POLYESACARIDE EXTRACTION PROCESS FROM UPPER PLANTS OR FUNGI AND POLYSACARIDE

专利摘要:
polysaccharide extraction process from higher plants or polysaccharide fungi proves to be a process for preparing water soluble polysaccharides with higher plants and fungi. the process comprises the following steps: placing residue from higher plants or fungi defatted by an organic solvent or raw material from higher plants or fungi directly sprayed in a microwave reaction chamber where the reaction occurs in the presence of an organic acid system; then distill or wash with organic solvent to remove excess acid; extract with aqueous solution, concentrate the extracted fluid, then subject to ethanol precipitation, and separate the polysaccharide precipitates. the process of this invention has the advantages of a fast processing rate, high yield and purity of polysaccharides, low consumption of organic acid and easy recycling, and low energy consumption.
公开号:BR112014010924B1
申请号:R112014010924-9
申请日:2012-11-01
公开日:2020-12-15
发明作者:Jinsong Zhang；Mingtian Li；Zhiyu Liu；Lei Xu
申请人:Shenyang Kesi High-Technology Co. Ltd；
IPC主号:

专利说明:

Technical field
[001] This invention refers to the field of pharmaceutical chemistry, it refers to a process of preparing water-soluble polysaccharides using higher plants and fungi as a raw material and, particularly, it refers to a polysaccharide extraction process of higher plants and fungi based on a chemical method that uses microwaves. Description of prior art
[002] Polysaccharides are natural macromolecular compounds that comprise a plurality of monosaccharide molecules linked through glycosidic bonds, and are one of the fundamental substances of life. In the last twenty years, with the development of molecular biology and cell biology, it has been found that polysaccharides have a variety of biological functions, polysaccharides and their conjugates are involved in cell life activities, such as specific cell recognition, they are components of a variety of antigens and drug receptors on the cell surface and participate in the activation of immune cells. Thus, polysaccharides arouse great research interest.
[003] Polysaccharides from higher plants and fungi have a long history of applications in China, and also have very abundant sources. They have become a focus and a point of excellence in research. Modern pharmacological studies indicate that these two types of polysaccharides have very important and special physiological activities, and play a central role in promoting immunity, they are antibacterial, antiviral, antiparasitic, antitumor, anti-radiation, antithrombotic, anticoagulant, anti-aging, act on inflammation, na reduction of the level of fat in the blood and improve the fertility of animals and other aspects. In addition, most polysaccharides have no direct cytotoxicity and can be used in the long term. Polysaccharides from higher plants and fungi have now become one of the most promising health care resources.
[004] Polysaccharide bioactivity largely determines the application value of polysaccharides. Constituent components, composition and spatial conformation, molecular weight and molecular weight distribution and polysaccharide water solubility are the main factors affecting biological activities Several studies show that the molecular weight of active polysaccharides is one of the necessary conditions to have biological activity.The higher molecular weights of polysaccharides and the larger apparent volumes of the molecule do not benefit the polysaccharides to pass through the various membrane barriers to perform activities biological in vivo. Another important condition is the close relationship of water-soluble polysaccharides with their molecular weight, to perform their biological activities.
[005] The very complex structure of the polysaccharides makes their synthesis extremely difficult. Currently, all active polysaccharides are extracted from natural products. Polysaccharides from higher plants and polysaccharides from fungi are extracted and isolated from different plants or from different parts of the same plant, and from the sporocarp, mycelium and mycelium fermentation broth of the fungus.
[006] There is no commonly accepted, effective and unified separation method for polysaccharide extraction. The existing processes can generally be summarized as water extraction, acid extraction, basic extraction, salt extraction and supplementary enzyme extraction. These methods have significant deficiencies in terms of aspects of polysaccharide extraction efficiency, cleaning of the production process, energy and material consumption or modification of the polysaccharide structure, etc.
[007] The technology value of the polysaccharide products obtained is not very high (particularly in: low polysaccharide purity, wide molecular weight distribution, poor water solubility, etc.), which limits the applications of high added value of polysaccharides. Specifically, existing polysaccharide extraction methods have the following problems:
[008] Aqueous extraction is generally time consuming, consumes a lot of energy, uses a large amount of extraction solvent and has low polysaccharide extraction yield.
[009] It is difficult to control the amount of strong inorganic acid, strong base and reaction time in acid / alkaline extraction, which easily causes the activity of the polysaccharide molecules to be destroyed and even causes the polysaccharides to generate molecules of small molecular weight pigment, overloading the subsequent bleaching process. In addition, after the end of the reaction, neutralization or dialysis for the acidic, alkaline solution must be done quickly, otherwise it will generate contaminated products and increase product insecurity for food and health applications. In addition, the use of non-degradable inorganic acid or base can cause serious environmental pollution in large-scale industrial production.
