CN112592413B - Preparation method of wild buckwheat rhizome polysaccharide - Google Patents
Preparation method of wild buckwheat rhizome polysaccharide Download PDFInfo
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- 150000004676 glycans Chemical class 0.000 title claims abstract description 55
- 229920001282 polysaccharide Polymers 0.000 title claims abstract description 55
- 239000005017 polysaccharide Substances 0.000 title claims abstract description 55
- 244000248416 Fagopyrum cymosum Species 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000000243 solution Substances 0.000 claims abstract description 79
- 238000000605 extraction Methods 0.000 claims abstract description 32
- 239000007864 aqueous solution Substances 0.000 claims abstract description 25
- 238000000967 suction filtration Methods 0.000 claims abstract description 19
- 239000006228 supernatant Substances 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 8
- 239000002253 acid Substances 0.000 claims abstract description 7
- 238000010298 pulverizing process Methods 0.000 claims abstract description 7
- 238000005119 centrifugation Methods 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims description 23
- 239000000463 material Substances 0.000 claims description 20
- 239000007787 solid Substances 0.000 claims description 17
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 15
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- OVARTBFNCCXQKS-UHFFFAOYSA-N propan-2-one;hydrate Chemical compound O.CC(C)=O OVARTBFNCCXQKS-UHFFFAOYSA-N 0.000 claims description 7
- 235000010852 Fagopyrum cymosum Nutrition 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- 239000003929 acidic solution Substances 0.000 claims 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 abstract description 38
- 230000001376 precipitating effect Effects 0.000 abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 8
- 239000000284 extract Substances 0.000 abstract description 7
- 229930014626 natural product Natural products 0.000 abstract description 2
- 239000003814 drug Substances 0.000 description 11
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 238000001556 precipitation Methods 0.000 description 5
- 229940079593 drug Drugs 0.000 description 4
- 239000003513 alkali Substances 0.000 description 3
- 238000007796 conventional method Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 3
- 239000003208 petroleum Substances 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- 238000002791 soaking Methods 0.000 description 3
- 241000196324 Embryophyta Species 0.000 description 2
- 238000005238 degreasing Methods 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 201000003453 lung abscess Diseases 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 208000024172 Cardiovascular disease Diseases 0.000 description 1
- 206010020751 Hypersensitivity Diseases 0.000 description 1
- 206010061218 Inflammation Diseases 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- 206010037660 Pyrexia Diseases 0.000 description 1
- 206010044302 Tracheitis Diseases 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 208000026935 allergic disease Diseases 0.000 description 1
- 230000007815 allergy Effects 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000001093 anti-cancer Effects 0.000 description 1
- 230000002790 anti-mutagenic effect Effects 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 230000000259 anti-tumor effect Effects 0.000 description 1
- 230000000840 anti-viral effect Effects 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 201000011510 cancer Diseases 0.000 description 1
- 239000002775 capsule Substances 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 230000003467 diminishing effect Effects 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000012869 ethanol precipitation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 230000007760 free radical scavenging Effects 0.000 description 1
- 235000013376 functional food Nutrition 0.000 description 1
- 235000013402 health food Nutrition 0.000 description 1
- 235000008216 herbs Nutrition 0.000 description 1
- 230000004054 inflammatory process Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000000144 pharmacologic effect Effects 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000003495 polar organic solvent Substances 0.000 description 1
- 239000002798 polar solvent Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000003405 preventing effect Effects 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 230000001225 therapeutic effect Effects 0.000 description 1
- 229940126672 traditional medicines Drugs 0.000 description 1
- 238000003809 water extraction Methods 0.000 description 1
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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
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/125—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives containing carbohydrate syrups; containing sugars; containing sugar alcohols; containing starch hydrolysates
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/70—Carbohydrates; Sugars; Derivatives thereof
- A61K31/7088—Compounds having three or more nucleosides or nucleotides
- A61K31/713—Double-stranded nucleic acids or oligonucleotides
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/70—Polygonaceae (Buckwheat family), e.g. spineflower or dock
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
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Abstract
The invention discloses a preparation method of wild buckwheat rhizome polysaccharide. Belongs to the technical field of natural product extraction. The method comprises the following steps: pulverizing rhizoma Fagopyri Dibotryis residue, or extracting rhizoma Fagopyri Dibotryis residue; adding an alkaline aqueous solution with the mass concentration of 0.1-10%, and performing extraction treatment to obtain an extraction solution; concentrating the supernatant of the extractive solution under reduced pressure to obtain concentrated solution; adding ethanol into the concentrated solution, adjusting the mass concentration to 60-90%, and precipitating to obtain crude polysaccharide; or adding the concentrated solution into an acid solution with the mass concentration of 5-36% to adjust the pH value to 0-5, and performing suction filtration or centrifugation to obtain the wild buckwheat rhizome crude polysaccharide. The invention can extract the wild buckwheat rhizome polysaccharide for many times, has higher total sugar content than that directly extracted by the water solution in the prior art, and can improve the utilization rate of the wild buckwheat rhizome.
