CN112125979A - Extraction method of hericium erinaceus polysaccharide - Google Patents
Extraction method of hericium erinaceus polysaccharide Download PDFInfo
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- 150000004676 glycans Chemical class 0.000 title claims abstract description 119
- 229920001282 polysaccharide Polymers 0.000 title claims abstract description 119
- 239000005017 polysaccharide Substances 0.000 title claims abstract description 119
- 240000000588 Hericium erinaceus Species 0.000 title claims abstract description 80
- 235000007328 Hericium erinaceus Nutrition 0.000 title claims abstract description 80
- 238000000605 extraction Methods 0.000 title claims abstract description 34
- 239000002245 particle Substances 0.000 claims abstract description 83
- 239000003208 petroleum Substances 0.000 claims abstract description 35
- 239000000741 silica gel Substances 0.000 claims abstract description 35
- 229910002027 silica gel Inorganic materials 0.000 claims abstract description 35
- 239000000084 colloidal system Substances 0.000 claims abstract description 31
- 238000001914 filtration Methods 0.000 claims abstract description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000000203 mixture Substances 0.000 claims abstract description 29
- 238000002791 soaking Methods 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 25
- 239000000706 filtrate Substances 0.000 claims abstract description 23
- 238000003756 stirring Methods 0.000 claims abstract description 16
- 238000000227 grinding Methods 0.000 claims abstract description 15
- 239000011347 resin Substances 0.000 claims abstract description 8
- 229920005989 resin Polymers 0.000 claims abstract description 8
- 238000000194 supercritical-fluid extraction Methods 0.000 claims abstract description 8
- 238000000108 ultra-filtration Methods 0.000 claims abstract description 8
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 14
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 2
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 238000010298 pulverizing process Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 40
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 26
- 150000002632 lipids Chemical class 0.000 description 6
- 238000002474 experimental method Methods 0.000 description 5
- 239000007864 aqueous solution Substances 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 238000000746 purification Methods 0.000 description 4
- 235000001674 Agaricus brunnescens Nutrition 0.000 description 3
- 241000289669 Erinaceus europaeus Species 0.000 description 3
- 241000233866 Fungi Species 0.000 description 3
- 241000577951 Hydnum Species 0.000 description 3
- 238000004090 dissolution Methods 0.000 description 3
- 239000003814 drug Substances 0.000 description 3
- 238000003809 water extraction Methods 0.000 description 3
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- 206010028980 Neoplasm Diseases 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
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- 235000013305 food Nutrition 0.000 description 2
- 238000004128 high performance liquid chromatography Methods 0.000 description 2
- 150000002576 ketones Chemical class 0.000 description 2
- 238000002386 leaching Methods 0.000 description 2
- 102000004169 proteins and genes Human genes 0.000 description 2
- 108090000623 proteins and genes Proteins 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 241000282693 Cercopithecidae Species 0.000 description 1
- 206010012735 Diarrhoea Diseases 0.000 description 1
- 208000000461 Esophageal Neoplasms Diseases 0.000 description 1
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- UPYKUZBSLRQECL-UKMVMLAPSA-N Lycopene Natural products CC(=C/C=C/C=C(C)/C=C/C=C(C)/C=C/C1C(=C)CCCC1(C)C)C=CC=C(/C)C=CC2C(=C)CCCC2(C)C UPYKUZBSLRQECL-UKMVMLAPSA-N 0.000 description 1
- 208000007443 Neurasthenia Diseases 0.000 description 1
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- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 208000005718 Stomach Neoplasms Diseases 0.000 description 1
- 208000007107 Stomach Ulcer Diseases 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 229930013930 alkaloid Natural products 0.000 description 1
- 150000003797 alkaloid derivatives Chemical class 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 206010003549 asthenia Diseases 0.000 description 1
- 230000001580 bacterial effect Effects 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
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- 210000004556 brain Anatomy 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
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- 201000011510 cancer Diseases 0.000 description 1
- 150000001746 carotenes Chemical class 0.000 description 1