[010] The enzyme used in enzyme-assisted extraction is generally expensive, is often easily inactivated and has other short-term deficiencies and a low degree of purity. In the process of enzymatic hydrolysis, the ideal temperature is often on a very small scale, and small fluctuations in the reaction conditions can cause the enzyme activity to decrease significantly. Therefore, enzymatic extraction has relatively high requirements in terms of experimental conditions and still requires very complicated pre-treatment for extraction of raw materials. Enzymatic extraction technology still needs more research to be used in industrial polysaccharide extraction.
[011] There are many reasons for these difficulties. In general, polysaccharides from higher plants and fungi have high molecular weight and low solubility in water. They have a low content of plant materials and complex distribution status and distribution status, some of which are in a free state, some are linked with macromolecules like proteins and hemicellulose to form complex conjugates, some are in the cytoplasm and some are in the cell wall. The main components of plant cell walls are cellulose and other substances, including hemicellulose, pectin, lignin, etc. Cellulose has a stable supermolecular structure of the high-grade crystalline region, which is difficult to hydrolyze. The common extraction method can only apply a large number of solvents for long-term immersion, so that full plant cell expansion will loosen the compact structure and reduce the resistance to mass transfer of the active ingredients that diffuse from the cell to the solvent. Thus, conventional methods have high energy and material consumption and use polysaccharides in a free state in plants, but have poor extraction effects on polysaccharides wrapped in the cell wall or linked, in certain ways, to other macromolecules.
[012] Patent application CN03133778.3 discloses a method for fully releasing active ingredients from lucid ganoderma spores. The method places lucid ganoderma spores in a microwave reaction chamber, adds an organic acid solution, performs microwave treatment after mixing, then distills under vacuum to remove organic acid and finally uses extraction conventional aqueous solution, alcohol precipitation method to extract polysaccharides from crude lucid ganoderma spores from microwave-treated lucid ganoderma spores. In comparison with conventional extraction methods, the method exponentially increases the yield of polysaccharides (over 3 times), but presents the following main problems. First, only the use of vacuum distillation instead of additional washing with an organic solvent to remove residual acid after microwave treatment causes the resulting product to have a high residual acid content. And in the removal of oxalic acid, the calcium precipitation method is adopted, which first removes the oxalic acid from the spores by washing with water together with dissolved polysaccharide; when calcium ions are added to form calcium oxalate precipitates, a small amount of polysaccharides could be enveloped and released. Second, the mechanism is based on that increased microwave reaction between organic acid and chitin, and glial in the cell wall of lucid ganoderma spore, in order to reduce the restrictions of these substances on the release of the polysaccharide, but does not recognize the importance of breaking the chemical bond between polysaccharides and protein, cellulose, hemicellulose and chitin, and the degradation of polysaccharides in improving polysaccharide yield and water solubility.
[013] US8110677 discloses a method of microwave extraction of active polysaccharides from artemisia songarica schrenk. The method has technical flaws such as the use of a large amount of extraction solvent (water 30 to 50 times is necessary), and that enzymolysis is necessary after obtaining polysaccharides, in which enzymolysis causes many restrictions, such as the long reaction time (10 to 12 hours in the patent) and removal of the enzyme after the reaction (extraction with n-butanol and chloroform in the patent).
[014] Patent application CN200510026889.1 discloses a microwave extraction method for astragalus polysaccharides. The method uses a strong inorganic acid (hydrochloric acid or sulfuric acid), a strong inorganic base (potassium hydroxide, sodium hydroxide, ammonia), in which the strong inorganic acid and the strong inorganic base can cause serious corrosion of the equipment, it is difficult to recycle and easily cause environmental pollution, with the amount of inorganic acid still relatively large. The hydrolysis of polysaccharides by the acid or inorganic base is carried out mainly by adjusting the acid concentration, if there are only acids, the alkaline degradation and the cleavage effects of binding on polysaccharides, and the hydrolysis of polysaccharides under conditions of strong inorganic acid and strong base. it is difficult to control and cannot achieve the protective effects on polysaccharide molecules.
[015] Therefore, there is a need to continue to develop a new method for extracting active polysaccharides from higher plants or fungi. Summary of the invention
[016] To overcome the above technical flaws, the present invention provides a new process for extracting polysaccharides from higher plants and fungi through a chemical treatment with microwave. In the process of the present invention, a small amount of acid is used, the raw materials are heated homogeneously, the yield of polysaccharide extraction is high and the polysaccharides have high solubility in water and good activity.
[017] The process of the present invention for extracting polysaccharides from higher plants and fungi based on microwave chemistry comprises the following steps: 1) treating higher plants and sprayed fungi with an organic solvent to remove their fat-soluble components to obtain residue from higher plants and fungi; or directly use higher plants and sprayed fungi; 2) place residues or higher plants and pulverized fungi obtained in step 1) in a microwave reaction chamber, add an acid solution with a mass concentration of 5 to 99%, perform the mixer reaction for 5 to 120 min at a microwave power with a mass power density of 1 kW per kilogram of material - 10 kilowatts per kilogram of material under a working pressure of 20 mmHg to 760 mmHg; optionally, concentrate the mixer to remove the organic acid and then wash with an organic solvent to additionally remove the residual acid; 3) add aqueous solution 5 to 15 times in the product obtained from step 2), perform aqueous extraction and filtration, subject the filtered solution after concentration to precipitation with alcohol, preferably adding alcohol in the solution to an ethanol content of 70 % to 85%, to separate the precipitates, that is, the polysaccharide products.