Description
Technical Field
The invention relates to the technical field of natural product extraction, in particular to a preparation method of wild buckwheat rhizome polysaccharide.
Background
The wild buckwheat rhizome is a traditional Chinese medicine with homology of medicine and food, is a variety accepted in both Chinese pharmacopoeia and veterinary pharmacopoeia, and is used as a root and stem medicine. The tablet and capsule of the extract of the Chinese patent medicine are approved to be human therapeutic medicines, powder and the like are used as veterinary medicines, and meanwhile, the health food is used as one of the components.
The product is traditionally used for treating lung abscess, and the modern literature reports show that the main pharmacological activity of the product is stronger antioxidation, free radical scavenging, antimutagenic, cardiovascular disease preventing, antibacterial, antiviral, anticancer and antitumor, and the like, and the product has the efficacies of reducing blood sugar, resisting cancer, treating tracheitis, treating lung abscess and other diseases, relieving fever, diminishing inflammation, resisting allergy and the like.
Most of the extracts of the approved medicines reported in the literature are alcohol extracts, while the traditional medicines are water decoction. After extraction or decoction residues are generally discarded, the wild buckwheat is a national secondary protection plant, and the existing treatment mode is relatively waste.
Therefore, it is an urgent need to solve the problem of providing a preparation method for further extracting active substances from fagopyrum cymosum.
Disclosure of Invention
In view of the above, the invention provides a preparation method of wild buckwheat rhizome polysaccharide, which fully utilizes natural resources and secondarily develops and utilizes medicinal dregs after medicinal extraction. The wild buckwheat rhizome is rich in polysaccharide, and polysaccharide substances of wild buckwheat rhizome can be further extracted from medicinal extraction material residues by a water extraction method, and particularly, alkali-soluble polysaccharide can be obtained by extracting with an alkaline solution by the method provided by the invention.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of wild buckwheat rhizome polysaccharide comprises the following steps:
(1) pulverizing rhizoma Fagopyri Dibotryis residue, or extracting rhizoma Fagopyri Dibotryis residue; adding an alkaline aqueous solution with the mass concentration of 0.1-10%, and performing extraction treatment to obtain an extraction solution C2;
(2) concentrating the supernatant of the extractive solution C2 under reduced pressure to obtain concentrated solution D;
adding ethanol into the concentrated solution D, adjusting the mass concentration to 60-90%, and precipitating to obtain crude polysaccharide A2;
or the like, or, alternatively,
and adding the concentrated solution D into an acid solution with the mass concentration of 5-36% to adjust the pH value to 0-5, and performing suction filtration or centrifugation to obtain the wild buckwheat rhizome crude polysaccharide A3.
Has the advantages that: the medicine residue is the medicine residue after the extraction of the medicinal material decoction pieces (residues of the wild buckwheat rhizome medicinal material decoction pieces are extracted by various production enterprises according to the production process requirements of wild buckwheat rhizome products), so that the waste can be reduced, and the polysaccharide in the material can be fully extracted.
