CN113230319A - Process for extracting polyphenol from aronia melanocarpa - Google Patents
Process for extracting polyphenol from aronia melanocarpa Download PDFInfo
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- CN113230319A CN113230319A CN202110712195.2A CN202110712195A CN113230319A CN 113230319 A CN113230319 A CN 113230319A CN 202110712195 A CN202110712195 A CN 202110712195A CN 113230319 A CN113230319 A CN 113230319A
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/73—Rosaceae (Rose family), e.g. strawberry, chokeberry, blackberry, pear or firethorn
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/10—Preparation or pretreatment of starting material
- A61K2236/15—Preparation or pretreatment of starting material involving mechanical treatment, e.g. chopping up, cutting or grinding
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/10—Preparation or pretreatment of starting material
- A61K2236/19—Preparation or pretreatment of starting material involving fermentation using yeast, bacteria or both; enzymatic treatment
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
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Abstract
The invention provides a process for extracting aronia melanocarpa polyphenol, and relates to the field of polyphenol extraction. The extraction process of the aronia melanocarpa polyphenol comprises the following steps: the method comprises the following steps: preparing Aronia melanocarpa liquid; step two: carrying out extraction; step three: removing grease; step four: performing ultrasonic-microwave composite extraction; step five: leaching and extracting; step six: performing rough treatment; step seven: carrying out dealcoholization treatment; step eight: and (5) drying at low temperature. Unfreezing through the quick-freeze and broken wall machine to the cell than breaking away, add the cellulase through the later stage simultaneously, break away remaining cell wall for the cell sap is appeared completely, can obtain the inside polyphenol of more aronia melanocarpa, through reasonable step, can obtain comparatively pure polyphenol product, and inside only adds the ethanol solution that has volatility moreover, and the product that obtains is harmless to the human body, uses safety that can be more.
Description
Technical Field
The invention relates to the technical field of polyphenol extraction, in particular to a process for extracting aronia melanocarpa polyphenol.
Background
The black chokeberry generally refers to black and astringent photinia serrulata, which is a rosebush of acerbita in Rosaceae, the berries of the black and astringent photinia are rich in flavone, anthocyanin, polyphenol and other substances, the extract has special effects on treating cancers, diabetes, cardiovascular and cerebrovascular diseases and other diseases, and is widely applied to the medicine and food industry in European and American areas. In addition, the aronia melanocarpa has dense and bright flower bundles, longer flowering phase, red and bright autumn leaves, and strong cold resistance, drought resistance, disease and pest resistance, and has huge development potential in the aspects of ornamental value and ecological function.
The applicant finds that a Chinese patent discloses a process for extracting aronia melanocarpa polyphenol through retrieval when applying the invention, the application number of the process is '201910780293.2', the process mainly uses aronia melanocarpa pomace as a raw material to pretreat the aronia melanocarpa pomace, so that the subsequent extraction of active substances is facilitated, the waste of resources is reduced, and the utilization rate of the resources is improved.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a process for extracting aronia melanocarpa polyphenol, which solves the problem of incomplete extraction.
(II) technical scheme
In order to achieve the purpose, the invention is realized by the following technical scheme: a process for extracting polyphenol from Aronia melanocarpa comprises the following steps:
the method comprises the following steps: preparing a aronia melanocarpa liquid, selecting aronia melanocarpa fruits which are not damaged by worms and have plump fruits, then quickly freezing and unfreezing the aronia melanocarpa, crushing by using crushing equipment to break internal cells, enabling cell liquid to flow out, and performing circulation operation for multiple times to form a mixed solution;
step two: carrying out extraction: adding cellulase and protease into the mixed solution, and then carrying out standing reaction for a period of time;
step three: removing grease: the internal components are purified by scraping the fat and volatile oils from the surface of the resting liquid.
Step four: performing ultrasonic-microwave composite extraction: sequentially carrying out ultrasonic extraction and microwave extraction on the reacted solution to obtain a final extracting solution;
step five: leaching and extracting: adding ethanol solution into the extracted solution, placing the solution in a water bath oscillator, performing water bath oscillation on the solution to obtain upper layer extract and lower layer filter residue, and adding ethanol solution into the filter residue again to perform water bath oscillation to extract upper layer extract;
step six: carrying out rough treatment: filtering the obtained extracting solution through a plurality of layers of activated carbon filter screens to remove internal colors and internal fine impurities, so that the extracting solution is purer;
step seven: carrying out dealcoholization treatment: heating the mixed solution, fractionating the ethanol inside with water, and then recovering the ethanol through condensation for recycling;
step eight: and (3) carrying out low-temperature drying: and concentrating the obtained extracting solution at low temperature, and then performing freeze drying treatment to obtain the final polypeptide product.
Preferably, the crushing equipment in the first step is a wall breaking machine, and the wall breaking time is 20 to 30 minutes.