[018] In the process of the present invention, according to one of the modalities, when the organic acid in the acid solution used in step 2) is a non-volatile acid, there is no need to remove the acid by concentration after the reaction by micro- waves be completed; when the organic acid used is a volatile acid, after the completion of the microwave reaction, concentration is performed to remove the acid and then washing with an organic solvent is performed to remove a small amount of residual acid.
[019] Since the concentration in step 2) can be performed using common methods in the art, preferably by heating with microwave under reduced pressure, and then washing with an organic solvent is performed to remove residual acid.
[020] In the process of the present invention, as one of the modalities, the method of applying the microwave power in said step 2) is a continuous microwave mode or a combination of the continuous microwave and micro modes -pulses pulsed until the acid solution undergoes reflux, the microwaves are maintained for 5 min to 120 min after the beginning of reflux; where, in the case of using the combination of continuous microwave and pulsed microwave, continuous microwave irradiation is first used until the acid solution is refluxed, and then it is switched to pulsed microwave for 5 min to 120 min;
[021] As one of the preferred modalities, in said step 2), in the case of continuous microwave, the mass power density is from 1 kW per kilogram of material to 5 kilowatts per kilogram of material; in the case of pulsed microwaves, the mass power density is 2 kW per kilogram of material - 10 kilowatts per kilogram of material, with the service ratio being A / B, where A = 1 s to 100 s, B = 1 s 100 s.
[022] In the process of the present invention, a microwave reaction chamber common in the art can be used for microwave reaction, which is a propagation microwave reaction chamber or a microwave reaction chamber. resonance waves.
[023] In the process of the present invention, as one of the embodiments, the acid solution in said step 2) is an organic acid or a mixed solution of an organic acid and an inorganic acid; wherein the organic acid solution is selected from oxalic acid, formic acid, acetic acid or propionic acid; even more preferably, a weight percentage concentration of oxalic acid is 5% to 50%, preferably 10% to 35%; a weight percentage concentration of formic acid is 10% to 99%, preferably 30 to 85%; a weight percentage concentration of acetic acid is 10% to 99%, preferably 60 to 95%; or a weight percentage concentration of propionic acid is 10% to 99%, preferably 70 to 95%.
[024] In the process of the present invention, as one of the modalities, in the mixed solution of organic and inorganic acids used in said step 2), the concentration of organic acid in the mixed solution is above the defined concentration of organic acid; and the mass percentage concentration of inorganic acid is 0.1% to 15%; even more preferably, the inorganic acid is selected from hydrochloric acid, sulfuric acid, nitric acid or phosphoric acid.
[025] The aforementioned inorganic acid solution can be purchased commercially and then used to prepare the corresponding concentration of the mixed organic-inorganic acid solution, using conventional methods in the art. For example, hydrochloric acid at a concentration of 36% is added to the organic acid to reach the corresponding concentration.
[026] In the process of the present invention, as one of the modalities, in step 2), the ratio of the residue or higher plants and pulverized fungi obtained in step 1) and the amount of acid solution is from 5/1 to 1/5; a person skilled in the art can make adjustments by adding or reducing the scale above to ensure sufficient wetting of the materials, but cannot use an excessively acidic solution which, on the contrary, would cause difficult post-processing and consume a lot of energy .
[027] In the process of the present invention, as one of the modalities, the organic solvent used in said step 2) is selected from methanol, ethanol, propanol or acetone.
[028] In the process of the present invention, said step 2) is a microwave chemical treatment of raw materials, in which the function of microwave chemical treatment mainly comprises: cleaving various bonds between polysaccharides and organic macromolecules, including proteins, cellulose, hemicellulose, lignin, chitin of cell walls of higher plants and fungi, to convert bound polysaccharides into free polysaccharides, in order to increase the extraction yield in the subsequent process; second, to cut moderately the glycosidic bonds of macromolecular polysaccharides to achieve their partial degradation, in order to increase their solubility in water; and organic acid is used since in addition to the degradation effects of H + ions on polysaccharides, organic radical ions can protect polysaccharide molecules by forming hydrogen bonds with the hydroxyl groups of the polysaccharides.
[029] The process of the present invention, the pretreatment methods of raw materials of higher plants and fungi in said step 1) include, but are not limited to, the following two methods: 1) flowers, leaves, seeds, bark, fruit, roots or tubers of said higher plants, or mycelium or sporocarp of fungal raw materials are dried, decontaminated and mechanically pulverized to be used as raw material in the next stage; or 2) the flowers, leaves, seeds, barks, fruits, roots or tubers of higher plants, or mycelium or sporocarp of fungal raw materials are dried, decontaminated, mechanically sprayed and extracted with an organic solvent to remove the fat-soluble active substances from including volatile oils, flavonoids, triterpenoids or saponins, and the extraction residue after drying is used as a raw material in the next step.