Preferably: the preparation method of the residue after wild buckwheat rhizome extraction comprises the following steps: pulverizing rhizoma Fagopyri Dibotryis, adding acetone water solution or ethanol water solution, stirring, and vacuum filtering to obtain extractive solution and residual solid; extracting the rest solid twice, mixing extractive solutions to obtain C1, and collecting residue after rhizoma Fagopyri Dibotryis extraction.
Preferably: the preparation method of the residue after wild buckwheat rhizome extraction also comprises the following steps: concentrating the extractive solution C1 under reduced pressure, collecting supernatant, adding ethanol, standing for precipitation, and filtering to obtain rhizoma Fagopyri Dibotryis crude polysaccharide A1.
Has the advantages that: suction filtration can be used for degreasing and removing phenols and other substances, thereby further facilitating polysaccharide extraction.
Preferably: in the preparation method of the residue after the wild buckwheat rhizome is extracted, the volume concentration of an acetone aqueous solution or an ethanol aqueous solution is 5-60%;
the mass volume ratio of the wild buckwheat rhizome to the acetone aqueous solution or the ethanol aqueous solution is 1: (3-10) Kg/L;
the stirring condition is that the rotating speed is 50-200 r/min at the temperature of 25-90 ℃, and the stirring time is more than or equal to 1 h;
concentrating under reduced pressure at 30-60 deg.C under 400-600 mmHg at stirring speed of 20-200 r/min until the volume of extractive solution C1 is 1/10-1/3;
adding ethanol to a concentration of above 70%.
Preferably: the alkaline aqueous solution in the step (1) is sodium hydroxide aqueous solution or potassium hydroxide aqueous solution or ammonia water; the mass volume ratio of the wild buckwheat rhizome dregs or the wild buckwheat rhizome extraction residues to the alkaline aqueous solution is 1: (3-50) g/ml.
Preferably: the extraction treatment in the step (1) is soaking, the temperature is 30-90 ℃, and the soaking time is 1-5 days; or, the extraction treatment is stirring, the temperature is 30-90 ℃, and the stirring time is more than or equal to 1 h;
wherein the stirring speed is 50-200 r/min;
and after soaking or stirring, performing suction filtration, repeatedly extracting the residual solid for 2-3 times, and combining filtrates to obtain an extraction solution C2.
Preferably: and (3) concentrating under reduced pressure in the step (2) at the temperature of 30-60 ℃, under the pressure of 400-600 mmHg, stirring at the speed of 20-200 r/min, and concentrating to 1/10-1/2 of the volume of the extracting solution C2.
Preferably: the acid solution in the step (2) is hydrochloric acid, sulfuric acid or nitric acid; the centrifugal rotating speed is 1000-10000 rpm, and the time is 10-240 min.
Preferably: the crushing degree of the wild buckwheat rhizome dregs or the crushing degree of the wild buckwheat rhizome is 20-80 meshes; the suction filtration is performed by using a filter material with the aperture of 3-30 mu m.
The invention also provides application of the wild buckwheat rhizome polysaccharide prepared by the method in preparing functional food, health-care products or medicines.
According to the technical scheme, compared with the prior art, the preparation method of the wild buckwheat rhizome polysaccharide has the technical effects that the wild buckwheat rhizome is subjected to organic solvent petroleum ether (industrial purity) or high-purity ethanol and the like, degreasing and pigment removal are carried out on the wild buckwheat rhizome, then the polysaccharide is extracted by water, the polysaccharide content of the polysaccharide extract is higher, and the polysaccharide can be extracted in multiple steps, the wild buckwheat rhizome is extracted by (5% -60%) acetone water or (5% -60%) ethanol water solution, the filtrate is subjected to reduced pressure concentration and alcohol precipitation to obtain the polysaccharide A1 with the extraction rate of about 3%, and the total sugar content of the polysaccharide A1 is about 25%; further, the polysaccharide A2 is obtained by extracting polysaccharide with alkali liquor and precipitating with ethanol, the extraction rate is about 13%, and the total sugar content is more than 30%; the extraction rate of polysaccharide A3 is about 5% by extracting polysaccharide with alkali solution and precipitating with acid, and the total sugar content is above 70%.
