CN113694561A - Extraction and separation method of elderberry polyphenol - Google Patents
Extraction and separation method of elderberry polyphenol Download PDFInfo
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- CN113694561A CN113694561A CN202110998500.9A CN202110998500A CN113694561A CN 113694561 A CN113694561 A CN 113694561A CN 202110998500 A CN202110998500 A CN 202110998500A CN 113694561 A CN113694561 A CN 113694561A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0261—Solvent extraction of solids comprising vibrating mechanisms, e.g. mechanical, acoustical
- B01D11/0265—Applying ultrasound
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0288—Applications, solvents
Abstract
The invention discloses an extraction and separation method of elderberry polyphenol, which comprises the following preparation steps: s1: cleaning, preparing the good elderberry, cleaning the elderberry, removing some rotten elderberry in the cleaning process, preparing saline water after cleaning, and soaking the elderberry in the saline water for 30-45 minutes to remove chemical pesticides; s2: crushing, namely sequentially putting the elderberries obtained in the steps into a crusher to be crushed. According to the invention, the elderberry is soaked by the saline water, so that residual pesticides on the elderberry can be effectively eliminated, the pesticide interference in the extraction process is avoided, meanwhile, the rubus parvifolius powder is subjected to full enzymolysis, the extraction efficiency is effectively improved, meanwhile, the rubus parvifolius powder can be effectively extracted by ultrasonic extraction, and meanwhile, the extracted residues can be extracted by acidic ethanol, so that the waste of the residues is avoided, the production efficiency of polyphenol is effectively improved, and the practicability is strong.
Description
Technical Field
The invention relates to the technical field of extraction and separation of elderberry polyphenol, in particular to an extraction and separation method of elderberry polyphenol.
Background
The polyphenol refers to a general term of plant components containing several phenolic hydroxyl groups in a molecular structure, and comprises flavonoids, tannins, phenolic acids, anthocyanins and the like, and the elderberry polyphenol has indirect and direct antibacterial, antiallergic and antihypertensive effects besides antioxidant and anti-inflammatory effects.
However, the existing extraction and separation method of elderberry polyphenol is immature, has the problem of low extraction rate, wastes a large amount of elderberry, reduces the production efficiency and needs to be improved.
Disclosure of Invention
The invention aims to provide an extraction and separation method of elderberry polyphenol, which aims to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme:
a method for extracting and separating elderberry polyphenol comprises the following preparation steps;
s1: cleaning, preparing the good elderberry, cleaning the elderberry, removing some rotten elderberry in the cleaning process, preparing saline water after cleaning, and soaking the elderberry in the saline water for 30-45 minutes to remove chemical pesticides;
s2: crushing, namely sequentially putting the elderberry obtained in the steps into a crusher to be crushed, wherein the rotating speed of the crusher is 880-900r/min, and the time is 10-15 minutes, and then obtaining the crushed elderberry powder;
s3: performing enzymolysis, namely adding water into the obtained elderberry powder for dissolving, adding cellulase again after 5-10 minutes of dissolution, and performing full enzymolysis on the elderberry powder under the action of 330-380Hz ultrasonic waves;
s4: ultrasonic extracting, adding ethanol solution into elderberry powder, performing ultrasonic extraction at 45-48 deg.C, filtering to obtain extractive solution for 4-5 times, and mixing the extractive solutions to obtain polyphenol fusion solution and residue;
s5: extracting the filter residue with acidic ethanol at 50-60 deg.C for 20-30min to obtain extractive solution, filtering the filter residue, repeatedly extracting the filter residue until the extractive solution is colorless, and mixing the extractive solution and polyphenol fusion solution to obtain mixed solution;
s6: the preparation method comprises the steps of filtering the mixed solution by using an ultrafiltration membrane, concentrating penetrating fluid of the ultrafiltration membrane by using a nanofiltration membrane to obtain concentrated solution, and drying the concentrated solution to obtain the elderberry polyphenol.
In order to effectively perform the secondary extraction, the invention improves that in the step of S5, the preparation step of the acidic ethanol comprises the following steps:
(1) stirring, firstly preparing 90-95% ethanol solution and 1M hydrochloric acid solution, and storing the ethanol solution and the hydrochloric acid solution for later use;
(2) mixing, and then mixing the 1M hydrochloric acid solution and the ethanol solution according to the volume ratio of 16: 83 ratio to obtain the acidic ethanol.
In order to improve the extraction effect, the invention improves that in the step S3, the addition amount of the cellulase is 2-5mg of cellulase per gram of elderberry powder.
