CN111690076A - Dendrobium pectin extraction process method - Google Patents
Dendrobium pectin extraction process method Download PDFInfo
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- CN111690076A CN111690076A CN202010573947.7A CN202010573947A CN111690076A CN 111690076 A CN111690076 A CN 111690076A CN 202010573947 A CN202010573947 A CN 202010573947A CN 111690076 A CN111690076 A CN 111690076A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0045—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid alpha-D-Galacturonans, e.g. methyl ester of (alpha-1,4)-linked D-galacturonic acid units, i.e. pectin, or hydrolysis product of methyl ester of alpha-1,4-linked D-galacturonic acid units, i.e. pectinic acid; Derivatives thereof
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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Abstract
The invention discloses a dendrobium pectin extraction process method, which comprises the following steps: the method comprises the steps of raw material pretreatment, stock solution extraction and extraction purification, wherein in the stock solution extraction step, the pretreated raw material is extracted in a mode of water extraction and ultrasonic extraction, so that the extraction rate of pectin stock solution in the raw material can be greatly improved; in the step of extraction and purification, a freeze-thaw protein removal manner is adopted to be matched with a supercritical carbon dioxide manner for extraction, so that the conditions of removing protein and bringing external solvent in the extraction process can be effectively avoided, the content of impurities in the pectin solution is greatly reduced, the purity of the pectin is improved, and the method is favorable for industrial production and application.
Description
Technical Field
The invention relates to the technical field of plant extraction processes, and particularly relates to a dendrobium pectin extraction process method.
Background
The natural pectins are widely present in fruits, roots, stems and leaves of plants in the form of protopectin, pectin and pectic acid, are one of the components of cell walls, and exist along with cellulose to form an interlayer adhesive of adjacent cells, so that plant tissue cells are tightly bonded together. Pectin is essentially a linear polysaccharide polymer, and the extraction process of pectin in the prior art generally comprises raw material pretreatment, extraction, decolorization, filter pressing concentration and drying to obtain a finished product. The dendrobium nobile is a traditional rare Chinese herbal medicine in China, the medicinal history is over 2000 years, the main chemical components of the dendrobium nobile comprise alkaloids, polysaccharides, polyphenols and the like, wherein the polysaccharides (namely pectin) are one of the most effective components in the dendrobium nobile, and the dendrobium nobile polysaccharide has stronger pharmacological activities of resisting aging, oxidation and tumors, enhancing the immunity of organisms and the like on the surface of pharmacological research. With the enhancement of health care consciousness of people in recent years, the demand of dendrobe polysaccharide is continuously increased, the market demand is vigorous, and the demand is not met, but the extraction rate is low when dendrobe polysaccharide, namely dendrobe pectin, is extracted according to the conventional extraction process in the prior art, and the purity of the extracted pectin is low, so that the requirements of people cannot be met.
Disclosure of Invention
In order to solve the problems, the invention provides a dendrobium pectin extraction process method which is high in extraction rate and high in purity of the obtained product.
The invention adopts the following technical scheme:
a process method for extracting dendrobe pectin comprises the following steps:
pretreatment of raw materials:
(1) cleaning fresh herba Dendrobii, freeze drying, and pulverizing to obtain herba Dendrobii powder;
(2) performing multiple primary impurity extractions on the dendrobium powder by using petroleum ether until an extracting solution is clear, filtering, and volatilizing a solvent to obtain primary filter residue;
(3) performing secondary extraction of impurities on the primary filter residue obtained in the step (2) by using ethanol, filtering, and volatilizing the solvent to obtain secondary filter residue;
extracting stock solution:
(4) mixing and extracting the secondary filter residue obtained in the step (3) and distilled water according to the volume ratio of 1: 2-4, placing the mixture in a water bath kettle for water bath heating, performing auxiliary extraction by adopting ultrasonic waves after heating is completed, and filtering to obtain tertiary filter residue and primary filtrate;
(5) repeating the step (4) to extract the three filter residues for multiple times to obtain multiple filter residues and multiple filtrates, and finally mixing and concentrating the primary filtrate and the subsequent multiple filtrates to obtain a dendrobe stock solution;
extraction and purification:
(6) performing repeated freeze thawing on the dendrobium stock solution obtained in the step (5) for 6-8 times, and performing centrifugal separation to remove protein to obtain primary pectin liquid;
(7) putting the primary pectin liquid obtained in the step (6) into a supercritical carbon dioxide fluid instrument for extraction to obtain a secondary pectin liquid;
(8) and (4) adding ion exchange resin into the secondary pectin liquid obtained in the step (7) for decoloring. Filtering, concentrating the filtrate, and drying to obtain herba Dendrobii pectin.