Detailed Description
The following will clearly and completely describe the technical solutions in 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 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 discloses a preparation method of wild buckwheat rhizome polysaccharide.
Example 1
Taking 0.5Kg of dried wild buckwheat rhizome dregs (abandoned dregs of medicine enterprises), adding 2.5L of 0.1% sodium hydroxide aqueous solution, heating to 30 ℃, stirring for 2 hours at the rotating speed of 50r/min, carrying out suction filtration (using filter material with aperture of 3 mu m, centrifugal rotating speed of 1000rpm, time of 10min), repeatedly extracting solid residues for 2 times by using the solution and conditions, combining the extracted solutions, decompressing to 400 mm Hg at 30 ℃ under the condition of rotating speed of 20r/min, concentrating to 1/10 of the solution volume, taking supernatant of concentrated solution, adding 5% hydrochloric acid solution to adjust pH to 2, separating out precipitate, and carrying out suction filtration (using filter material with aperture of 3 mu m, centrifugal rotating speed of 1000rpm, time of 10min) to obtain alkali-soluble wild buckwheat rhizome crude polysaccharide A1.
Example 2
Taking 0.5Kg of dried wild buckwheat rhizome dregs (abandoned dregs of medicinal plants), adding 2.5L of 5% sodium hydroxide aqueous solution, heating to 50 ℃, stirring for 2 hours at the rotating speed of 100r/min, performing suction filtration (using filter material with the aperture of 15 mu m for suction filtration, the centrifugal rotating speed of 3000rpm, the time of 120min), repeatedly extracting the solid residues for 2 times by using the solution and the conditions, combining the extracted solutions, decompressing to 500 mm Hg at the temperature of 40 ℃, concentrating to 1/8 of the solution volume at the rotating speed of 120r/min, taking the supernatant of the concentrated solution, adding 10% hydrochloric acid solution to adjust the pH to 2, separating out the precipitate, centrifuging at the rotating speed of 1000rpm, and obtaining the alkali-soluble wild buckwheat rhizome crude polysaccharide A1 after 120 min.
Example 3
Taking 0.5Kg of dried wild buckwheat rhizome dregs (abandoned dregs of medicinal herbs), adding 2.5L of 10% sodium hydroxide aqueous solution, heating to 90 ℃, stirring for 2 hours at the rotating speed of 50r/min, performing suction filtration (using filter material with aperture of 30 mu m for suction filtration, centrifugal rotating speed of 10000rpm, time of 240min), repeatedly extracting the solid residues for 2 times by using the solution and the conditions, combining the extracted solutions, performing concentration to 1/2 of the volume of the solution at the temperature of 60 ℃ under the condition of decompression to 600mm Hg at the rotating speed of 200r/min, taking supernatant of the concentrated solution, adding 36% hydrochloric acid solution to adjust the pH to 2, separating out precipitates, and performing suction filtration (using filter material with aperture of 30 mu m for suction filtration, centrifugal rotating speed of 10000rpm, time of 240min) to obtain the wild buckwheat rhizome crude polysaccharide A1.
Example 4
Pulverizing dried rhizoma Fagopyri Dibotryis 1Kg to 20 mesh, adding 3L 5% acetone water solution, stirring at 25 deg.C and 50r/min for at least 1 hr, vacuum filtering (using filter material with 3 μm pore diameter, centrifuging at 1000rpm for 10min) to obtain extractive solution, extracting the rest solid materials twice, and mixing extractive solutions to obtain filter residue (drying by conventional method).
Concentrating the extractive solution at 30 deg.C under reduced pressure to 400 mm Hg at 20r/min to 1/10, collecting supernatant, adding ethanol to concentration of above 70%, standing for precipitation, and vacuum filtering (using filter material with aperture of 3 μm, centrifugal rotation speed of 1000rpm, and time of 10min) to obtain crude rhizoma Fagopyri Dibotryis polysaccharide A1.
