CN102600216A - Method for extracting plant polyphenol from Chinese chestnut involucre - Google Patents
Method for extracting plant polyphenol from Chinese chestnut involucre Download PDFInfo
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- CN102600216A CN102600216A CN2011104611299A CN201110461129A CN102600216A CN 102600216 A CN102600216 A CN 102600216A CN 2011104611299 A CN2011104611299 A CN 2011104611299A CN 201110461129 A CN201110461129 A CN 201110461129A CN 102600216 A CN102600216 A CN 102600216A
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Abstract
The invention discloses a method for extracting plant polyphenol from Chinese chestnut involucre. The method comprises the following steps of: adding Chinese chestnut involucre powder to an ethanol aqueous solution to obtain an ethanol aqueous dispersion of the Chinese chestnut involucre, carrying out ultrasonic auxiliary extraction on the ethanol aqueous dispersion, centrifuging, carrying out vacuum rotary evaporation on extracting liquid, purifying the concentrated extracting liquid by utilizing macroporous adsorption resin, collecting ethanol eluting liquid, reducing pressure, rotatably evaporating, concentrating and drying to powders to obtain brown Chinese chestnut involucre extract powder. The method for extracting the plant polyphenol from the Chinese chestnut involucre, disclosed by the invention, has the following advantages that the yield of Chinese chestnut involucre extract is high, wherein the content of the plant polyphenol is high, and the quality of the polyphenol is good; and the production process is simple, the operation is simple and convenient, the cost is low, no pollution exists, the extraction ratio is high, and the method is suitable for industrial production. Through the method for extracting the plant polyphenol from the Chinese chestnut involucre, disclosed by the invention, the Chinese chestnut involucre waste, the yield of which is 1.8 times of the yield of the Chinese chestnut, is utilized to the maximum extent, and the additional value of the Chinese chestnut industry is increased; simultaneously, a new natural plant polyphenol antioxidant resource is developed for food and feed industries.
Description
Technical field
A kind of method of extracting plant polyphenol from the Semen Castaneae involucre.
Background technology
Semen Castaneae (castanea mollissina Blume) belongs to Fagaceae (Fagceae) Castanea arbor economic plants, have the laudatory title of " king of dry fruit ", is one of world-renowned dry fruit.China's most of areas all has distribution, especially concentrates with North China and Yangtze river basin cultivation, and output ranks first in the world.In recent years, China's Semen Castaneae output reaches more than 60% of whole world annual production, still increases with the speed in year 11% now.The Semen Castaneae involucre has another name called wind epicarpium Castaneae, Semen Castaneae acorn-cup; Effect with invigorating the spleen and benefiting QI, the strong muscle of the kidney invigorating, powder detoxifcation; Diseases such as treatment erysipelas, toxic swelling, scrofula; The decocting liquid of Semen Castaneae involucre, alcohol soluble substance, ethyl acetate extract have extremely strong antibiotic, antiinflammation and biological activitys such as anticoagulation, leukocyte increasing; Also have antioxidation, anti-aging effects and antidiabetic effect simultaneously, can be used to process natural additive for foodstuff, cosmetics additive and feed additive with disease-resistant growth-promoting effect.Semen Castaneae hair shell aboundresources is with low cost simultaneously, can substitute the use of feeding antibiotic to its development and use.The a large amount of uses in animal husbandry of antibiotic, hormone drugs and chemical synthetic drug bring serious chemical medicinal residue, drug resistance and toxic and side effects, make consumer to present hanging back.Extensively be present in the intravital polyphenol compound of plant and polyphenol is one type, comprise flavanol compound, anthocyanin class, flavonoid, flavonols, phenolic acids, ellagic acid, procyanidin etc., catechin.Exploitation to the Semen Castaneae involucre at present only has Chinese patent CN102140123A to report the method for from Semen Castaneae Li Peng, extracting the ellagic acid tannin; The method discloses the extraction and the Determination on content method thereof of ellagic acid in the tannin; CN102115611A has reported Semen Castaneae bud steam explosion coproduction pigment, tannic extract and process of active carbon; CN101402657A has reported the method for preparing of