- 235000005473 carotenes Nutrition 0.000 description 1
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- 229910052742 iron Inorganic materials 0.000 description 1
- 210000003734 kidney Anatomy 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000000874 microwave-assisted extraction Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
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- NCYCYZXNIZJOKI-UHFFFAOYSA-N vitamin A aldehyde Natural products O=CC=C(C)C=CC=C(C)C=CC1=C(C)CCCC1(C)C NCYCYZXNIZJOKI-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- 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
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
-
- 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- 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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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Molecular Biology (AREA)
- General Health & Medical Sciences (AREA)
- Sustainable Development (AREA)
- Biochemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention discloses a method for extracting hericium erinaceus polysaccharide, which comprises the following steps: pulverizing, adding water, and stirring to obtain colloid; adding into colloid mill for further grinding; adding petroleum ether-silica gel particle mixture, dissolving, and filtering to obtain filtrate and crude polysaccharide particles; adding a petroleum ether-silica gel particle mixture into the crude polysaccharide particles, dissolving, and filtering to form secondary filtrate and purified crude polysaccharide particles; adding 10-20 times of hot water at 40-80 deg.C into the purified crude polysaccharide particles, and soaking to obtain first extractive solution; ultrasonic soaking for 30-50 min; filtering to obtain residue, and performing CO2 supercritical extraction on the residue to obtain second extractive solution; and (4) performing resin decoloration and ultrafiltration on the first extracting solution and the second extracting solution to obtain the hericium erinaceus polysaccharide. The invention has the following beneficial effects: the extraction method of Hericium erinaceus polysaccharide has high efficiency and high purity of polysaccharide.
Description
Technical Field
The invention relates to a polysaccharide extraction technology, in particular to a method for extracting hericium erinaceus polysaccharide.
Background
Hericium erinaceus is a large fleshy fungus commonly seen in the section or the tree hole of a broad-leaf trunk, turns yellow brown after being mature, is plush, is extremely similar to the brain bag of a mao monkey, and is a rare fungus with homology of medicine and food. The traditional Chinese medicine considers that the hericium erinaceus is neutral in nature and sweet in taste, is beneficial to five internal organs, helps digestion, has the effects of invigorating stomach, tonifying deficiency, resisting cancer and benefiting kidney essence, and is mainly used for treating symptoms such as loose stool, gastric and duodenal ulcer, superficial gastritis, neurasthenia, esophageal cancer, gastric cancer and the like. Hericium erinaceus is a medical and edible fungus, has been advocated by nutriologists and medical scientists all the time, and is a food deeply loved by consumers.
The hericium erinaceus polysaccharide is a main active ingredient of hericium erinaceus, has various physiological functions of improving immunity, resisting tumors, resisting aging, reducing blood fat and the like, is widely applied to the fields of medicines, functional foods, chemical industry and the like at present, and has wide market prospect.
At present, various extraction methods of hericium erinaceus polysaccharide are developed, such as hot water extraction, acid extraction, alkaline extraction, microwave-assisted extraction, ultrasonic-assisted extraction, enzymolysis and the like. The acid leaching method and the alkali leaching method have high polysaccharide extraction rate, but have high requirements on equipment, and the molecular structure of the polysaccharide is easily damaged by acid-base conditions; the hot water extraction method is most commonly used, but the polysaccharide yield obtained by single hot water extraction is low, and the molecular structure of the polysaccharide can be damaged by long-time high-temperature treatment; the extraction methods have the problems of low extraction efficiency on one hand and insufficient purity of extracted hericium erinaceus polysaccharide on the other hand.
Disclosure of Invention
The invention aims to provide an extraction method of hericium erinaceus polysaccharide. The extraction method of Hericium erinaceus polysaccharide has high efficiency and high purity of polysaccharide.