Preferably, the reaction time in the second step is 60 minutes to 90 minutes, and the stirring is carried out for 1 minute for 10 minutes in the reaction process and lasts for four times.
Preferably, in the third step, an oil scraping plate is used for scraping, and oil absorption paper is used for absorbing residual floating oil after scraping.
Preferably, in the fourth step, the ultrasonic extraction time is 3-5 minutes, the microwave extraction time is 3-5 minutes, and the microwave radiation power is 700-900W.
Preferably, the temperature of the water bath in the fifth step is 50-60 ℃, the adding amount of the first ethanol is the same as the volume of the extracting solution, and the adding amount of the second ethanol is 10-15 times of the mass of the residue.
Preferably, the temperature for heating in the seventh step is 72-80 ℃, and the distillation is carried out until no excessive liquid is generated.
Preferably, the temperature of the low-temperature concentration is 40-50 ℃, the pressure of the freeze drying is below 646.5Pa, and the temperature is below-2 ℃.
(III) advantageous effects
The invention provides a process for extracting aronia melanocarpa polyphenol. The method has the following beneficial effects:
1. according to the method, the cell ratio is broken through quick-freezing and unfreezing and a wall breaking machine, and simultaneously, the residual cell walls are broken through adding cellulase at the later stage, so that the cell sap is completely separated out, and more polyphenol in the aronia melanocarpa can be obtained.
2. According to the invention, through reasonable steps, relatively pure polyphenol products can be obtained, and only volatile ethanol solution is added inside the polyphenol product, so that the obtained polyphenol product is harmless to human bodies and is safer to use.
3. According to the invention, the bottom stirring is carried out in the reaction process, and then the standing is carried out, so that the fat and volatile oil in the aronia melanocarpa can be effectively floated, the internal oil component can be effectively removed, and the extracted polyphenol extract is purer.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The first embodiment is as follows:
the embodiment of the invention provides a process for extracting aronia melanocarpa polyphenol, which comprises the following steps:
the method comprises the following steps: preparing a aronia melanocarpa liquid, selecting aronia melanocarpa fruits which are not damaged by worms and have plump fruits, then quickly freezing and unfreezing the aronia melanocarpa, crushing by using crushing equipment to crush internal cells, enabling cell liquid to flow out, and performing circulation operation for multiple times to form a mixed solution, so that the cells can be more thoroughly crushed;
step two: carrying out extraction: adding cellulase and protease into the mixed solution, then carrying out standing reaction for a period of time, removing cell walls of cells in the mixed solution, and simultaneously decomposing a small amount of protein into polypeptide;
step three: removing grease: scraping fat and volatile oil on the surface of the liquid on which the liquid is placed to purify internal components and remove internal grease;
step four: performing ultrasonic-microwave composite extraction: sequentially carrying out ultrasonic extraction and microwave extraction on the reacted solution to separate out the polypeptide in the internal cell sap to obtain a final extracting solution;
step five: leaching and extracting: adding an ethanol solution into the extracted solution, placing the solution in a water bath oscillator, performing water bath oscillation on the solution to obtain an upper-layer extracting solution and a lower-layer filter residue, adding the ethanol solution into the filter residue again, performing water bath oscillation to extract the upper-layer extracting solution, enabling the ethanol solution to absorb polyphenol substances, and then enabling polysaccharide substances to separate out crystals to purify the inside;
step six: carrying out rough treatment: filtering the obtained extracting solution through a plurality of layers of activated carbon filter screens to remove internal colors and internal fine impurities, so that the extracting solution is purer;
step seven: carrying out dealcoholization treatment: heating the mixed solution, fractionating the ethanol inside with water, and then recovering the ethanol through condensation for recycling;
step eight: and (3) carrying out low-temperature drying: and concentrating the obtained extracting solution at low temperature, and then performing freeze drying treatment to obtain the final polypeptide product.
In the first step, crushing equipment is a wall breaking machine, the wall breaking time is 20-30 minutes, a part of internal cells can be crushed, in the second step, the reaction time is 60-90 minutes, stirring is carried out for 1 minute in the reaction process for four times, a small amount of fat and volatile oil in the internal cells can be separated out, the volatile oil can be conveniently removed, in the third step, an oil scraping plate is adopted for scraping, the residual floating oil is scraped and absorbed by oil absorption paper, the internal oil can be completely removed, in the fourth step, the ultrasonic extraction time is 3-5 minutes, the microwave radiation power is 700-900W, the polyphenol substances in the internal cells can be completely fused with an ethanol solution, in the fifth step, the water bath temperature is 50-60 ℃, the first ethanol addition is consistent in volume of an extracting solution, and the second ethanol addition is 10-15 times of the residue mass, the polyphenol substances in the tea can be completely extracted, the heating temperature in the step seven is 72-80 ℃, the tea is distilled until no redundant liquid is generated, the alcohol in the tea is distilled, the residue is less, the residual alcohol can be lower than 5%, the alcohol is convenient to recover, the waste of resources is reduced, the low-temperature concentration temperature is 40-50 ℃, the freeze-drying pressure is below 646.5Pa, and the temperature is below-2 ℃, so that the water and alcohol in the tea can be further removed, and the pure polyphenol product is obtained.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (8)
1. A process for extracting aronia melanocarpa polyphenol is characterized by comprising the following steps: the method comprises the following steps:
the method comprises the following steps: preparing a aronia melanocarpa liquid, selecting aronia melanocarpa fruits which are not damaged by worms and have plump fruits, then quickly freezing and unfreezing the aronia melanocarpa, crushing by using crushing equipment to break internal cells, enabling cell liquid to flow out, and performing circulation operation for multiple times to form a mixed solution;
step two: carrying out extraction: adding cellulase and protease into the mixed solution, and then carrying out standing reaction for a period of time;
step three: removing grease: the internal components are purified by scraping the fat and volatile oils from the surface of the resting liquid.