chestnut shell polyphenol, and CN101407640A has reported the method for distilling of chestnut shell brown pigment.Also do not have but the patent that Semen Castaneae involucre polyphenol extracts is domestic, how to handle these garbages, improve its utilization rate; Realize its circulation industry development, increase traditional Semen Castaneae plant husbandry new growth engines and become new research direction to have excellent development prospect and economic and social benefits; Simultaneously, reduce environmental pollution, improve the added value of Semen Castaneae; Increase peasant's pair income, drive rural economic development.The invention discloses the method for Semen Castaneae involucre polyphenol ultrasonic-assisted extraction,
The good and bad utilization rate that directly influences polyphenol of extraction process, in general, the method for polyphenols mainly contains solvent extraction, ultrasonic assisted extraction method, microwave-assisted extraction method, supercritical CO in the extraction plant commonly used
2Extraction etc.The present invention adopts ultrasonic assisted extraction method, Semen Castaneae involucre polyphenol is extracted, and optimize extraction conditions.In recent years; Utilize the active substance in the ultrasonic extraction plant to obtain good effect, the ultrasonic-assisted extraction technology is to utilize the elastic mechanical vibration wave, cavitation effect, mechanical effect and heat effect three big effects; Destroy plant cell; Solvent is penetrated in the plant cell, thereby quickens the dissolving of plant polyphenol composition, to improve its leaching rate.Existing research shows that ultrasonic technology has begun to be widely used in the extracted form natural plant research field.Ultrasonic-assisted extraction is compared with the water-bath method for distilling; Have that technology is simple, extraction time is short, extract that temperature is low, the response rate is high, oxidation loss is little, during joint, energy-conservation, extraction ratio is high, characteristics such as with low cost, has potential suitability for industrialized production promotional value.Zhang Lihua etc. study the Folium Granati polyphenol extracting method; The result shows; No matter be which kind of adopts extract solvent, the effect of ultrasonic extraction all than water-bath extract effective, be that the extraction ratio of solvent has approximately improved 5% than water-bath extraction ratio wherein with 50% ethanol and 70% acetone.Virot etc. have studied the antioxidant content in the ultrasonic assisted extraction food processing process by-product, compare with traditional method, and ultrasonic auxiliary extraction can significantly improve the product yield, are a kind of method for distilling relatively fast, can substitute traditional method.Anti-oxidation active substance in the ultrasonic assisted extraction Morinda Citifolia of Hemwimol etc. research, with immersion with Suo Shi extracting compare, ultrasonic assisted extraction can improve extraction efficiency.
Summary of the invention
The purpose of this invention is to provide a kind of method of from the Semen Castaneae involucre, extracting polyphenol.
A kind of method of from the Semen Castaneae involucre, extracting polyphenol provided by the invention comprises the steps: said Semen Castaneae involucre powder is added to the ethanol aqueous dispersions that obtains said Semen Castaneae involucre in the ethanol water, said ethanol aqueous dispersions is carried out ultrasonic assisted extraction after; Centrifugal, the rotary evaporation in vacuo lixiviating solution will concentrate lixiviating solution and utilize macroporous adsorbent resin to carry out purification; Collect ethanol elution; Vacuum rotary steam concentrates, and is dried to powder, obtains henna Semen Castaneae involucre extract powder.
In the said method, the granularity of said Semen Castaneae involucre powder is 60 orders.
In the said method, ethanol quality percentage composition is 30%-70% in the said ethanol water, as 40%.
In the said method, the ethanol aqueous dispersions of said Semen Castaneae involucre is liquid material ratio: every 1g Semen Castaneae involucre powder adds the ethanol water of 10-35mL, and liquid material ratio can be 10: 1,15: 1,20: 1 etc.
In the said method, be provided with two factors of ultrasonic temperature and ultrasonic time in the said ultrasonic assisted extraction, wherein ultrasonic temperature is 25 ℃-75 ℃, as, 25 ℃, 35 ℃ etc.; Ultrasonic time is (20-60) min, as, 20min, 30min etc.
In the said method, said centrifugal condition is 4000r/min, 15min.