As a preferred technical scheme of the invention, the secondary extraction of impurities in the raw material pretreatment process comprises the following steps: and standing and extracting the primary filter residue and ethanol according to the volume ratio of 1: 1.2-2, wherein the standing and extracting time is 3-6 h.
As a preferred technical scheme of the invention, the water bath temperature is 40-55 ℃ when the water bath is heated in the raw liquid extraction process.
As a preferable technical scheme of the invention, the time of water bath heating in the stock solution extraction process is 3-5 h.
As a preferred technical scheme of the invention, the freeze-thaw process is a process of placing the dendrobe stock solution in an environment with the temperature of-30 ℃ for freezing, then taking out the dendrobe stock solution, and then placing the dendrobe stock solution in an environment with the temperature of 35-50 ℃ for thawing.
The invention has the beneficial effects that:
according to the invention, the pretreated raw material is extracted by adopting a water extraction and ultrasonic extraction mode, so that the extraction rate of pectin stock solution in the raw material can be greatly improved; and in the extraction and purification process, the freeze thawing protein removal and supercritical carbon dioxide extraction are adopted, so that the conditions of removing protein and bringing external solvent in the extraction process can be effectively avoided, the content of impurities in the pectin solution is greatly reduced, and the purity of the pectin is improved.
Detailed Description
The present invention will now be described in further detail with reference to examples.
Example 1
A process method for extracting dendrobe pectin comprises the following steps:
pretreatment of raw materials:
(1) cleaning fresh herba Dendrobii, freeze drying, and pulverizing to obtain herba Dendrobii powder;
(2) performing multiple primary impurity extractions on the dendrobium powder by using petroleum ether until an extracting solution is clear, filtering, and volatilizing a solvent to obtain primary filter residue;
(3) performing secondary extraction of impurities on the primary filter residue obtained in the step (2) by using ethanol, filtering, and volatilizing the solvent to obtain secondary filter residue;
extracting stock solution:
(4) mixing and extracting the secondary filter residue obtained in the step (3) and distilled water according to the volume ratio of 1:2, placing the mixture in a water bath kettle for water bath heating, performing auxiliary extraction by adopting ultrasonic waves after heating is finished, and filtering to obtain third filter residue and primary filtrate;
(5) repeating the step (4) to extract the three filter residues for multiple times to obtain multiple filter residues and multiple filtrates, and finally mixing and concentrating the primary filtrate and the subsequent multiple filtrates to obtain a dendrobe stock solution;
extraction and purification:
(6) performing repeated freeze thawing on the dendrobium stock solution obtained in the step (5) for 6 times, and performing centrifugal separation to remove protein to obtain primary pectin liquid;
(7) putting the primary pectin liquid obtained in the step (6) into a supercritical carbon dioxide fluid instrument for extraction to obtain a secondary pectin liquid;
(8) and (4) adding ion exchange resin into the secondary pectin liquid obtained in the step (7) for decoloring. Filtering, concentrating the filtrate, and drying to obtain herba Dendrobii pectin.
Further, the secondary extraction of impurities in the raw material pretreatment process comprises the following steps: and (3) standing and extracting the primary filter residue and ethanol according to the volume ratio of 1:1.5, wherein the standing and extracting time is 5 hours.
Further, the temperature of the water bath during heating in the water bath during the extraction of the stock solution was 45 ℃.
Further, the time of water bath heating in the stock solution extraction process is 4 h.
Further, the freeze-thawing process is a process of placing the dendrobium stock solution in an environment with the temperature of-30 ℃ for freezing, then taking out the dendrobium stock solution, and then placing the dendrobium stock solution in an environment with the temperature of 35 ℃ for thawing.
Example 2
A process method for extracting dendrobe pectin comprises the following steps:
pretreatment of raw materials:
(1) cleaning fresh herba Dendrobii, freeze drying, and pulverizing to obtain herba Dendrobii powder;
(2) performing multiple primary impurity extractions on the dendrobium powder by using petroleum ether until an extracting solution is clear, filtering, and volatilizing a solvent to obtain primary filter residue;
(3) performing secondary extraction of impurities on the primary filter residue obtained in the step (2) by using ethanol, filtering, and volatilizing the solvent to obtain secondary filter residue;
extracting stock solution:
(4) mixing the secondary filter residue obtained in the step (3) with distilled water according to the volume ratio of 1:3 for extraction, placing the mixture in a water bath kettle for water bath heating, performing auxiliary extraction by adopting ultrasonic waves after heating is completed, and filtering to obtain third filter residue and primary filtrate;
(5) repeating the step (4) to extract the three filter residues for multiple times to obtain multiple filter residues and multiple filtrates, and finally mixing and concentrating the primary filtrate and the subsequent multiple filtrates to obtain a dendrobe stock solution;
extraction and purification:
(6) performing repeated freeze thawing on the dendrobium stock solution obtained in the step (5) for 8 times, and performing centrifugal separation to remove protein to obtain primary pectin liquid;
(7) putting the primary pectin liquid obtained in the step (6) into a supercritical carbon dioxide fluid instrument for extraction to obtain a secondary pectin liquid;
(8) and (4) adding ion exchange resin into the secondary pectin liquid obtained in the step (7) for decoloring. Filtering, concentrating the filtrate, and drying to obtain herba Dendrobii pectin.
