CN112851830A - Extraction method of dendrobium officinale polysaccharide and application of dendrobium officinale polysaccharide in preparation of product - Google Patents

Extraction method of dendrobium officinale polysaccharide and application of dendrobium officinale polysaccharide in preparation of product Download PDF

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CN112851830A
CN112851830A CN202110286802.3A CN202110286802A CN112851830A CN 112851830 A CN112851830 A CN 112851830A CN 202110286802 A CN202110286802 A CN 202110286802A CN 112851830 A CN112851830 A CN 112851830A
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dendrobium officinale
polysaccharide
extraction
centrifuging
solution
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周涛
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Feilang Biotechnology Hubei Co ltd
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08BPOLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B37/00Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
    • C08B37/0003General processes for their isolation or fractionation, e.g. purification or extraction from biomass

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Abstract

The invention relates to an extraction method of dendrobium officinale polysaccharide and application of the dendrobium officinale polysaccharide in preparation of products, and relates to the technical field of polysaccharide extraction. The method comprises the following steps: pulverizing dried herba Dendrobii, and weighing; fixing the ratio of material to liquid, extraction temperature, extraction time, ultrasonic power and the like, and extracting in a pulse mode; after sufficient extraction, the polysaccharide solution is concentrated and purified with absolute ethanol. The method only uses a pulse mode, ensures higher polysaccharide extraction rate, solves the problem of energy consumption, and extracts the dendrobium officinale residue, thereby having the effects of tonifying stomach, promoting fluid production, nourishing yin, clearing heat, regulating immunity, delaying senescence and the like; the obtained Dendrobium officinale polysaccharide has good effects of moisturizing, tendering skin, caring skin, relieving inflammation and resisting aging.