In order to improve the extraction effect, the invention improves that in the step S4, the adding amount of the ethanol solution is 15 times of the volume of the elderberry powder, and the mass concentration of the ethanol solution is between 75 and 85 percent.
In order to fully extract, the invention improves that in the step of S5, the dosage ratio of the filter residue to the acidic ethanol is 4 g: 80 mL.
In order to improve the drying efficiency, the invention improves that in the step S6, the drying time is 1-2 hours, the drying temperature is 60-70 ℃, and the drying ambient pressure is 1000-1200 Pa.
In order to improve the extraction efficiency, the invention improves that in the step S4, the frequency of the ultrasonic extraction is 550-600Hz, and the time of the ultrasonic extraction is 45-55 min.
Compared with the prior art, the invention has the beneficial effects that:
this extraction and separation method of elderberry polyphenol, compare in traditional extraction and separation method of elderberry polyphenol, soak elderberry through the salt solution, can effectively eliminate remaining pesticide on the elderberry, the pesticide interference extraction process has been avoided, carry out abundant enzymolysis through butt joint elderberry powder simultaneously, the effectual extraction efficiency that has improved, simultaneously extract through the supersound can effectually extract butt joint elderberry powder, the residue that extracts simultaneously can carry out the leaching through acid ethanol, the waste of residue has been avoided, the effectual production efficiency who improves polyphenol, therefore, the practicality is stronger, the progressive is showing.
Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention. The objectives and other advantages of the invention will be realized and attained by the structure particularly pointed out in the written description and claims hereof as well as the appended drawings.
The technical solution of the present invention is further described in detail by the accompanying drawings and embodiments.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a step diagram of the extraction and separation method of elderberry polyphenol according to the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the 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 embodiment of the invention provides a method for extracting and separating elderberry polyphenol, which comprises the following preparation steps:
s1: cleaning, preparing the good elderberry, cleaning the elderberry, removing some rotten elderberry in the cleaning process, preparing saline water after cleaning, and soaking the elderberry in the saline water for 30-45 minutes to remove chemical pesticides;
s2: crushing, namely sequentially putting the elderberry obtained in the steps into a crusher to be crushed, wherein the rotating speed of the crusher is 880-900r/min, and the time is 10-15 minutes, and then obtaining the crushed elderberry powder;
s3: performing enzymolysis, namely adding water into the obtained elderberry powder for dissolving, adding cellulase again after 5-10 minutes of dissolution, and performing full enzymolysis on the elderberry powder under the action of 330-380Hz ultrasonic waves;
s4: ultrasonic extracting, adding ethanol solution into elderberry powder, performing ultrasonic extraction at 45-48 deg.C, filtering to obtain extractive solution for 4-5 times, and mixing the extractive solutions to obtain polyphenol fusion solution and residue;
s5: extracting the filter residue with acidic ethanol at 50-60 deg.C for 20-30min to obtain extractive solution, filtering the filter residue, repeatedly extracting the filter residue until the extractive solution is colorless, and mixing the extractive solution and polyphenol fusion solution to obtain mixed solution;
s6: the preparation method comprises the steps of filtering the mixed solution by using an ultrafiltration membrane, concentrating penetrating fluid of the ultrafiltration membrane by using a nanofiltration membrane to obtain concentrated solution, and drying the concentrated solution to obtain the elderberry polyphenol.
In this embodiment: in the step S5, the step of preparing acidic ethanol comprises the following steps:
(1) stirring, firstly preparing 90-95% ethanol solution and 1M hydrochloric acid solution, and storing the ethanol solution and the hydrochloric acid solution for later use;
(2) mixing, and then mixing the 1M hydrochloric acid solution and the ethanol solution according to the volume ratio of 16: 83 ratio to obtain the acidic ethanol.
In this embodiment: in the step S3, the addition amount of the cellulase is 2-5mg per gram of elderberry powder, and the microbial cellulase can easily destroy the cell wall in the elderberry so as to improve the polyphenol yield.
In this embodiment: in the step S4, the adding amount of the ethanol solution is 15 times of the volume of the elderberry powder, the mass concentration of the ethanol solution is 75-85%, the structural formula of the ethanol is CH3CH2OH, the ethanol is one of alcohols and is a main component of the wine, so the ethanol is called the alcohol, and the ethanol has dissolubility and can achieve the effect of extraction.
In this embodiment: in the step S5, the usage ratio of the filter residue to the acidic ethanol is 4 g: 80mL, the filter residue can be fully extracted.