In the said method, said vacuum is revolved the contract condition of Semen Castaneae involucre polyphenol of inspissation, 0.1MP, 40 ℃.
In the said method, said purification with macroreticular resin polyphenol lixiviating solution promptly is an enrichment process: the polyphenol crude extract is pumped into the good macroporous adsorbent resin of balance that filters out, polyphenol is carried out enrichment; Earlier use the distilled water flushing pillar, reuse 40%-70% ethanol water eluting polyphenol is collected eluent.
Method provided by the invention adopts ultrasonic assisted extraction, has following advantage: (1) utilizes ultrasonic mechanical wave strengthening extraction, does not destroy the active function composition in the medical material, has preserved all active component in the Semen Castaneae involucre.(2) adopt the ethanol atmospheric extraction, safety is good, and operation is simple, and maintaining is convenient; (3) the ultrasonic-assisted extraction technology is to utilize the elastic mechanical vibration wave, and cavitation effect, mechanical effect and heat effect three big effects are destroyed plant cell, and solvent is penetrated in the plant cell, thereby quickens the dissolving of plant polyphenol composition, to improve its leaching rate; (4) have broad spectrum activity, the suitability is wide, but the equal supersound extraction of most each constituents of Chinese crude drug; (5) ultrasonic extraction is little to the character relation of solvent and target extract, and it is many therefore can to supply to extract solvent types, and target is extracted in extensive range; (6) the medicinal raw material treating capacity is big, and effective ingredient is easy to separate, purify; (7) the extraction process cost is low, and the mixed economy effect is remarkable.Macroreticular resin absorbing method has that selectivity is good, adsorption capacity is big, Regeneration Treatment is convenient, absorption rapidly and advantage such as desorbing is easy.
Advantage of the present invention is that (1) leaching process adopts ethanol water, mild condition, and the made polyphenol safety non-toxic that comes out has no injury to human body.(2) technology is simple, cost is low, can be generalized to large-scale commercial production and goes.(4) the polyphenol extraction ratio of Semen Castaneae involucre is high, and has stronger oxidation resistance, removes free radical, simultaneously, antiviral is arranged, antimutagenic, bacteriostasis.
The practical implementation method
Employed experimental technique is conventional method like no specified otherwise among the following embodiment.
Used material, reagent etc. like no specified otherwise, all can have been bought from commercial sources in the following implementation method.
The content of the Semen Castaneae involucre polyphenol extract among the following embodiment of the present invention is measured according to following method: accurately take by weighing 5mg gallic acid standard substance; Standardize solution 50mL; Be made into the titer of 0.1mg/mL; Draw respectively 0.5,1.0,1.5,2.0 and 2.5mL gallic acid titer (0.1mg/mL) be settled to 10mL, be mixed with mass concentration and be 0.005,0.010,0.015,0.020, the standard solution of 0.025mg/mL.Accurately draw above-mentioned titer 0.4mL in the 10mL centrifuge tube, add 0.2mol/L FC reagent 1mL, 15%Na
2CO
3Solution 2mL, distilled water is settled to 8mL, 25 ℃ of reaction 2h.Accurately draw distilled water 0.4mL in addition, operate as blank with method.Measure its absorbance A at the 765nm place.Drafting is with the standard curve of absorbance (A) with concentration (C), and the match equation of linear regression.
The equation of linear regression of gained standard curve is:
Y=4.323x+0.0166, correlation coefficient are R
2=0.9998 (1)
Y-absorbance in the formula; X-Galla Turcica (Galla Helepensis) acidity scale article concentration, mg/mL
The calculating of total polyphenols extraction ratio and content:
Polyphenol concentration (mg/mL)=(absorbance-0.0166)/4.323 * extension rate/1000 (2)
Polyphenol content (%)=extraction polyphenol quality/extract quality * 100% (3)
Polyphenol yield (%)=extract quality/raw materials quality * 100% (4)
Embodiment 1
The Semen Castaneae involucre is crushed to 60 orders, takes by weighing 30% ethanol water that 10g Semen Castaneae involucre powder adds 200mL and mix, with supersound extraction 30min under 55 ℃, 500W power; Centrifugal 15min under the 4000r/min condition, vacuum decompression revolve and steam lixiviating solution (40 ℃, 0.1MP), pump into the LSA-21 macroporous resin column that balance is good with concentrating the speed of lixiviating solution with 2mL/min; Elder generation is with the distilled water flushing pillar of 2 times of column volumes; Reuse 70% ethanol water is collected 70% ethanol elution with the flow velocity eluting of 2mL/min, and vacuum rotary steam concentrates under 40 ℃, 0.1MP; Be dried to powder; Obtain the henna Semen Castaneae involucre of 1.368g extract powder, the yield of extract is 13.68%, and wherein the content of polyphenol is 74.90%.