Taking 0.5Kg of dried filter residue, adding 2.5L of 0.1% potassium hydroxide aqueous solution, heating to 30 ℃, stirring at the rotating speed of 50r/min for 2 hours, performing suction filtration (using filter material with the aperture of 3 mu m for suction filtration, the centrifugal rotating speed of 1000rpm, the time of 10min), repeatedly extracting the solid residues for 2 times by using the solution and the conditions, combining the extracted solutions, decompressing to 400 mm Hg at the temperature of 30 ℃, concentrating at the rotating speed of 20r/min to 1/10 of the volume of the solution, taking the supernatant of the concentrated solution, adding 36% acid solution with mass concentration to adjust the pH to 3, and centrifuging (the centrifugal rotating speed of 1000-10000 rpm, the time of 10-240 min) to obtain the wild buckwheat rhizome crude polysaccharide A3.
Example 5
Pulverizing dried rhizoma Fagopyri Dibotryis 1Kg to 80 mesh, adding 10L 60% acetone water solution, stirring at 90 deg.C and 200r/min for at least 1 hr, vacuum filtering (using filter material with 30 μm pore diameter, centrifuging at 10000rpm, and centrifuging for 240min) to obtain extractive solution, extracting the rest solid twice, and mixing extractive solutions to obtain filter residue (drying by conventional method).
And (3) decompressing the extracting solution to 600mm Hg at 60 ℃, concentrating the extracting solution to 1/3 of the volume of the solution under the condition of the rotating speed of 200r/min, taking the supernatant of the concentrated solution, adding ethanol to the concentration of more than 70%, standing for precipitation, and performing suction filtration (using a filter material with the aperture of 30 mu m for suction filtration, the centrifugal rotating speed of 10000rpm, and the time of 240min) to obtain the wild buckwheat rhizome crude polysaccharide A1.
Taking 0.5Kg of dried filter residue, adding 2.5L of 10% potassium hydroxide aqueous solution, heating to 90 deg.C, stirring at 200r/min for 2 hours, suction filtering (using filter material with aperture of 30 μm, centrifugal rotation speed 10000rpm, time 240min), repeatedly extracting solid residue with the above solution and conditions for 3 times, mixing the extractive solutions, decompressing to 600mm Hg at 60 deg.C, concentrating at 200r/min to 1/2 of solution volume, taking the supernatant of the concentrated solution, adding ethanol to concentration of 70%, standing and precipitating to obtain crude rhizoma Fagopyri Dibotryis polysaccharide A2.
Example 6
Pulverizing dried rhizoma Fagopyri Dibotryis 1Kg to 80 mesh, adding 10L 60% acetone water solution, stirring at 90 deg.C and 200r/min for at least 1 hr, vacuum filtering (using filter material with 30 μm pore diameter, centrifuging at 10000rpm, and centrifuging for 240min) to obtain extractive solution, extracting the rest solid twice, and mixing extractive solutions to obtain filter residue (drying by conventional method).
Concentrating the extractive solution at 60 deg.C under reduced pressure to 600mm Hg at rotation speed of 200r/min to 1/3, collecting the supernatant, adding ethanol to concentration of above 70%, standing for precipitation, and vacuum filtering (using filter material with aperture of 30 μm, centrifuging at 10000rpm, and time of 240min) to obtain crude rhizoma Fagopyri Dibotryis polysaccharide A1.
Taking 0.5Kg of dried filter residue, adding 2.5L of 10% potassium hydroxide aqueous solution, heating to 90 deg.C, stirring at 200r/min for 2 hours, suction filtering (using filter material with aperture of 30 μm, centrifugal rotation speed 10000rpm, time 240min), repeatedly extracting solid residue with the above solution and conditions for 3 times, mixing the extractive solutions, decompressing to 600mm Hg at 60 deg.C, concentrating at 200r/min to 1/2 of solution volume, taking the supernatant of the concentrated solution, adding ethanol to concentration of 70%, standing and precipitating to obtain crude rhizoma Fagopyri Dibotryis polysaccharide A2.