The invention aims to be realized by the following technical scheme: a method for extracting Hericium erinaceus polysaccharide comprises:
step (1): crushing the dried hericium erinaceus in a crusher to obtain the crushing fineness of 120-300 meshes;
step (2): adding 6-10 times of water by mass, and fully stirring to form colloid;
and (3): adding the colloid into a colloid mill for further grinding;
and (4): adding petroleum ether-silica gel particle mixture in an amount which is 3-6 times the mass of the colloid, dissolving, and filtering to form filtrate and crude polysaccharide particles;
and (5): adding a petroleum ether-silica gel particle mixture of which the mass is 10-15 times that of the crude polysaccharide particles, dissolving, and filtering to form secondary filtrate and purified crude polysaccharide particles;
and (6): adding 10-20 times of hot water at 40-80 deg.C into the purified crude polysaccharide particles, and soaking to obtain first extractive solution; ultrasonic soaking for 30-50 min;
and (7): filtering to obtain residue, and performing CO2 supercritical extraction on the residue to obtain second extractive solution;
and (8) carrying out resin decoloration and ultrafiltration on the primary extracting solution and the secondary extracting solution to obtain the hericium erinaceus polysaccharide.
After adopting above-mentioned technical scheme, the hedgehog hydnum mushroom is the bacterial strain biology, not only includes the hedgehog hydnum mushroom polysaccharide in the hedgehog hydnum mushroom, still includes numerous lipids, insoluble organic matter and other granule impurity. Therefore, the difficulty of separating and purifying the hericium erinaceus polysaccharide is high, the separation difficulty is greatly increased due to the similar properties of various organic matters, and the purity after purification cannot reach a high level.
In order to solve the problems, the invention designs an industrialized extraction method of hericium erinaceus polysaccharide. Wherein,
the hericium erinaceus is crushed in the step (1), and the fineness of the hericium erinaceus is controlled to be 120-mesh and 300-mesh, so that the primary crushing fineness is kept at a finer level. And (3) adding water in the step (2) to carry out colloid existing in particles in different states, and laying a foundation for further grinding. And (3) further grinding to obtain larger fineness. And (4) adding a petroleum ether-silica gel particle mixture. The petroleum ether-silica gel particle mixture with 3-6 times of the mass can be screened to wash away particle impurities, and meanwhile, part of organic matters with smaller molecular weight, such as lipid matters, can be dissolved for primary purification. And (5) further increasing the usage amount of the petroleum ether-silica gel particle mixture, so that organic matters with small molecular weight in an internal organic system are fully filtered. And (6) adding hot water for soaking, and obtaining the polysaccharide extracting solution by using a hot water soaking method. And (7) extracting the filtered residue, recycling the waste, and fully extracting polysaccharide in the residue. And (8) performing post-treatment to obtain the hericium erinaceus polysaccharide.
The hericium erinaceus comprises the following components: hericium erinaceus ketone, hericium erinaceus alkaloid, polysaccharide, volatile oil, protein, fat, crude fiber, carotene, B vitamins, calcium, phosphorus, iron, amino acid and the like.
The industrialized hericium erinaceus extraction technology designed by the invention is characterized in that before the hot water soaking method is carried out, an organic system in the hericium erinaceus is firstly destroyed, and lipid substances and impurities in the hericium erinaceus are filtered, so that the extraction purity of the hericium erinaceus polysaccharide is further improved. The reason is that the hot water immersion method mainly enables hericium erinaceus polysaccharide to be dissolved in hot water and then crystallized and purified, but the lipid can be attached to the surface of hot water, and meanwhile, the lipid has certain solubility in the hot water, so that the purity of later-stage purification is influenced. Meanwhile, the silica gel particles have better adsorbability. In the whole system, petroleum ether is adsorbed on the silica gel particles at the beginning, so that the petroleum ether is not easy to be attached to hericium erinaceus polysaccharide molecules.
The invention is further configured to: the following steps are arranged between the step (5) and the step (6): adding 5-10 mass times of 35% -60% ethanol water solution into the purified crude polysaccharide particles, stirring, standing for 5-10min, and filtering to obtain secondary purified crude polysaccharide particles and tertiary filtrate.