[030] In the process of the present invention, as one of the embodiments, the organic solvent used to treat pulverized higher plants or fungi in said step 1) is petroleum ether, methanol, ethanol, propanol or ethyl acetate. A person skilled in the art can determine the amount of organic solvent to be used in accordance with the present invention and common knowledge in the art, which is to allow materials to be immersed, and is generally 6 to 8 times their volume, from in order to remove fat-soluble active substances from them including, but not limited to, volatile oils, flavonoids, triterpenoids or saponins.
[031] In the process of the present invention, as one of the modalities, the alcohol used in said step 3) is ethanol.
[032] In the process of the present invention, the active polysaccharides obtained using the process of the present invention can be further refined using conventional refining methods in the art. Refining includes, but is not limited to, the following: the crude polysaccharide product obtained is added in distilled water of 10 to 20 times its weight, sufficiently agitated to dissolve and centrifuged at an RPM of 4000 to 8000r / min for 10 to 30 minutes, the precipitate is discarded and the supernatant is dialyzed in distilled water for 24h, the dialysate is lyophilized directly to obtain high purity polysaccharides, or the dialysate is concentrated to 1/5 of its original volume and then added with ethanol until there is no precipitation in the solution, centrifuged and the precipitates are dried to obtain refined polysaccharides.
[033] In the process of the invention, the higher plants used to extract active polysaccharides by the process of the present invention include, but are not limited to, raw materials, flowers, leaves, seeds, bark, fruits, roots or tubers of the astragalus, medlar -red, gingko leaf, papaya, honeysuckle, Chinese angelica, orange peel, ephedra sinica, ligusticum chuanxiong hort, acorus gramineus, garlic, galangal fruits with strong leaves, angelica, Chinese sagebrush leaves, asarum, cystanche, elaeagnus angustifolia, eucalyptus leaf, cordata, ligustrum lucidum, notopterygium, ginseng, panax pseudoginseng, sarcandra glabra, plantago, oriental fruit of polygonum, lilac daphne, bergamot, white mulberry root, mistletoe, scutellaria baicalensis, tarred goat seed tea leaf, pine, aloe, oats, konjac, yam, gastrodia elata, radix bupleuri or acanthopanax; fungi include, but are not limited to, the sporocarp or fungal mycelium of lucid ganoderma, exidia auricula judae, mushrooms, polyporus, tremela, maitake, poria, rainbow conk, hericium erinaceus or cordyceps sinensis; as preferred modalities, among the higher plants are astragalus, red medlar, yam, gingko leaves, panax pseudoginseng, plantain, elata gastronomy, eucommia ulmoides, sage or kudzu; fungi include lucid ganoderma, poria, exidia auricula judae or mushrooms.
[034] In the process of the present invention, as one of the modalities, the present invention also provides a process for preparing astragalus polysaccharides, comprising: placing astragalus, after being sprayed and degreased with ethanol in a microwave extraction chamber, add 10% to 35% oxalic acid from 1.5 to 2.5 times its weight, in a microwave power density of 1 to 2 kW / kg, under pressure from 500 mmHg to 760 mmHg, maintaining the reflux of the oxalic acid solution for 15 to 30 min and then evaporating under reduced pressure the liquid in the microwave extraction chamber until dryness. An ethanol solution of 3 to 5 times the weight of the astragalus is added to the reaction chamber. The mixer is stirred and washed for 40 to 60 minutes and filtered. The filtration residue, after drying, is extracted twice with water, where each time the amount of water is 6 to 8 times the weight of the residue, the extraction temperature is 70oC and the extraction time about 40 minutes . Filtration is performed and the two filtrate solutions are combined and concentrated to 1/5 volume of the original extraction solution; then, ethanol is added for the precipitation and the precipitates are dried to obtain the astragalus polysaccharides.
[035] The present invention also provides astragalus polysaccharides prepared using the above process, wherein the molecular weight distribution of said astragalus polysaccharides is from 3000 to 40,000.
[036] In the process of the present invention, as one of the modalities, the present invention also provides a process for preparing red medlar polysaccharides, comprising: placing red medlar, after being defatted by petroleum ether or ethanol, in a chamber extraction with microwave, add 30% to 85% formic acid solution of 1 to 2.5 times their weight, in a microwave power density of 1 to 2 kW / kg under pressure of 500 mmHg to 760 mmHg, maintaining the reflux of the formic acid solution for 15 to 25 min and then evaporating the formic acid under reduced pressure to dryness. An ethanol solution of 3 to 5 times the weight of the red medlar is added to the reaction chamber. The mixer is stirred and washed for 40 to 60 minutes and filtered. The filtration residue, after drying, is extracted twice with water, where each time the amount of water is 6 to 8 times the weight of the residue, the extraction temperature is 70oC and the extraction time about 40 minutes . Filtration is performed and the two filtrate solutions are combined and concentrated to 1/5 volume of the original extraction solution; then, ethanol is added for the precipitation and the precipitates are dried to obtain the medlar-red polysaccharides.