Embodiment 2
The Semen Castaneae involucre is crushed to 60 orders, takes by weighing 40% ethanol water that 10g Semen Castaneae involucre powder adds 250mL and mix, with supersound extraction 40min under 65 ℃, 500W power; Centrifugal 15min under the 4000r/min condition, vacuum decompression revolve and steam lixiviating solution (40 ℃, 0.1MP), pump into the LSA-21 macroporous resin column that balance is good with concentrating the speed of lixiviating solution with 2mL/min; Elder generation is with the distilled water flushing pillar of 2 times of column volumes; Reuse 70% ethanol water is collected 70% ethanol elution with the flow velocity eluting of 2mL/min, and vacuum rotary steam concentrates under 40 ℃, 0.1MP; Be dried to powder; Obtain the henna Semen Castaneae involucre of 1.445g extract powder, the yield of extract is 14.45%, and wherein the content of polyphenol is 74.27%.
Embodiment 3
The Semen Castaneae involucre is crushed to 60 orders, takes by weighing 50% ethanol water that 10g Semen Castaneae involucre powder adds 300mL and mix, with supersound extraction 50min under 75 ℃, 500W power; Centrifugal 15min under the 4000r/min condition, vacuum decompression revolve and steam lixiviating solution (40 ℃, 0.1MP), pump into the LSA-21 macroporous resin column that balance is good with concentrating the speed of lixiviating solution with 2mL/min; Elder generation is with the distilled water flushing pillar of 2 times of column volumes; Reuse 70% ethanol water is collected 70% ethanol elution with the flow velocity eluting of 2mL/min, and vacuum rotary steam concentrates under 40 ℃, 0.1MP; Be dried to powder; Obtain the henna Semen Castaneae involucre of 1.337g extract powder, the yield of extract is 13.37%, and wherein the content of polyphenol is 74.31%.
Embodiment 4
The Semen Castaneae involucre is crushed to 60 orders, takes by weighing 60% ethanol water that 10g Semen Castaneae involucre powder adds 350mL and mix, with supersound extraction 60min under 65 ℃, 500W power; Centrifugal 15min under the 4000r/min condition, vacuum decompression revolve and steam lixiviating solution (40 ℃, 0.1MP), pump into the LSA-21 macroporous resin column that balance is good with concentrating the speed of lixiviating solution with 2mL/min; Elder generation is with the distilled water flushing pillar of 2 times of column volumes; Reuse 70% ethanol water is collected 70% ethanol elution with the flow velocity eluting of 2mL/min, and vacuum rotary steam concentrates under 40 ℃, 0.1MP; Be dried to powder; Obtain the henna Semen Castaneae involucre of 1.325g extract powder, the yield of extract is 13.25%, and wherein the content of polyphenol is 75.23%.
Claims (8)
1. one kind is extracted the method for plant polyphenol from the Semen Castaneae involucre, comprises the steps: said Semen Castaneae involucre powder is added to the ethanol aqueous dispersions that obtains said Semen Castaneae involucre in the ethanol water, said ethanol aqueous dispersions is carried out ultrasonic assisted extraction after; Centrifugal, the rotary evaporation in vacuo lixiviating solution will concentrate lixiviating solution and utilize macroporous adsorbent resin to carry out purification; Collect ethanol elution; Vacuum rotary steam concentrates, and is dried to powder, obtains henna Semen Castaneae involucre extract powder; The yield of extract is that polyphenol content is more than 70% in the extract more than 13%.