Comparative experiment
Comparative example 1
Pretreating wild buckwheat rhizome by using an organic solvent such as petroleum ether or an ethanol aqueous solution (5-60%), directly extracting polysaccharide from the dried residual solid with water, concentrating, and precipitating with ethanol to obtain the polysaccharide.
Comparative example 2
Pretreating rhizoma Fagopyri Dibotryis with small polar solvent such as petroleum ether (industrial purity) or 95% ethanol, directly extracting polysaccharide from dried residue with water, concentrating, and precipitating with ethanol to obtain polysaccharide.
The methods of examples 1-6 and comparative examples 1-2 were used for polysaccharide extraction, and the polysaccharide content was determined as follows (taking the mean):
the extraction rate of polysaccharide extracted by water in comparative examples 1 and 2 is 4.5 percent, and the total sugar content is only 7 percent;
the extraction rate of the polysaccharide A1 extracted in examples 1-6 is 3%, but the total sugar content is 25%; the extraction rate of A2 is 13 percent, and the total sugar content is 30 percent; the extraction rate of A3 is about 5%, and the total sugar content is about 70%
The results show that: in the embodiment, a part of polysaccharide product can be obtained after extraction by using a polar organic solvent (acetone or ethanol) and water mixture, then the solid residue can be used for further extracting the polysaccharide by using an alkali solution, and the residue (dregs or solid residue after extraction by using acetone water (or ethanol water)) is subjected to direct ethanol precipitation or acid adjustment to precipitate the polysaccharide after extraction. The method can extract rhizoma Fagopyri Dibotryis polysaccharide for multiple times, has higher total sugar content than that of water solution directly extracted in the prior art, and can extract rhizoma Fagopyri Dibotryis for multiple times, and improves utilization rate and extraction amount of rhizoma Fagopyri Dibotryis.
The embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (3)
1. A preparation method of wild buckwheat rhizome polysaccharide A3 is characterized by comprising the following steps:
(1) adding an alkaline aqueous solution with the mass concentration of 0.1-10% into the residue after the wild buckwheat rhizome is extracted, heating to 30-90 ℃, stirring for more than or equal to 1 hour, carrying out suction filtration, repeatedly extracting the solid residue for 2 times by using the solution and conditions, and combining the extraction solutions; the alkaline aqueous solution is sodium hydroxide aqueous solution or potassium hydroxide aqueous solution or ammonia water; the mass-volume ratio of the residue after the wild buckwheat rhizome is extracted to the alkaline aqueous solution is 1: (3-50) g/ml, wherein the stirring speed is 50-200 r/min;
(2) concentrating the extracted solution under reduced pressure to 1/10-1/2 of the volume of the extracted solution, taking the supernatant of the concentrated solution, adding an acid solution with the mass concentration of 5-36% to adjust the pH value to 0-5, and centrifuging to obtain crude polysaccharide A3;
the preparation method of the residue after wild buckwheat rhizome extraction comprises the following steps: pulverizing rhizoma Fagopyri Dibotryis, adding acetone water solution, stirring, and vacuum filtering to obtain extractive solution and residual solid; extracting the rest solid twice, mixing extractive solutions to obtain rhizoma Fagopyri Dibotryis residue;
the volume concentration of the acetone aqueous solution is 5-60%;
the mass volume ratio of the wild buckwheat rhizome to the acetone aqueous solution is 1: (3-10) Kg/L;
the stirring condition after adding the acetone aqueous solution is that the rotation speed is 50-200 r/min at the temperature of 25-90 ℃, and the stirring time is more than or equal to 1 h.
2. The method for preparing fagopyrum cymosum polysaccharide A3 according to claim 1, wherein the acidic solution in step (2) is hydrochloric acid, sulfuric acid or nitric acid; the rotating speed of the centrifugation is 1000-10000 rpm, and the time is 10-240 min.
3. The method for preparing fagopyrum cymosum polysaccharide A3 according to any one of claims 1 to 2, wherein the ground fagopyrum cymosum rhizome is 20 to 80 mesh; and the suction filtration is performed by using a filter material with the aperture of 3-30 mu m.
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