After the technical scheme is adopted, since the petroleum ether-silica gel particle mixture has certain dangerousness, in order to reduce the dangerousness of the petroleum ether-silica gel particle mixture and carry out subsequent purification, the step (6) of adding the ethanol aqueous solution is designed. Because the hericium erinaceus polysaccharide is insoluble in ethanol, the petroleum ether-silica gel particle mixture is quickly dissolved after the ethanol aqueous solution is added, so that the petroleum ether-silica gel particle mixture in the solution is removed, and the danger is reduced. Meanwhile, after the petroleum ether-silica gel particle mixture is added with ethanol, the petroleum ether is absorbed by the ethanol, the silica gel particles have certain adsorbability again, and oil in the hericium erinaceus, hericium erinaceus alkali, hericium erinaceus ketone and other small molecules are adsorbed to further remove impurities in the hericium erinaceus. Protein and fat are dissolved by ethanol and petroleum ether, while the solubility of polysaccharide is lower, so that the ratio of polysaccharide in the system is increased.
The invention is further configured to: the concentration of the ethanol water solution is 45 percent.
By adopting the technical scheme, the concentration of the ethanol water solution is designed to be 45%. Generally, in order to improve the solubility of hericium erinaceus in hot water, a conventional method is to add an ethanol solution with the concentration of 95%, and the high-concentration ethanol solution can improve the dissolving amount of polysaccharide in ethanol organic matters, so that the dissolving amount of hericium erinaceus polysaccharide is improved, and more polysaccharide is purified. The invention uses low-concentration ethanol water solution, and aims to dissolve the hericium erinaceus polysaccharide in the ethanol water solution as little as possible instead of dissolving the hericium erinaceus polysaccharide in the ethanol water solution. The ethanol aqueous solution added in the invention is mainly used for removing the petroleum ether-silica gel particle mixture and ensuring the safety.
The invention is further configured to: the standing time is 5 min.
By adopting the technical scheme, when the standing time is set to be 5min, the ethanol molecules in the ethanol water solution reach the surfaces of the polysaccharide molecules of the hericium erinaceus, and the petroleum ether-silica gel particle mixture molecules attached to the surfaces of the polysaccharide molecules are removed. The effect is optimal within 5min, so that the petroleum ether-silica gel particle mixture molecules are quickly removed, the ethanol water solution can further dissolve lipid and micromolecular organic matters, macromolecular insoluble matters are filtered and removed, and the proportion of the hericium erinaceus polysaccharide in the system is further improved.
The invention is further configured to: the standing time is 8 min.
By adopting the technical scheme, the removal rate of the petroleum ether-silica gel particle mixture is maximized when the standing time is 8 min.
The invention is further configured to: the extraction pressure is 25MPa, the extraction temperature is 50 ℃, and the extraction time is 2-5 h.
By adopting the technical scheme, the extraction temperature is set to be 50%, the polysaccharide is prevented from being thermally decomposed at a higher temperature, and the loss of the hericium erinaceus polysaccharide is reduced.
The invention is further configured to: the ultrasonic soaking time is 45 min.
By adopting the technical scheme, when the ultrasonic soaking time is 45min, the dissolution amount of the hericium erinaceus polysaccharide in hot water is maximum.
The invention is further configured to: the ultrasonic soaking time is 50 min.
By adopting the technical scheme, when the ultrasonic soaking time is 50min, the dissolution amount of the hericium erinaceus polysaccharide in hot water cannot continuously rise.
The invention is further configured to: the hot water temperature was 50 ℃.
By adopting the technical scheme, the dissolution amount of the hericium erinaceus is the largest when the temperature of hot water is 50 ℃.
The invention is further configured to: the material ratio of the petroleum ether to the silica gel particles is 1: 15.
By adopting the technical scheme, the dosage of the silica gel particles is controlled, and the cost is reduced.
In summary, the present invention has the following advantageous objects: the extraction method of Hericium erinaceus polysaccharide has high efficiency and high purity of polysaccharide.
Detailed Description
The present embodiment is only for explaining the present invention, and it is not limited to the present invention, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present invention.
