific embodiment：
Below in conjunction with the accompanying drawings with specific embodiment to the method for extraction ellagic acid in a kind of hair shell from Chinese chestnut of the present invention
It further illustrates, so that those skilled in the art becomes more apparent upon the present invention, but the present invention is not limited with this.
Embodiment 1：
A. the Chinese chestnut hair shell of collection is crushed using pulverizer, after crushing, powder is sieved, removes large particulate matter, it will
It is spare that Chinese chestnut hair shell powder under sieve is placed in refrigerator cold-storage.
B. Chinese chestnut hair shell powder 2g is accurately weighed, is dissolved and impregnated according to solid-liquid ratio 1/20 using 80% ethanol water.
By above-mentioned solution under conditions of microwave 400W, 70 DEG C of heating temperature, 12min is extracted, extracting solution cooled and filtered is removed and is filtered
Slag obtains Chinese chestnut hair shell extracting solution.
C. extracting solution is evaporated, is redissolved using methanol, and is recrystallized, is quantified by HPLC, the extracted amount of ellagic acid is
2.644mg/g.
Embodiment 2：
A. the Chinese chestnut hair shell of collection is crushed using pulverizer, after crushing, powder is sieved, removes large particulate matter, it will
It is spare that Chinese chestnut powder under sieve is placed in refrigerator cold-storage.
B. Chinese chestnut powder 2g is accurately weighed, is dissolved and impregnated according to solid-liquid ratio 1/10 using 50% ethanol water.It will be upper
Solution is stated under conditions of microwave 400W, 65 DEG C of heating temperature, extracts 4min, extracting solution cooled and filtered is removed into filter residue to obtain the final product
To Chinese chestnut hair shell extracting solution.
C. extracting solution is evaporated, is redissolved using methanol, and is recrystallized, is quantified by HPLC, the extracted amount of ellagic acid is
1.240mg/g.
Embodiment 3：
A. the Chinese chestnut hair shell of collection is crushed using pulverizer, after crushing, powder is sieved, removes large particulate matter, it will
It is spare that Chinese chestnut powder under sieve is placed in refrigerator cold-storage.
B. Chinese chestnut powder 2g is accurately weighed, is dissolved and impregnated according to solid-liquid ratio 1/25 using 90% ethanol water.It will be upper
Solution is stated under conditions of microwave 400W, 80 DEG C of heating temperature, extracts 12min, is by extracting solution cooled and filtered removing filter residue
Obtain Chinese chestnut hair shell extracting solution.
C. extracting solution is evaporated, is redissolved using methanol, and is recrystallized, is quantified by HPLC, the extracted amount of ellagic acid is
2.102mg/g.
Embodiment 4：
A. the Chinese chestnut hair shell of collection is crushed using pulverizer, after crushing, powder is sieved, removes large particulate matter, it will
It is spare that Chinese chestnut powder under sieve is placed in refrigerator cold-storage.
B. Chinese chestnut powder 2g is accurately weighed, is dissolved and impregnated according to solid-liquid ratio 1/20 using 60% ethanol water.It will be upper
Solution is stated under conditions of microwave 400W, 80 DEG C of heating temperature, extracts 4min, extracting solution cooled and filtered is removed into filter residue to obtain the final product
To Chinese chestnut hair shell extracting solution.
C. extracting solution is evaporated, is redissolved using methanol, and is recrystallized, is quantified by HPLC, the extracted amount of ellagic acid is
2.126mg/g.
Embodiment 5：
A. the Chinese chestnut hair shell of collection is crushed using pulverizer, after crushing, powder is sieved, removes large particulate matter, it will
It is spare that Chinese chestnut powder under sieve is placed in refrigerator cold-storage.
B. Chinese chestnut powder 2g is accurately weighed, is dissolved and impregnated according to solid-liquid ratio 1/15 using 80% ethanol water.It will be upper
Solution is stated under conditions of microwave 400W, 75 DEG C of heating temperature, extracts 4min, extracting solution cooled and filtered is removed into filter residue to obtain the final product
To Chinese chestnut hair shell extracting solution.
C. extracting solution is evaporated, is redissolved using methanol, and is recrystallized, is quantified by HPLC, the extracted amount of ellagic acid is
2.262mg/g.
Embodiment 6：
A. the Chinese chestnut hair shell of collection is crushed using pulverizer, after crushing, powder is sieved, removes large particulate matter, it will
It is spare that Chinese chestnut powder under sieve is placed in refrigerator cold-storage.