In this embodiment: in the step S6, the drying time is 1-2 hours, the drying temperature is 60-70 ℃, and the drying ambient pressure is 1000-1200Pa, and by adjusting the drying time, the drying temperature, and the drying ambient pressure, the drying efficiency can be effectively improved, and further the production efficiency can be improved, and the practicability is strong.
In this embodiment: in the step S4, the frequency of the ultrasonic extraction is 550-.
It can be seen through above-mentioned embodiment, compare in traditional elderberry polyphenol's extraction separation method, soak elderberry through the salt solution, can effectively eliminate remaining pesticide on the elderberry, the pesticide interference extraction process has been avoided, carry out abundant enzymolysis through butt joint elderberry powder simultaneously, the effectual extraction efficiency that has improved, simultaneously extract through the supersound can effectually extract butt joint elderberry powder, the residue that extracts simultaneously can carry out the leaching through acid ethanol, the waste of residue has been avoided, the effectual production efficiency who improves polyphenol, therefore, the practicality is stronger, the progressive is showing.
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that various changes in the embodiments and/or modifications of the invention can be made, and equivalents and modifications of some features of the invention can be made without departing from the spirit and scope of the invention.
Claims (7)
1. The extraction and separation method of elderberry polyphenol is characterized by comprising the following preparation steps:
s1: cleaning, preparing the good elderberry, cleaning the elderberry, removing some rotten elderberry in the cleaning process, preparing saline water after cleaning, and soaking the elderberry in the saline water for 30-45 minutes to remove chemical pesticides;
s2: crushing, namely sequentially putting the elderberry obtained in the steps into a crusher to be crushed, wherein the rotating speed of the crusher is 880-900r/min, and the time is 10-15 minutes, and then obtaining the crushed elderberry powder;
s3: performing enzymolysis, namely adding water into the obtained elderberry powder for dissolving, adding cellulase again after 5-10 minutes of dissolution, and performing full enzymolysis on the elderberry powder under the action of 330-380Hz ultrasonic waves;
s4: ultrasonic extracting, adding ethanol solution into elderberry powder, performing ultrasonic extraction at 45-48 deg.C, filtering to obtain extractive solution for 4-5 times, and mixing the extractive solutions to obtain polyphenol fusion solution and residue;
s5: extracting the filter residue with acidic ethanol at 50-60 deg.C for 20-30min to obtain extractive solution, filtering the filter residue, repeatedly extracting the filter residue until the extractive solution is colorless, and mixing the extractive solution and polyphenol fusion solution to obtain mixed solution;
s6: the preparation method comprises the steps of filtering the mixed solution by using an ultrafiltration membrane, concentrating penetrating fluid of the ultrafiltration membrane by using a nanofiltration membrane to obtain concentrated solution, and drying the concentrated solution to obtain the elderberry polyphenol.
2. The method for extracting and separating elderberry polyphenol according to claim 1, which is characterized in that: in the step S5, the step of preparing acidic ethanol comprises the following steps:
(1) stirring, firstly preparing 90-95% ethanol solution and 1M hydrochloric acid solution, and storing the ethanol solution and the hydrochloric acid solution for later use;
(2) mixing, and then mixing the 1M hydrochloric acid solution and the ethanol solution according to the volume ratio of 16: 83 ratio to obtain the acidic ethanol.
3. The method for extracting and separating elderberry polyphenol according to claim 2, which is characterized in that: in the step S3, the addition amount of the cellulase is 2-5mg of cellulase per gram of elderberry powder.
4. The method for extracting and separating elderberry polyphenol according to claim 1, which is characterized in that: in the step S4, the adding amount of the ethanol solution is 15 times of the volume of the elderberry powder, and the mass concentration of the ethanol solution is 75-85%.
5. The method for extracting and separating elderberry polyphenol according to claim 1, which is characterized in that: in the step S5, the usage ratio of the filter residue to the acidic ethanol is 4 g: 80 mL.
6. The method for extracting and separating elderberry polyphenol according to claim 1, which is characterized in that: in the step S6, the drying time is 1-2 hours, the drying temperature is 60-70 ℃, and the drying ambient pressure is 1000-1200 Pa.
7. The method for extracting and separating elderberry polyphenol according to claim 1, which is characterized in that: in the step S4, the frequency of the ultrasonic extraction is 550-600Hz, and the time of the ultrasonic extraction is 45-55 min.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP4190341A1 (en) * | 2021-12-06 | 2023-06-07 | Iprona AG/SpA | Elderberry extract for use in a method of preventing or treating sars-cov-2 infection |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP4190341A1 (en) * | 2021-12-06 | 2023-06-07 | Iprona AG/SpA | Elderberry extract for use in a method of preventing or treating sars-cov-2 infection |
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