Description

Extraction method of dendrobium officinale polysaccharide and application of dendrobium officinale polysaccharide in preparation of product
Technical Field
The invention belongs to the technical field of polysaccharide extraction, and particularly relates to a dendrobium officinale polysaccharide extraction method and application of a prepared product thereof.
Background
Dendrobium officinale (Dendrobium officinale) is an important plant used as both medicine and food, and can tonify stomach, promote fluid production, regulate immunity, delay aging and the like. Research shows that the Dendrobium officinale contains various active ingredients such as polysaccharide, alkaloid, polyphenol, flavone, amino acid and the like, wherein Dendrobium Officinale Polysaccharide (DOP) is the main active ingredient of the Dendrobium officinale polysaccharide, is also the substance with the highest content, and has the effects of moisturizing, skin tendering, skin care, skin soothing, inflammation relieving, aging resistance and the like.
But the prior art has insufficient application to the extraction of the dendrobium officinale and the extracted products.
Disclosure of Invention
The invention aims to provide a dendrobium officinale polysaccharide extraction method and application of a prepared product thereof, which aim to solve the existing problems: the prior art has insufficient application to extraction of dendrobium officinale and extracted products.
In order to solve the technical problems, the invention is realized by the following technical scheme: a method for extracting dendrobium officinale polysaccharide comprises the following steps:
step one, crushing dried dendrobium officinale, and weighing a proper amount;
step two, adding the sample and distilled water into a three-neck flask in a proper proportion, setting ultrasonic working parameters, and stirring and extracting;
step three, after full extraction, filtering, and carrying out vacuum freeze drying on the residues;
step four, concentrating the polysaccharide solution, and centrifuging the concentrated solution;
removing impurities by using absolute ethyl alcohol;
taking supernatant, adding absolute ethyl alcohol for alcohol precipitation, standing overnight, centrifuging to obtain precipitate, and adding pure water to dissolve the precipitate;
adding anhydrous ethanol into the solution, performing secondary alcohol precipitation, standing overnight, centrifuging to obtain precipitate, adding pure water for dissolving, centrifuging to obtain supernatant, and vacuum freeze drying the polysaccharide solution.
Further, in the step one, the granularity of the dendrobium officinale is 0.1-0.2 mm.
Further, in the step one, 4.8-5.2g of dendrobium officinale is weighed.
Further, in the second step, the ratio of the sample to distilled water is 1: 55-1: 65g/mL were mixed and charged into a 500mL three-necked flask.
Further, in the second step, setting ultrasonic working parameters, which mainly includes:
the 240W ultrasonic cleaner parameters were set to: heating at 68-72 deg.C for 20-160min, with ultrasonic power of 60% and duty ratio of 20% -100%, and stirring for extraction.
Further, in the third step, the vacuum freeze drying is carried out for 2-2.5 days at the temperature of-20 ℃ to-40 ℃ to obtain the dendrobium officinale residue.
Further, in the fourth step, the concentrated solution is centrifuged for 15-20min at 4000-.
Further, in the fourth step, the supernatant is taken, absolute ethyl alcohol is added for alcohol precipitation, the mixture is kept stand overnight, and precipitates are obtained by centrifugation, and the method mainly comprises the following steps:
adding anhydrous ethanol to the supernatant at a mixed concentration of 85%, and standing in a refrigerator at 4 deg.C for 12-13 hr;
centrifuging at 5000r/min for 15-20min, collecting precipitate, and adding pure water to dissolve the precipitate.
Further, in the fourth step, absolute ethyl alcohol is added into the solution for secondary alcohol precipitation, the solution is kept stand overnight, the precipitate is obtained by centrifugation, and pure water is added for dissolution, which mainly comprises:
adding absolute ethanol for secondary alcohol precipitation, and standing in a refrigerator at 4 ℃ for 4-5 h;
centrifuging at 4000-.
Further, in the fourth step, the supernatant is obtained by centrifugation, which mainly comprises:
centrifuging the solution at 4000-.
Further, in the fourth step, the vacuum freeze drying is carried out for 2-2.5 days at the temperature of-20 ℃ to-40 ℃ to obtain the dendrobium officinale polysaccharide solid.
The prepared dendrobium officinale residue is applied to the preparation of at least one food with the effects of promoting the secretion of saliva or body fluid, nourishing yin, clearing heat, regulating immunity, delaying aging and the like.
The dendrobium officinale polysaccharide solution prepared by the method is applied to preparing a product with at least one of effects of moisturizing, skin tendering, skin care, skin soothing, inflammation relieving and anti-aging.
The dendrobium officinale polysaccharide solid prepared by the method is applied to the preparation of at least one product with the effects of moisturizing, skin tendering, skin care, skin soothing, inflammation relieving and anti-aging.
The invention has the following beneficial effects:
the invention uses the ultrasonic pulse mode for extraction, but not a full ultrasonic auxiliary extraction method, has the characteristics of short ultrasonic time, low energy consumption and high yield, and is beneficial to large-scale industrial popularization and application; the extraction in the ultrasonic pulse mode not only dissolves out the dendrobium officinale polysaccharide, but also destroys the initial structure of the dendrobium officinale cellulose, does not cause pollution, and is beneficial to the application of the dendrobium officinale residue in food in the later period.
The invention provides a novel extraction process, which fully explores the influence of ultrasonic duty ratio on extraction rate, overcomes the defects of the traditional ultrasonic auxiliary extraction method, and realizes the rapid and efficient extraction of dendrobium polysaccharides.
The dendrobium officinale polysaccharide obtained by the invention has the effects of moisturizing, tendering skin, protecting skin, relieving skin, slowing down inflammation and resisting aging.
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 present invention will be described in detail with reference to examples, but the present invention is not limited thereto.
Example 1 extraction method of Dendrobium officinale polysaccharide