[037] The present invention also provides red medlar polysaccharides prepared using the above process, wherein the molecular weight distribution of said red medlar polysaccharides is from 3000 to 20000.
[038] In the process of the present invention, as one of the modalities, the present invention also provides a process for preparing yam polysaccharides, comprising: placing yam, after being sprayed, in a microwave extraction chamber, adding propionic acid 70% to 95% 1.5 to 2.5 times its weight, in a microwave power density of 1 to 2 kW / Kg under pressure of 500 mmHg to 760 mmHg, maintaining reflux of the propionic acid solution for 15 to 25 min and then evaporate the propionic acid under reduced pressure to dryness. An ethanol solution of 3 to 5 times the weight of the yam is added to the reaction chamber. The mixer is stirred and washed for 40 to 60 minutes and filtered. The filtration residue, after drying, is extracted twice with water, where each time the amount of water is 6 to 8 times the weight of the residue, the extraction temperature is 70oC and the extraction time about 40 minutes . Filtration is performed and the two filtrate solutions are combined and concentrated to 1/5 volume of the original extraction solution; then, ethanol is added for the precipitation and the precipitates are dried to obtain the yam polysaccharides.
[039] The present invention also provides yam polysaccharides prepared using the above process, wherein the molecular weight distribution of said yam polysaccharides is from 3000 to 20000.
[040] In the process of the present invention, as one of the modalities, the present invention also provides a process for preparing gingko polysaccharides, comprising: placing gingko, after being sprayed and defatted by ethanol, in a microwave extraction chamber , add 30% to 85% formic acid solution of 1.5 to 2.5 times its weight, in a microwave power density of 1 to 2 kW / Kg under pressure of 500 mmHg to 760 mmHg , maintaining the reflux of the formic acid solution for 15 to 25 min and then evaporating the formic acid under reduced pressure to dryness. An ethanol solution of 4 to 6 times the weight of the gingko is added to the reaction chamber. The mixer is stirred and washed for 40 to 60 minutes and filtered. The filtration residue, after drying, is extracted twice with water, where each time the amount of water is 6 to 8 times the weight of the residue, the extraction temperature is 70oC and the extraction time about 40 minutes . Filtration is performed and the two filtrate solutions are combined and concentrated to 1/5 volume of the original extraction solution; then, ethanol is added for the precipitation and the precipitates are dried to obtain the gingko polysaccharides.
[041] The present invention also provides gingko polysaccharides prepared using the above process, wherein the molecular weight distribution of said gingko polysaccharides is from 5000 to 12000.
[042] In the process of the present invention, as one of the modalities, the present invention also provides a process for preparing panax pseudoginseng polysaccharides, comprising: placing panax pseudoginseng, after being sprayed and defatted by ethanol, in an extraction chamber with micro microwave oven, add 60% to 95% acetic acid solution of 1.5 to 2.5 times its weight, in a microwave power density of 1 to 2 kW / Kg under pressure of 500 mmHg at 760 mmHg, maintaining the reflux of the acetic acid solution for 15 to 25 min and then evaporating the acetic acid under reduced pressure to dryness. An ethanol solution of 3 to 5 times the weight of panax pseudoginseng is added to the reaction chamber. The mixer is stirred and washed for 40 to 60 minutes and filtered. The filtration residue, after drying, is extracted twice with water, where each time the amount of water is 6 to 8 times the weight of the residue, the extraction temperature is 70oC and the extraction time about 40 minutes . Filtration is performed and the two filtrate solutions are combined and concentrated to 1/5 volume of the original extraction solution; then ethanol is added for the precipitation and the precipitates are dried to obtain the panax pseudoginseng polysaccharides.
[043] The present invention also provides panax pseudoginseng polysaccharides prepared using the above process, wherein the molecular weight distribution of said panax pseudoginseng polysaccharides is from 4000 to 20000.
[044] In the process of the present invention, as one of the modalities, the present invention also provides a process for preparing plantain polysaccharides, comprising: placing plantain, after being defatted by petroleum ether and ethanol, in a microwave extraction chamber , add 80% to 95% propionic acid solution of 1.5 to 2.5 times its weight, in a microwave power density of 1 to 2 kW / Kg under pressure of 500 mmHg to 760 mmHg , maintaining the reflux of the propionic acid solution for 15 to 25 min and then evaporating the propionic acid under reduced pressure until dryness. An ethanol solution of 3 to 5 times the weight of the plantain is added to the reaction chamber. The mixer is stirred and washed for 40 to 60 minutes and filtered. The filtration residue, after drying, is extracted twice with water, where each time the amount of water is 6 to 8 times the weight of the residue, the extraction temperature is 70oC and the extraction time about 40 minutes . Filtration is performed and the two filtrate solutions are combined and concentrated to 1/5 volume of the original extraction solution; then, ethanol is added for the precipitation and the precipitates are dried to obtain the plantain polysaccharides.
[045] The present invention also provides plantain polysaccharides prepared using the above process, wherein the molecular weight distribution of said plantain polysaccharides is from 4000 to 30000.