B. Chinese chestnut powder 2g is accurately weighed, is dissolved and impregnated according to solid-liquid ratio 1/20 using 70% ethanol water.It will be upper
Solution is stated under conditions of microwave 400W, 80 DEG C of heating temperature, extracts 8min, extracting solution cooled and filtered is removed into filter residue to obtain the final product
To Chinese chestnut hair shell extracting solution.
C. extracting solution is evaporated, is redissolved using methanol, and is recrystallized, is quantified by HPLC, the extracted amount of ellagic acid is
2.514mg/g.
Embodiment 7：
A. the Chinese chestnut hair shell of collection is crushed using pulverizer, after crushing, powder is sieved, removes large particulate matter, it will
It is spare that Chinese chestnut powder under sieve is placed in refrigerator cold-storage.
B. Chinese chestnut powder 2g is accurately weighed, is dissolved and impregnated according to solid-liquid ratio 1/25 using the NaOH aqueous solutions that pH is 9.5.It will
Above-mentioned solution extracts 16min under conditions of microwave 400W, 80 DEG C of heating temperature, and extracting solution cooled and filtered is removed filter residue
Obtain Chinese chestnut hair shell extracting solution.
C. extracting solution pH is adjusted to acidity, extracting solution is evaporated, is redissolved using methanol, and is recrystallized, and is determined by HPLC
Amount, the extracted amount of ellagic acid is 2.738mg/g.
Embodiment 8：
A. the Chinese chestnut hair shell of collection is crushed using pulverizer, after crushing, powder is sieved, removes large particulate matter, it will
It is spare that Chinese chestnut powder under sieve is placed in refrigerator cold-storage.
B. Chinese chestnut powder 2g is accurately weighed, is dissolved and impregnated according to solid-liquid ratio 1/25 using the NaOH aqueous solutions that PH is 12.It will
Above-mentioned solution extracts 16min under conditions of microwave 400W, 80 DEG C of heating temperature, and extracting solution cooled and filtered is removed filter residue
Obtain Chinese chestnut hair shell extracting solution.
C. extracting solution pH is adjusted to acidity, extracting solution is evaporated, is redissolved using methanol, and is recrystallized, and is determined by HPLC
Amount, the extracted amount of ellagic acid is 3.794mg/g.
Embodiment 9：
A. the Chinese chestnut hair shell of collection is crushed using pulverizer, after crushing, powder is sieved, removes large particulate matter, it will
It is spare that Chinese chestnut powder under sieve is placed in refrigerator cold-storage.
B. Chinese chestnut powder 2g is accurately weighed, is dissolved and impregnated according to solid-liquid ratio 1/25 using the KOH aqueous solutions that PH is 12.It will be upper
Solution is stated under conditions of microwave 400W, 80 DEG C of heating temperature, extracts 16min, is by extracting solution cooled and filtered removing filter residue
Obtain Chinese chestnut hair shell extracting solution.
C. extracting solution pH is adjusted to acidity, extracting solution is evaporated, is redissolved using methanol, and is recrystallized, and is determined by HPLC
Amount, the extracted amount of ellagic acid is 3.456mg/g.
Embodiment 9：
A. the Chinese chestnut hair shell of collection is crushed using pulverizer, after crushing, powder is sieved, removes large particulate matter, it will
It is spare that Chinese chestnut powder under sieve is placed in refrigerator cold-storage.
B. Chinese chestnut powder 2g is accurately weighed, uses the Na that PH is 122CO3Aqueous solution is dissolved according to solid-liquid ratio 1/25 and impregnated.It will
Above-mentioned solution extracts 16min under conditions of microwave 400W, 80 DEG C of heating temperature, and extracting solution cooled and filtered is removed filter residue
Obtain Chinese chestnut hair shell extracting solution.
C. extracting solution pH is adjusted to acidity, extracting solution is evaporated, is redissolved using methanol, and is recrystallized, and is determined by HPLC
Amount, the extracted amount of ellagic acid is 2.361mg/g.
Embodiment 10：
A. the Chinese chestnut hair shell of collection is crushed using pulverizer, after crushing, powder is sieved, removes large particulate matter, it will
It is spare that Chinese chestnut powder under sieve is placed in refrigerator cold-storage.
B. Chinese chestnut powder 2g is accurately weighed, uses the K that PH is 122CO3Aqueous solution is dissolved according to solid-liquid ratio 1/25 and impregnated.It will
Above-mentioned solution extracts 16min under conditions of microwave 400W, 80 DEG C of heating temperature, and extracting solution cooled and filtered is removed filter residue
Obtain Chinese chestnut hair shell extracting solution.