Example 1:
a method for extracting hericium erinaceus polysaccharide is characterized by comprising the following steps: the method comprises the following steps:
step (1): putting the dried hericium erinaceus into a grinder to be ground, wherein the grinding fineness is 150 meshes;
step (2): adding 6 mass times of water, and fully stirring to form a colloid;
and (3): adding the colloid into a colloid mill for further grinding;
and (4): adding petroleum ether-silica gel particle mixture in an amount which is 3 times the mass of the colloid, dissolving, and filtering to form filtrate and crude polysaccharide particles;
and (5): adding a petroleum ether-silica gel particle mixture in an amount which is 10 times the mass of the crude polysaccharide particles, dissolving, and filtering to form secondary filtrate and purified crude polysaccharide particles;
and (6): and adding 5 mass times of 35% ethanol aqueous solution into the purified crude polysaccharide particles, stirring, standing for 5min, and filtering to obtain secondary purified crude polysaccharide particles and third filtrate.
And (7): adding hot water with the temperature of 40 and the mass time of 10 into the purified crude polysaccharide particles for soaking to form a first extracting solution; the ultrasonic soaking time is 30 min;
and (8): filtering to obtain residue, and performing CO2 supercritical extraction on the residue to obtain second extractive solution;
and (9) carrying out resin decoloration and ultrafiltration on the primary extracting solution and the secondary extracting solution to obtain the hericium erinaceus polysaccharide.
Example 2:
a method for extracting hericium erinaceus polysaccharide is characterized by comprising the following steps: the method comprises the following steps:
step (1): putting the dried hericium erinaceus into a grinder to be ground, wherein the grinding fineness is 150 meshes;
step (2): adding 7 times of water by mass, and fully stirring to form a colloid;
and (3): adding the colloid into a colloid mill for further grinding;
and (4): adding a petroleum ether-silica gel particle mixture with the mass of 4 times of that of the colloid, dissolving, and filtering to form filtrate and crude polysaccharide particles;
and (5): adding 11 mass times of petroleum ether-silica gel particle mixture into the crude polysaccharide particles, dissolving, and filtering to form secondary filtrate and purified crude polysaccharide particles;
and (6): adding 6 mass times of 40% ethanol water solution into the purified crude polysaccharide particles, stirring, standing for 6min, and filtering to obtain secondary purified crude polysaccharide particles and third filtrate.
And (7): adding hot water with the mass being 12 times of the temperature of 45 ℃ into the purified crude polysaccharide particles for soaking to form a first extracting solution; the ultrasonic soaking time is 35 min;
and (8): filtering to obtain residue, and performing CO2 supercritical extraction on the residue to obtain second extractive solution;
and (9) carrying out resin decoloration and ultrafiltration on the primary extracting solution and the secondary extracting solution to obtain the hericium erinaceus polysaccharide.
Example 3:
a method for extracting hericium erinaceus polysaccharide is characterized by comprising the following steps: the method comprises the following steps:
step (1): putting the dried hericium erinaceus into a grinder to be ground, wherein the grinding fineness is 150 meshes;
step (2): adding 8 times of water by mass, and fully stirring to form a colloid;
and (3): adding the colloid into a colloid mill for further grinding;
and (4): adding a petroleum ether-silica gel particle mixture with the mass of 4.5 times of that of the colloid, dissolving, and filtering to form filtrate and crude polysaccharide particles;
and (5): adding a petroleum ether-silica gel particle mixture in an amount which is 13 times the mass of the crude polysaccharide particles, dissolving, and filtering to form secondary filtrate and purified crude polysaccharide particles;
and (6): adding 8 mass times of 45% ethanol water solution into the purified crude polysaccharide particles, stirring, standing for 8min, and filtering to obtain secondary purified crude polysaccharide particles and third filtrate.
And (7): adding hot water with the mass time of 15 at the temperature of 50 ℃ into the purified crude polysaccharide particles for soaking to form a first extracting solution; the ultrasonic soaking time is 40 min;
and (8): filtering to obtain residue, and performing CO2 supercritical extraction on the residue to obtain second extractive solution;
and (9) carrying out resin decoloration and ultrafiltration on the primary extracting solution and the secondary extracting solution to obtain the hericium erinaceus polysaccharide.