[046] In the process of the present invention, as one of the modalities, the present invention also provides a process for preparing polysaccharides of gastrodia elata comprising: placing gastrodia elata, after being sprayed and defatted by ethanol, in an extraction chamber with waves, add mixed solution of formic acid-hydrochloric acid (0.3% to 0.6% hydrochloric acid and 30% to 85% formic acid) of 1.5 to 2.5 times the weight of the same, in a microwave power density of 1 to 2 kW / kg under pressure of 500 mmHg to 760 mmHg, maintaining the reflux of the mixed acid solution for 15 to 25 min and then evaporating under reduced pressure the mixed acid solution until dryness. An ethanol solution of 3 to 5 times the weight of the gastrodyte is added to the reaction chamber. The mixer is stirred and washed for 40 to 60 minutes and filtered. The filtration residue, after drying, is extracted twice with water, where each time the amount of water is 6 to 8 times the weight of the residue, the extraction temperature is 70oC and the extraction time about 40 minutes . Filtration is performed and the two filtrate solutions are combined and concentrated to 1/5 volume of the original extraction solution; then, ethanol is added for the precipitation and the precipitates are dried to obtain the gastrodia elata polysaccharides.
[047] The present invention also provides gastrodia elata polysaccharides prepared using the above process, wherein the molecular weight distribution of said gastrodia elata polysaccharides is from 3000 to 20000.
[048] In the process of the present invention, as one of the modalities, the present invention also provides a process for preparing eucommia ulmoid polysaccharides, comprising: placing eucommia ulmoides, after being sprayed and defatted by ethanol, in an extraction chamber with micro microwave oven, add 30% to 85% formic acid solution of 1.5 to 2.5 times its weight, in a microwave power density of 1 to 2 kW / kg under pressure of 500 mmHg at 760 mmHg, maintaining the reflux of the formic acid solution for 15 to 25 min and then evaporating the formic acid under reduced pressure to dryness. An ethanol solution of 3 to 5 times the weight of eucommia ulmoides is added to the reaction chamber. The mixer is stirred and washed for 40 to 60 minutes and filtered. The filtration residue, after drying, is extracted twice with water, where each time the amount of water is 6 to 8 times the weight of the residue, the extraction temperature is 70oC and the extraction time about 40 minutes . Filtration is performed and the two filtrate solutions are combined and concentrated to 1/5 volume of the original extraction solution; then, ethanol is added for the precipitation and the precipitates are dried to obtain the eucommia ulmoides polysaccharides.
[049] The present invention also provides eucommia ulmoid polysaccharides prepared using the above process, wherein the molecular weight distribution of said eucommia ulmoides polysaccharides is from 3000 to 20000.
[050] In the process of the present invention, as one of the modalities, the present invention also provides a process for preparing sage polysaccharides, comprising: placing sage, after being sprayed and degreased by ethanol, in a microwave extraction chamber , add 60% to 95% acetic acid solution of 1.5 to 2.5 times its weight, in a microwave power density of 1 to 2 kW / Kg under pressure of 500 mmHg to 760 mmHg , refluxing the acetic acid solution for 15 to 25 min and then evaporating the acetic acid under reduced pressure to dryness. An ethanol solution of 3 to 5 times the weight of the sage is added to the reaction chamber. The mixer is stirred and washed for 40 to 60 minutes and filtered. The filtration residue, after drying, is extracted twice with water, where each time the amount of water is 6 to 8 times the weight of the residue, the extraction temperature is 70oC and the extraction time about 40 minutes . Filtration is performed and the two filtrate solutions are combined and concentrated to 1/5 volume of the original extraction solution; then, ethanol is added for the precipitation and the precipitates are dried to obtain the sage polysaccharides.
[051] The present invention also provides sage polysaccharides prepared using the above process, wherein the molecular weight distribution of said sage polysaccharides is from 5000 to 25000.
[052] In the process of the present invention, as one of the modalities, the present invention also provides a process for preparing kudzu polysaccharides, comprising: placing kudzu, after being sprayed and degreased by ethanol, in a microwave extraction chamber , add 70% to 95% propionic acid solution of 1.5 to 2.5 times its weight, in a microwave power density of 1 to 2 kW / Kg under pressure from 500 mmHg to 760 mmHg , maintaining the reflux of the propionic acid solution for 15 to 25 min and then evaporating the propionic acid under reduced pressure until dryness. An ethanol solution of 3 to 5 times the weight of the kudzu is added to the reaction chamber. The mixer is stirred and washed for 40 to 60 minutes and filtered. The filtration residue, after drying, is extracted twice with water, where each time the amount of water is 6 to 8 times the weight of the residue, the extraction temperature is 70oC and the extraction time about 40 minutes . Filtration is performed and the two filtrate solutions are combined and concentrated to 1/5 volume of the original extraction solution; then, ethanol is added for the precipitation and the precipitates are dried to obtain the kudzu polysaccharides.