Weighing 5g of Dendrobium officinale with particle size of 0.1-0.2 mm. The sample was mixed with distilled water at 1: 60g/mL and charged to a 500mL three-necked flask. The 240W ultrasonic cleaner parameters were set to: heating at 70 deg.C for 120min, with ultrasonic power of 60% and duty ratio of 20%, and stirring for extraction. And after full extraction, filtering, and carrying out vacuum freeze drying on the residue at the temperature of-20 to-40 ℃ for 2 days to obtain the dendrobium officinale residue. The concentrate was centrifuged at 5000r/min for 20 min. Adding absolute ethyl alcohol into the supernatant, mixing the mixture with the concentration of 85%, and standing the mixture for 12 hours in a refrigerator at the temperature of 4 ℃; centrifuging at 5000r/min for 20min, collecting precipitate, and adding pure water to dissolve the precipitate. Adding absolute ethyl alcohol for secondary alcohol precipitation, and standing for 4 hours in a refrigerator at the temperature of 4 ℃; centrifuging at 5000r/min for 20min, collecting precipitate, and dissolving with pure water. Centrifuging the solution at 5000r/min for 20min, and collecting supernatant to obtain herba Dendrobii officinalis polysaccharide solution. And (3) carrying out vacuum freeze drying on the polysaccharide solution at the temperature of-20 to-40 ℃ for 2 days to obtain the dendrobium officinale polysaccharide solid. The result showed an extraction of 38.96% and an energy consumption of 819 w/h.
Example 2 extraction method of Dendrobium officinale polysaccharide
Weighing 5g of Dendrobium officinale with particle size of 0.1-0.2 mm. The sample was mixed with distilled water at 1: 60g/mL and charged to a 500mL three-necked flask. The 240W ultrasonic cleaner parameters were set to: heating at 70 deg.C for 120min, with ultrasonic power of 60% and duty ratio of 60%, and stirring for extraction. And after full extraction, filtering, and carrying out vacuum freeze drying on the residue at the temperature of-20 to-40 ℃ for 2 days to obtain the dendrobium officinale residue. The concentrate was centrifuged at 5000r/min for 20 min. Adding anhydrous ethanol into the supernatant, mixing at 85% (v/v), and standing in a refrigerator at 4 deg.C for 12 hr; centrifuging at 5000r/min for 20min, collecting precipitate, and adding pure water to dissolve the precipitate. Adding absolute ethyl alcohol for secondary alcohol precipitation, and standing for 4 hours in a refrigerator at the temperature of 4 ℃; centrifuging at 5000r/min for 20min, collecting precipitate, and dissolving with pure water. Centrifuging the solution at 5000r/min for 20min, and collecting supernatant to obtain herba Dendrobii officinalis polysaccharide solution. And (3) carrying out vacuum freeze drying on the polysaccharide solution at the temperature of-20 to-40 ℃ for 2 days to obtain the dendrobium officinale polysaccharide solid. The result showed that the extraction rate was 40.46% and the energy consumption was 852 w/h.
Example 3 extraction method of Dendrobium officinale polysaccharide
Weighing 5g of Dendrobium officinale with particle size of 0.1-0.2 mm. The sample was mixed with distilled water at 1: 60g/mL and charged to a 500mL three-necked flask. The 240W ultrasonic cleaner parameters were set to: heating at 70 deg.C for 120min, with ultrasonic power of 60% and duty ratio of 100%, and stirring for extraction. And after full extraction, filtering, and carrying out vacuum freeze drying on the residue at the temperature of-20 to-40 ℃ for 2 days to obtain the dendrobium officinale residue. The concentrate was centrifuged at 5000r/min for 20 min. Adding anhydrous ethanol into the supernatant, mixing at 85% (v/v), and standing in a refrigerator at 4 deg.C for 12 hr; centrifuging at 5000r/min for 20min, collecting precipitate, and adding pure water to dissolve the precipitate. Adding absolute ethyl alcohol for secondary alcohol precipitation, and standing for 4 hours in a refrigerator at the temperature of 4 ℃; centrifuging at 5000r/min for 20min, collecting precipitate, and dissolving with pure water. Centrifuging the solution at 5000r/min for 20min, and collecting supernatant to obtain herba Dendrobii officinalis polysaccharide solution. And (3) carrying out vacuum freeze drying on the polysaccharide solution at the temperature of-20 to-40 ℃ for 2 days to obtain the dendrobium officinale polysaccharide solid. The result shows that the extraction rate is 42.02 percent and the energy consumption is 1443 w/h.
Example 4 Dendrobium officinale polysaccharide moisturizing and repairing lotion
The following parts by weight of each component were prepared.
Figure BDA0002980804820000061
The preparation method comprises the following steps: thoroughly cleaning and sterilizing related production equipment and related production tools, and preparing materials one by one; b1, adding B2 into an emulsifying pot after separately heating and dissolving, and heating to about 85 ℃; adding B3 while homogenizing, homogenizing for 5min, stirring at constant temperature for 10min, stirring, and cooling; cooling to about 45 deg.C, adding B4 and B5, stirring and dispersing; sampling, inspecting and discharging qualified materials.
In addition, the dendrobium officinale residue prepared by the method can be applied to the preparation of food with the effects of promoting the secretion of saliva or body fluid, nourishing yin, clearing heat, regulating immunity, delaying senescence and the like, and is within the protection range of the invention;
the dendrobium officinale polysaccharide solution prepared by the method can be applied to preparing food with the effects of moisturizing, skin tendering, skin care, skin soothing, inflammation relieving and aging resisting, and also is within the protection range of the invention; .
The dendrobium officinale polysaccharide solid prepared by the method can be applied to preparing foods with the effects of moisturizing, skin tendering, skin care, skin soothing, inflammation relieving and anti-aging, and also is within the protection scope of the invention.
The method provided by the embodiment has the following characteristics:
1. the ultrasonic pulse mode is used for extraction, but a full ultrasonic auxiliary extraction method is not used, so that the method has the characteristics of short ultrasonic time, low energy consumption and high yield, and is beneficial to large-scale industrial popularization and application.
2. The extraction in the ultrasonic pulse mode not only dissolves out the dendrobium officinale polysaccharide, but also destroys the initial structure of the dendrobium officinale cellulose, is not polluted by reagents, and is beneficial to the application of the dendrobium officinale residue in food in the later period.
3. The invention provides a novel extraction process, which fully explores the influence of ultrasonic duty ratio on extraction rate, overcomes the defects of the traditional ultrasonic auxiliary extraction method, and realizes the rapid and efficient extraction of dendrobium polysaccharides.
4. The obtained herba Dendrobii polysaccharide has effects of keeping moisture, caring skin, relieving inflammation, and resisting aging.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.