Example 4:
a method for extracting hericium erinaceus polysaccharide is characterized by comprising the following steps: the method comprises the following steps:
step (1): putting the dried hericium erinaceus into a grinder to be ground, wherein the grinding fineness is 150 meshes;
step (2): adding 9 times of water by mass, and fully stirring to form a colloid;
and (3): adding the colloid into a colloid mill for further grinding;
and (4): adding a petroleum ether-silica gel particle mixture of which the mass is 5 times that of the colloid, dissolving, and filtering to form filtrate and crude polysaccharide particles;
and (5): adding a petroleum ether-silica gel particle mixture with the mass of 14 times of that of the crude polysaccharide particles, dissolving, and filtering to form secondary filtrate and purified crude polysaccharide particles;
and (6): adding 9 mass times of 55% ethanol water solution into the purified crude polysaccharide particles, stirring, standing for 9min, and filtering to obtain secondary purified crude polysaccharide particles and third filtrate.
And (7): adding hot water with the temperature of 70 ℃ and the mass time of 18 into the purified crude polysaccharide particles for soaking to form a first extracting solution; the ultrasonic soaking time is 48 min;
and (8): filtering to obtain residue, and performing CO2 supercritical extraction on the residue to obtain second extractive solution;
and (9) carrying out resin decoloration and ultrafiltration on the primary extracting solution and the secondary extracting solution to obtain the hericium erinaceus polysaccharide.
Example 5:
a method for extracting hericium erinaceus polysaccharide is characterized by comprising the following steps: the method comprises the following steps:
step (1): putting the dried hericium erinaceus into a grinder to be ground, wherein the grinding fineness is 150 meshes;
step (2): adding 10 mass times of water, and fully stirring to form colloid;
and (3): adding the colloid into a colloid mill for further grinding;
and (4): adding a petroleum ether-silica gel particle mixture with the mass of 6 times of the colloid, dissolving, and filtering to form filtrate and crude polysaccharide particles;
and (5): adding 15 mass times of petroleum ether-silica gel particle mixture into the crude polysaccharide particles, dissolving, and filtering to form secondary filtrate and purified crude polysaccharide particles;
and (6): adding 10 mass times of 60% ethanol water solution into the purified crude polysaccharide particles, stirring, standing for 10min, and filtering to obtain secondary purified crude polysaccharide particles and third filtrate.
And (7): adding hot water with the temperature of 80 ℃ and the mass time of 20 into the purified crude polysaccharide particles for soaking to form a first extracting solution; the ultrasonic soaking time is 50 min;
and (8): filtering to obtain residue, and performing CO2 supercritical extraction on the residue to obtain second extractive solution;
and (9) carrying out resin decoloration and ultrafiltration on the primary extracting solution and the secondary extracting solution to obtain the hericium erinaceus polysaccharide.
Comparative example: the hericium erinaceus polysaccharide is prepared by a method for extracting the hericium erinaceus polysaccharide by using a common hot water soaking method.
The experimental method comprises the following steps:
the experiment groups 1 to 5 are respectively the experiment group 1 to the experiment group 5, and the comparative example is the control group, wherein, each group quantitatively controls 50g of hericium erinaceus to carry out the experiment.
The data are shown in table 1:
TABLE 1 Experimental groups 1-5, control group experimental data table
Wherein the solid-to-liquid ratio of the petroleum ether-silica gel particle mixture is 1: 15.
determining the conditions, respectively dissolving in 95% ethanol 20 times by mass under laboratory conditions, stirring thoroughly until no particulate organic matter is present, and measuring polysaccharide content in the experimental group 1-5 and the control group by HPLC OR GC (high performance liquid chromatography).
Experimental test data are shown in table 2:
in conclusion, the experimental data show that the extraction purity of the hericium erinaceus polysaccharide is improved by the extraction method of the hericium erinaceus polysaccharide, the process is simple, and the method is suitable for industrial production.