[053] The present invention also provides kudzu polysaccharides prepared using the above process, wherein the molecular weight distribution of said kudzu polysaccharides is from 3000 to 25000.
[054] In the process of the present invention, as one of the modalities, the present invention also provides a process for preparing lucid ganoderma polysaccharides, comprising: placing lucid ganoderma sporocarp after being sprayed and degreased with ethanol in a micro extraction chamber microwave, add 10% to 35% oxalic acid solution of 1.5 to 2.5 times the weight of the same, in a microwave power density of 1 to 2 kW / kg, under pressure of 500 mmHg to 760 mmHg, maintaining the reflux of the oxalic acid solution for 15 to 25 min and then evaporating the liquid to dryness under reduced pressure. An ethanol solution of 3 to 5 times the weight of the lucid ganoderma sporocarp is added to the reaction chamber. The mixer is stirred and washed for 40 to 60 minutes and filtered. The filtration residue, after drying, is extracted twice with water, where each time the amount of water is 6 to 8 times the weight of the residue, the extraction temperature is 70oC and the extraction time about 40 minutes . Filtration is performed and the two filtrate solutions are combined and concentrated to 1/5 volume of the original extraction solution; then, ethanol is added for the precipitation and the precipitates are dried to obtain the lucid ganoderma polysaccharides.
[055] The present invention also provides lucid ganoderma polysaccharides prepared using the above process, wherein the molecular weight distribution of said lucid ganoderma polysaccharides is from 3000 to 12000.
[056] In the process of the present invention, as one of the modalities, the present invention also provides a process for preparing pore polysaccharides, comprising: placing pore, after being sprayed and defatted by ethanol, in a microwave extraction chamber , add 30% to 85% formic acid solution of 1.5 to 2.5 times its weight, in a microwave power density of 1 to 2 kW / Kg under pressure from 500 mmHg to 760 mmHg , maintaining the reflux of the formic acid solution for 15 to 25 min and then evaporating the formic acid under reduced pressure to dryness. An ethanol solution of 3 to 5 times the weight of the pore is added to the reaction chamber. The mixer is stirred and washed for 40 to 60 minutes and filtered. The filtration residue, after drying, is extracted twice with water, where each time the amount of water is 6 to 8 times the weight of the residue, the extraction temperature is 70oC and the extraction time about 40 minutes . Filtration is performed and the two filtrate solutions are combined and concentrated to 1/5 volume of the original extraction solution; then, ethanol is added for the precipitation and the precipitates are dried to obtain the pore polysaccharides.
[057] The present invention also provides pore polysaccharides prepared using the above process, wherein the molecular weight distribution of said pore polysaccharides is from 2000 to 8000.
[058] In the process of the present invention, as one of the modalities, the present invention also provides a process for preparing polysaccharides of exidia auricula judae, comprising: placing exidia auricula judae, after being sprayed, in a microwave extraction chamber , add 60% to 95% acetic acid solution of 1.5 to 2.5 times the weight of the same, in a microwave power density of 1 to 2 kW / Kg under pressure of 500 mmHg to 760 mmHg , refluxing the acetic acid solution for 15 to 25 min and then evaporating the acetic acid under reduced pressure to dryness. An ethanol solution of 3 to 5 times the weight of the actual auricula judae is added to the reaction chamber. The mixer is stirred and washed for 40 to 60 minutes and filtered. The filtration residue, after drying, is extracted twice with water, where each time the amount of water is 6 to 8 times the weight of the residue, the extraction temperature is 70oC and the extraction time about 40 minutes . Filtration is performed and the two filtrate solutions are combined and concentrated to 1/5 volume of the original extraction solution; then, ethanol is added for the precipitation and the precipitates are dried to obtain the polysaccharides of exidia auricula judae.
[059] The present invention also provides exidia auricula judae polysaccharides prepared using the above process, wherein the molecular weight distribution of said exidia auricula judae polysaccharides is from 5000 to 40,000.
[060] In the process of the present invention, as one of the modalities, the present invention also provides a process for preparing mushroom polysaccharides, comprising: placing sporocarp of mushrooms, after being sprayed, in a microwave extraction chamber, adding 70% to 95% propionic acid solution of 1.5 to 2.5 times the weight of the same, in a microwave power density of 1 to 2 kW / Kg under pressure of 500 mmHg to 760 mmHg, maintaining reflux the propionic acid solution for 15 to 25 min and then evaporate the propionic acid under reduced pressure to dryness. An ethanol solution of 3 to 5 times the weight of the mushroom is added to the reaction chamber. The mixer is stirred and washed for 40 to 60 minutes and filtered. The filtration residue, after drying, is extracted twice with water, where each time the amount of water is 6 to 8 times the weight of the residue, the extraction temperature is 70oC and the extraction time about 40 minutes . Filtration is performed and the two filtrate solutions are combined and concentrated to 1/5 volume of the original extraction solution; then, ethanol is added for the precipitation and the precipitates are dried to obtain the mushroom polysaccharides.
[061] The present invention also provides mushroom polysaccharides prepared using the above process, wherein the molecular weight distribution of said mushroom polysaccharides is from 3000 to 15000.