Further, the secondary extraction of impurities in the raw material pretreatment process comprises the following steps: and (3) standing and extracting the primary filter residue and ethanol according to the volume ratio of 1:2, wherein the standing and extracting time is 3 hours.
Further, the temperature of the water bath during heating in the water bath during the extraction of the stock solution is 55 ℃.
Further, the time of water bath heating in the stock solution extraction process is 5 hours.
Further, the freeze-thawing process is a process of placing the dendrobium stock solution in an environment with the temperature of-30 ℃ for freezing, then taking out the dendrobium stock solution, and then placing the dendrobium stock solution in an environment with the temperature of 50 ℃ for thawing.
Comparative example 1
Extracting the dendrobe pectin according to the conventional technical means (namely an enzymolysis method) which is well known by the technical personnel in the field to obtain the comparison dendrobe pectin.
The comparison analysis of the dendrobe pectin obtained in example 1, example 2 and comparative example 1 is carried out, and the results are shown in the following table:
| product numbering | Dendrobe pectin yield | Purity of dendrobe pectin (polysaccharide content) |
| Example 1 | 13.6％ | 80.5％ |
| Example 2 | 14.1％ | 78.6％ |
| Comparative example 1 | 11.2％ | 49.3％ |
Wherein the yield of the dendrobe pectin is (mass of dendrobe pectin/mass of dendrobe) multiplied by 100 percent;
the purity of the dendrobe pectin is measured by chromatography.
Finally, it should be noted that: these embodiments are merely illustrative of the present invention and do not limit the scope of the present invention. In addition, other variations and modifications will be apparent to persons skilled in the art based on the foregoing description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications of the invention may be made without departing from the scope of the invention.
Claims (5)
1. A dendrobium pectin extraction process method is characterized in that: the method comprises the following steps:
pretreatment of raw materials:
(1) cleaning fresh herba Dendrobii, freeze drying, and pulverizing to obtain herba Dendrobii powder;
(2) performing multiple primary impurity extractions on the dendrobium powder by using petroleum ether until an extracting solution is clear, filtering, and volatilizing a solvent to obtain primary filter residue;
(3) performing secondary extraction of impurities on the primary filter residue obtained in the step (2) by using ethanol, filtering, and volatilizing the solvent to obtain secondary filter residue;
extracting stock solution:
(4) mixing and extracting the secondary filter residue obtained in the step (3) and distilled water according to the volume ratio of 1: 2-4, placing the mixture in a water bath kettle for water bath heating, performing auxiliary extraction by adopting ultrasonic waves after heating is completed, and filtering to obtain tertiary filter residue and primary filtrate;
(5) repeating the step (4) to extract the three filter residues for multiple times to obtain multiple filter residues and multiple filtrates, and finally mixing and concentrating the primary filtrate and the subsequent multiple filtrates to obtain a dendrobe stock solution;
extraction and purification:
(6) performing repeated freeze thawing on the dendrobium stock solution obtained in the step (5) for 6-8 times, and performing centrifugal separation to remove protein to obtain primary pectin liquid;
(7) putting the primary pectin liquid obtained in the step (6) into a supercritical carbon dioxide fluid instrument for extraction to obtain a secondary pectin liquid;
(8) and (4) adding ion exchange resin into the secondary pectin liquid obtained in the step (7) for decoloring. Filtering, concentrating the filtrate, and drying to obtain herba Dendrobii pectin.
2. The extraction process method of dendrobe pectin according to claim 1, which is characterized in that: the secondary extraction of impurities in the raw material pretreatment process comprises the following steps: and standing and extracting the primary filter residue and ethanol according to the volume ratio of 1: 1.2-2, wherein the standing and extracting time is 3-6 h.
3. The extraction process method of dendrobe pectin according to claim 1, which is characterized in that: the water bath temperature during water bath heating in the stock solution extraction process is 40-55 ℃.
4. The extraction process method of dendrobe pectin according to claim 1, which is characterized in that: and the time of water bath heating in the stock solution extraction process is 3-5 h.
5. The extraction process method of dendrobe pectin according to claim 1, which is characterized in that: the freeze thawing process is a process of placing the dendrobe stock solution in an environment with the temperature of minus 30 ℃ for freezing, taking out the dendrobe stock solution, and then placing the dendrobe stock solution in an environment with the temperature of 35-50 ℃ for thawing.
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Application publication date: 20200922 |