C. extracting solution pH is adjusted to acidity, extracting solution is evaporated, is redissolved using methanol, and is recrystallized, and is determined by HPLC
Amount, the extracted amount of ellagic acid is 3.712mg/g.
Claims (6)
1. the method for ellagic acid is extracted in a kind of hair shell from Chinese chestnut, it is characterised in that：
A. the Chinese chestnut hair shell of collection is crushed using pulverizer, sieving, the rice-chestnut powder for removing large particulate matter is placed in refrigerator cold-storage
It is spare.
B. a certain amount of Chinese chestnut hair shell powder is weighed, it is molten using a certain proportion of ethanol water or certain density buck
Liquid dissolves according to solid-liquid ratio 1/10-1/25 and impregnates 1-30hr.
C. above-mentioned soak is placed in microwave reactor to extract, 65 DEG C -80 DEG C, extraction time 4-16min of Extracting temperature,
The solution cooling finished will be extracted, filter off filter residue, obtain Chinese chestnut hair shell extracting solution.
D. extracting solution is evaporated, is recrystallized with methanol, accurate quantification is carried out by high performance liquid chromatography.
2. the method for ellagic acid is extracted in a kind of hair shell from Chinese chestnut according to claim 1, it is characterised in that：Extraction process
Middle ethyl alcohol water concentration may be selected to be 50%-90%, be preferably 80%.
3. the method for ellagic acid is extracted in a kind of hair shell from Chinese chestnut according to claim 1, it is characterised in that：Aqueous alkali
Sodium hydrate aqueous solution, potassium hydroxide aqueous solution, aqueous sodium carbonate, wet chemical etc., preferably hydrogen-oxygen may be selected
Change sodium water solution；9.5-13 may be selected in sodium hydrate aqueous solution pH, is preferably that pH is 12.
4. the method for ellagic acid is extracted in a kind of hair shell from Chinese chestnut according to claim 1, it is characterised in that：Extraction process
Middle Chinese chestnut hair shell/ethanol water solid-liquid ratio is 1/10-1/25, is preferably 1/15.
5. the method for ellagic acid is extracted in a kind of hair shell from Chinese chestnut according to claim 1, it is characterised in that：Extracting temperature
It it is preferably 70 DEG C for 65 DEG C -80 DEG C.
6. the method for ellagic acid is extracted in a kind of hair shell from Chinese chestnut according to claim 1, it is characterised in that：Microwave Extraction
Time is 4min-16min, is preferably 12min.
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| CN201810006407.3A CN108101924A (en) | 2018-01-03 | 2018-01-03 | A kind of method that ellagic acid is extracted in the hair shell from Chinese chestnut |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109810116A (en) * | 2019-02-26 | 2019-05-28 | 北京理工大学 | A method of ellagic acid in purifying Chinese chestnut hair shell extracting solution |
| CN109810117A (en) * | 2019-02-26 | 2019-05-28 | 北京理工大学 | A kind of method that subcritical abstraction method extracts ellagic acid from chestnut shell |
| CN114605427A (en) * | 2022-03-25 | 2022-06-10 | 大连理工大学盘锦产业技术研究院 | Method for extracting and preparing raspberry ellagic acid |
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| CN103610212A (en) * | 2013-12-05 | 2014-03-05 | 北京农学院 | Application of castanea mollissima blume ellagitannin in preparing antioxidant |
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2018
- 2018-01-03 CN CN201810006407.3A patent/CN108101924A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103610212A (en) * | 2013-12-05 | 2014-03-05 | 北京农学院 | Application of castanea mollissima blume ellagitannin in preparing antioxidant |
Non-Patent Citations (2)
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| 乔延江: "《中华医学百科全书 中药制剂学》", 30 April 2017, 中国协和医科大学出版社 * |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109810116A (en) * | 2019-02-26 | 2019-05-28 | 北京理工大学 | A method of ellagic acid in purifying Chinese chestnut hair shell extracting solution |
| CN109810117A (en) * | 2019-02-26 | 2019-05-28 | 北京理工大学 | A kind of method that subcritical abstraction method extracts ellagic acid from chestnut shell |
| CN109810116B (en) * | 2019-02-26 | 2021-06-04 | 北京理工大学 | Method for purifying ellagic acid in chestnut shell extracting solution |
| CN114605427A (en) * | 2022-03-25 | 2022-06-10 | 大连理工大学盘锦产业技术研究院 | Method for extracting and preparing raspberry ellagic acid |
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