Claims (10)
1. A method for extracting hericium erinaceus polysaccharide is characterized by comprising the following steps: the method comprises the following steps:
step (1): crushing the dried hericium erinaceus in a crusher to obtain the crushing fineness of 120-300 meshes;
step (2): adding 6-10 times of water by mass, and fully stirring to form colloid;
and (3): adding the colloid into a colloid mill for further grinding;
and (4): adding petroleum ether-silica gel particle mixture in an amount which is 3-6 times the mass of the colloid, dissolving, and filtering to form filtrate and crude polysaccharide particles;
and (5): adding a petroleum ether-silica gel particle mixture of which the mass is 10-15 times that of the crude polysaccharide particles, dissolving, and filtering to form secondary filtrate and purified crude polysaccharide particles;
and (6): adding 10-20 times of hot water at 40-80 deg.C into the purified crude polysaccharide particles, and soaking to obtain first extractive solution; ultrasonic soaking for 30-50 min;
and (7): filtering to obtain residue, and performing CO2 supercritical extraction on the residue to obtain second extractive solution;
and (8) carrying out resin decoloration and ultrafiltration on the primary extracting solution and the secondary extracting solution to obtain the hericium erinaceus polysaccharide.
2. The extraction method of hericium erinaceus polysaccharide as claimed in claim 1, which is characterized in that: the following steps are arranged between the step (5) and the step (6): adding 5-10 mass times of 35% -60% ethanol water solution into the purified crude polysaccharide particles, stirring, standing for 5-10min, and filtering to obtain secondary purified crude polysaccharide particles and tertiary filtrate.
3. The extraction method of hericium erinaceus polysaccharide as claimed in claim 2, which is characterized in that: the concentration of the ethanol water solution is 45 percent.
4. The extraction method of hericium erinaceus polysaccharide as claimed in claim 3, which is characterized in that: the standing time is 5 min.
5. The extraction method of hericium erinaceus polysaccharide as claimed in claim 3, which is characterized in that: the standing time is 8 min.
6. The extraction method of hericium erinaceus polysaccharide as claimed in claim 1, which is characterized in that: the extraction pressure is 25MPa, the extraction temperature is 50 ℃, and the extraction time is 2-5 h.
7. The extraction method of hericium erinaceus polysaccharide as claimed in claim 1, which is characterized in that: the ultrasonic soaking time is 45 min.
8. The extraction method of hericium erinaceus polysaccharide as claimed in claim 1, which is characterized in that: the ultrasonic soaking time is 50 min.
9. The extraction method of hericium erinaceus polysaccharide as claimed in claim 1, which is characterized in that: the hot water temperature was 50 ℃.
10. The extraction method of hericium erinaceus polysaccharide as claimed in claim 1, which is characterized in that: the material ratio of the petroleum ether to the silica gel particles is 1: 15.
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Citations (3)
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| CN102627789A (en) * | 2012-03-31 | 2012-08-08 | 中华全国供销合作总社济南果品研究院 | Preparation process for edible fungus compound polysaccharide |
| CN104531803A (en) * | 2014-12-24 | 2015-04-22 | 刘桂香 | Production method of fine flour with high active hericium erinaceus polysaccharide content and comprehensive utilization method of byproduct of fine flour |
| CN106883304A (en) * | 2017-03-06 | 2017-06-23 | 南昌大学 | Heterogeneity polysaccharide is comprehensively prepared and purification process in a kind of Hericium erinaceus |
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| CN102627789A (en) * | 2012-03-31 | 2012-08-08 | 中华全国供销合作总社济南果品研究院 | Preparation process for edible fungus compound polysaccharide |
| CN104531803A (en) * | 2014-12-24 | 2015-04-22 | 刘桂香 | Production method of fine flour with high active hericium erinaceus polysaccharide content and comprehensive utilization method of byproduct of fine flour |
| CN106883304A (en) * | 2017-03-06 | 2017-06-23 | 南昌大学 | Heterogeneity polysaccharide is comprehensively prepared and purification process in a kind of Hericium erinaceus |
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