Claims (10)

1. The extraction method of the dendrobium officinale polysaccharide is characterized by comprising the following steps:
step one, crushing dried dendrobium officinale, and weighing a proper amount;
step two, adding the sample and distilled water into a three-neck flask in a proper proportion, setting ultrasonic working parameters, and stirring and extracting;
step three, after full extraction, filtering, and carrying out vacuum freeze drying on the residues;
step four, concentrating the polysaccharide solution, and centrifuging the concentrated solution;
removing impurities by using absolute ethyl alcohol;
taking supernatant, adding absolute ethyl alcohol for alcohol precipitation, standing overnight, centrifuging to obtain precipitate, and adding pure water to dissolve the precipitate;
adding anhydrous ethanol into the solution, performing secondary alcohol precipitation, standing overnight, centrifuging to obtain precipitate, adding pure water for dissolving, centrifuging to obtain supernatant, and vacuum freeze drying the polysaccharide solution.
2. The extraction method according to claim 1, wherein in the first step, the granularity of the dendrobium officinale is 0.1-0.2 mm;
in the first step, 4.8-5.2g of dendrobium officinale are weighed.
3. The extraction method according to claim 1, wherein in the second step, the ratio of the sample to the distilled water is 1: 55-1: mixing 65g/mL, and adding into a 500mL three-neck flask;
in the second step, setting ultrasonic working parameters, which mainly comprises:
the 240W ultrasonic cleaner parameters were set to: heating at 68-72 deg.C for 20-160min, with ultrasonic power of 60% and duty ratio of 20% -100%, and stirring for extraction.
4. The extraction method according to claim 1, wherein in the third step, the vacuum freeze drying is carried out at a temperature of-20 ℃ to-40 ℃ for 2-2.5 days to obtain the dendrobium officinale residue.
5. The extraction method as claimed in claim 1, wherein in step four, the concentrated solution is centrifuged at 4000-;
and in the fourth step, the supernatant is taken, absolute ethyl alcohol is added for alcohol precipitation, the mixture is kept stand overnight, and precipitates are obtained by centrifugation, and the method mainly comprises the following steps:
adding anhydrous ethanol to the supernatant at a mixed concentration of 85%, and standing in a refrigerator at 4 deg.C for 12-13 hr;
centrifuging at 5000r/min for 15-20min, collecting precipitate, and adding pure water to dissolve the precipitate.
6. The extraction method according to claim 5, wherein in the fourth step, absolute ethanol is added into the solution for secondary alcohol precipitation, the solution is left to stand overnight, the precipitate is obtained by centrifugation, and pure water is added for dissolution, and the method mainly comprises the following steps:
adding absolute ethanol for secondary alcohol precipitation, and standing in a refrigerator at 4 ℃ for 4-5 h;
centrifuging at 4000-;
in the fourth step, the supernatant fluid is obtained by centrifugation, which mainly comprises:
centrifuging the solution at 4000-.
7. The extraction method according to claim 1, wherein in the fourth step, the vacuum freeze drying is carried out at a temperature of-20 ℃ to-40 ℃ for 2-2.5 days to obtain the dendrobium officinale polysaccharide solid.
8. Use of the dendrobium officinale residue prepared according to any one of claims 1-7 in the preparation of food with at least one of stomach-benefiting, fluid production-promoting, yin-nourishing, heat-clearing, immunoregulatory, anti-aging and other effects.
9. Use of the dendrobium candidum polysaccharide solution prepared according to any one of claims 1 to 7 in the preparation of a product with at least one of the effects of moisturizing, skin rejuvenation, skin care, skin soothing, inflammation reduction and anti-aging.
10. Use of the solid dendrobium officinale polysaccharide prepared according to any one of claims 1-7 in the preparation of a product with at least one of the effects of moisturizing, skin rejuvenation, skin care, skin soothing, inflammation relieving and anti-aging.
CN202110286802.3A 2021-03-17 2021-03-17 Extraction method of dendrobium officinale polysaccharide and application of dendrobium officinale polysaccharide in preparation of product Pending CN112851830A (en)

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