2. in the method according to claim 1, it is characterized in that: the granularity of said Semen Castaneae involucre powder is 60 orders-80 orders.
3. in the method according to claim 1 and 2, it is characterized in that: ethanol quality percentage composition is 30%-70% in the said ethanol water.
4. according to arbitrary described method among the claim 1-3, it is characterized in that: the ethanol aqueous dispersions of said Semen Castaneae involucre is a liquid material ratio, and every 1g Semen Castaneae involucre powder adds the ethanol water of 10-35mL.
5. according to arbitrary described method among the claim 1-4, it is characterized in that: be provided with two factors of ultrasonic temperature and ultrasonic time in the said ultrasonic assisted extraction, wherein ultrasonic temperature is 25-75; Ultrasonic time is 20-60min.
6. according to arbitrary described method among the claim 1-5, it is characterized in that: said centrifugal condition is 4000r/min, 15min.
7. according to arbitrary described method among the claim 1-6, it is characterized in that: said vacuum is revolved the contract condition of Semen Castaneae involucre polyphenol of inspissation, 0.1MP, 40 ℃.
8. according to arbitrary described method among the claim 1-7; It is characterized in that: said purification with macroreticular resin polyphenol lixiviating solution; Promptly be enrichment process: the polyphenol lixiviating solution is pumped into the good LSA-21 macroporous adsorbent resin of balance that filters out, polyphenol is carried out enrichment; Earlier use the distilled water flushing pillar, reuse 40%-70% ethanol water eluting polyphenol is collected eluent.
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| CN2011104611299A CN102600216A (en) | 2011-12-30 | 2011-12-30 | Method for extracting plant polyphenol from Chinese chestnut involucre |
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| CN2011104611299A CN102600216A (en) | 2011-12-30 | 2011-12-30 | Method for extracting plant polyphenol from Chinese chestnut involucre |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104255882A (en) * | 2014-10-02 | 2015-01-07 | 陆建益 | Health-care fresh biscuit for preventing hyperlipidemia and manufacturing method thereof |
| CN110180216A (en) * | 2019-06-11 | 2019-08-30 | 南京农业大学 | A kind of method and device of intensified by ultrasonic wave fluidized bed type resin adsorption-parsing extraction purification anthocyanin |
| CN113527905A (en) * | 2021-06-24 | 2021-10-22 | 华中农业大学 | Method for extracting chestnut shell brown pigment from chestnut shells and application of chestnut shells brown pigment in hair dye |
Citations (1)
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| CN101402657A (en) * | 2008-11-14 | 2009-04-08 | 江苏大学 | Process for producing chestnut shell polyphenol |
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2011
- 2011-12-30 CN CN2011104611299A patent/CN102600216A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101402657A (en) * | 2008-11-14 | 2009-04-08 | 江苏大学 | Process for producing chestnut shell polyphenol |
Non-Patent Citations (2)
| Title |
|---|
| 张艳萍 等: "板栗中多酚物质的提取工艺优化", 《食品科技》, no. 09, 31 December 2009 (2009-12-31), pages 187 - 191 * |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104255882A (en) * | 2014-10-02 | 2015-01-07 | 陆建益 | Health-care fresh biscuit for preventing hyperlipidemia and manufacturing method thereof |
| CN110180216A (en) * | 2019-06-11 | 2019-08-30 | 南京农业大学 | A kind of method and device of intensified by ultrasonic wave fluidized bed type resin adsorption-parsing extraction purification anthocyanin |
| CN110180216B (en) * | 2019-06-11 | 2021-05-25 | 南京农业大学 | Method and device for extracting and purifying anthocyanin by ultrasonic-enhanced fluidized bed type resin adsorption-desorption |
| CN113527905A (en) * | 2021-06-24 | 2021-10-22 | 华中农业大学 | Method for extracting chestnut shell brown pigment from chestnut shells and application of chestnut shells brown pigment in hair dye |
| CN113527905B (en) * | 2021-06-24 | 2022-07-29 | 华中农业大学 | Method for extracting chestnut shell brown pigment from chestnut shells and application of chestnut shells brown pigment in hair dye |
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