Step four: performing ultrasonic-microwave composite extraction: sequentially carrying out ultrasonic extraction and microwave extraction on the reacted solution to obtain a final extracting solution;
step five: leaching and extracting: adding ethanol solution into the extracted solution, placing the solution in a water bath oscillator, performing water bath oscillation on the solution to obtain upper layer extract and lower layer filter residue, and adding ethanol solution into the filter residue again to perform water bath oscillation to extract upper layer extract;
step six: carrying out rough treatment: filtering the obtained extracting solution through a plurality of layers of activated carbon filter screens to remove internal colors and internal fine impurities, so that the extracting solution is purer;
step seven: carrying out dealcoholization treatment: heating the mixed solution, fractionating the ethanol inside with water, and then recovering the ethanol through condensation for recycling;
step eight: and (3) carrying out low-temperature drying: and concentrating the obtained extracting solution at low temperature, and then performing freeze drying treatment to obtain the final polypeptide product.
2. The process for extracting aronia melanocarpa polyphenol as claimed in claim 1, wherein the process comprises the following steps: the crushing equipment in the first step is a wall breaking machine, and the wall breaking time is 20-30 minutes.
3. The process for extracting aronia melanocarpa polyphenol as claimed in claim 1, wherein the process comprises the following steps: the reaction time in the second step is 60-90 minutes, and the stirring is carried out for 1 minute in 10 minutes in the reaction process and is continued for four times.
4. The process for extracting aronia melanocarpa polyphenol as claimed in claim 1, wherein the process comprises the following steps: and scraping by adopting an oil scraping plate in the third step, and scraping residual floating oil by adopting oil absorption paper.
5. The process for extracting aronia melanocarpa polyphenol as claimed in claim 1, wherein the process comprises the following steps: in the fourth step, the ultrasonic extraction time is 3-5 minutes, the microwave extraction time is 3-5 minutes, and the microwave radiation power is 700-900W.
6. The process for extracting aronia melanocarpa polyphenol as claimed in claim 1, wherein the process comprises the following steps: and the temperature of the water bath in the fifth step is 50-60 ℃, the adding amount of the first ethanol is the same as the volume of the extracting solution, and the adding amount of the second ethanol is 10-15 times of the mass of the residue.
7. The process for extracting aronia melanocarpa polyphenol as claimed in claim 1, wherein the process comprises the following steps: and the temperature for heating in the seventh step is 72-80 ℃, and the distillation is carried out until no excess liquid is generated.
8. The process for extracting aronia melanocarpa polyphenol as claimed in claim 1, wherein the process comprises the following steps: the low-temperature concentration temperature is 40-50 ℃, the freeze-drying pressure is below 646.5Pa, and the temperature is below-2 ℃.
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| CN202110712195.2A CN113230319A (en) | 2021-06-25 | 2021-06-25 | Process for extracting polyphenol from aronia melanocarpa |
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| CN202110712195.2A CN113230319A (en) | 2021-06-25 | 2021-06-25 | Process for extracting polyphenol from aronia melanocarpa |
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Citations (5)
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| CN105708919A (en) * | 2016-03-21 | 2016-06-29 | 吉林大学 | Extracting method for polyphenol and flavone in aronia melanocarpa |
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2021
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| CN105708919A (en) * | 2016-03-21 | 2016-06-29 | 吉林大学 | Extracting method for polyphenol and flavone in aronia melanocarpa |
| CN106806160A (en) * | 2017-03-08 | 2017-06-09 | 张仕英 | Ultrasonic microwave aids in Enzymatic Extraction green tea polyphenols and its application in shower cream |
| CN109851606A (en) * | 2019-04-12 | 2019-06-07 | 武威市文裕农业科技开发有限公司 | A method of extracting anthocyanidin from Black Box Tracing |
| CN110051739A (en) * | 2019-05-23 | 2019-07-26 | 武汉轻工大学 | A kind of extracting method of Black Box Tracing fruit polyphenol |
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Application publication date: 20210810 |