[062] The present invention has the following characteristics:
[063] First, the use of microwaves with an organic acid or a mixture of acids containing an organic acid works directly on medicinal raw materials, the use of organic acid cleaves the links between polysaccharides and macromolecules (including chitin, cellulose and proteins) from plant and fungal cell walls, in order to promote the release of polysaccharides from said medicinal materials and improve the extraction yield of the polysaccharides; furthermore in relation to organic acid, and in addition to the degradation effects of H + ions on polysaccharides, ions from organic acid radicals can protect polysaccharide molecules by forming hydrogen bonds with the hydroxyl groups of the polysaccharides.
[064] Second, organic acid or mixed acids containing an organic acid, enhanced by microwaves can further moderate the released polysaccharides, thereby significantly increasing the water solubility of the polysaccharides. Polysaccharides with relatively centralized molecular weight distribution and good solubility in water are obtained and the entire process achieves efficient extraction and restructuring of polysaccharides from higher plants and fungi.
[065] Thirdly, microwave heating can ensure that the internal and external parts of the materials are heated simultaneously and sufficiently overcome a series of insurmountable problems such as non-uniform heating of materials and high energy consumption in the methods of conventional heating.
[066] Compared to the prior art, the present invention also has the following advantages: 1) The present invention saves time, uses less organic acids or a mixture of acids containing an organic acid and has an easy and efficient recycling, in addition to notable water and energy saving effects. The use of microwave heating technology effectively overcomes the problem of heat transmission, which is difficult to avoid in conventional heating methods, significantly reducing the amount of organic acids used and the processing time, especially in the removal distillation process acids, and can solve the problem of non-uniform heating, which is not overcome in conventional heating methods. This feature in large-scale production has been particularly notable. 2) Organic acid or mixed acids containing an organic acid, enhanced by microwaves, can additionally moderately adjust the molecular structure of polysaccharides from higher plants and released fungi, in order to significantly improve the water solubility of the polysaccharides; while in relation to organic acid, in addition to the degradation effects of H + ions on polysaccharides, ions from radicals of organic acids can protect the polysaccharide molecules, forming hydrogen bonds with the hydroxyl groups of the polysaccharides.
[067] The process of the present invention uses an organic acid or mixed acids containing an organic acid to work directly on medicinal raw materials and overcomes many disadvantages of polysaccharide extraction in the prior art. The active polysaccharides obtained through the process of the present invention show better biological activities. Brief description of the drawings
[068] Figure 1 is a process flow chart of the present invention. Modalities
[069] The present invention will be further illustrated by the following Examples and Experimental Examples.
[070] The process of the present invention is as follows: 1) placing raw materials from higher plants and pretreated fungi into a microwave reactor chamber, adding an organic acid or an organic / acid mixture solution inorganic in this and shake sufficiently to moisten the powder well; 2) treat with microwaves and apply microwave power using the cooperative effects between microwaves, organic acid molecules and organic macromolecular substances in the cell wall of higher plants and fungi to separate polysaccharides from flowers, leaves, fruits or rhizomes of said higher plants, or mycelium or sporocarp of fungi, and selectively break the glycosidic bonds of macromolecular polysaccharides, in order to achieve their moderate degradation; 3) use distillation under reduced pressure by microwave heating to remove most organic acids or the mixed organic / inorganic acid solution and wash, sufficiently with an organic solvent to remove a small amount of residual acid in the materials to complete microwave pretreatment of raw materials from higher plants and fungi; 4) add about 5 to 15 times of water to extract the upper plants or fungi pretreated with microwaves, in which the extraction solution, after concentration, is subjected to precipitation with alcohol to obtain crude polysaccharides soluble in water of excellent quality.
[071] The entire process is shown in figure1.
[072] In the examples, the extraction yield, polysaccharide content, the polysaccharide molecular weight distribution, the amount of organic acids, the reaction time and other data are shown in Table 1. Where the yield of polysaccharide extraction is the weight percentage of products for raw materials from higher plants, the polysaccharide content is measured by the phenol-sulfuric acid method reported in an agricultural and technology magazine (Shiling Sun, Method for Determination of polysaccharide content of yam, "Agriculture and Technology", 2010, 20 (3), 35-39), the molecular weight distribution of polysaccharides is determined by gel chromatography (composition analysis of astragalus polysaccharide, Yaping Cai, Rui Zhao , Dan Zhu, "China Journal of Experimental Traditional Medical Formulae", 2011,17 (1), 81-83). Example 1 1) 1.5 kg of dry, clean and mechanically sprayed astragalus is placed in an extraction vessel, 10 L ethanol is added, the mixer is heated to reflux for extraction for 1 h and the above procedure is repeated once; 2) Filtration is performed, the two filtrates are combined and distilled under reduced pressure to recover ethanol, in order to obtain an alcohol extract rich in fat-soluble active components, including flavonoids, saponins and coumarin, etc., and the residue of filtration is dried at 60 to 80 ° C for further processing; 3) The dry filtration residue in step 2) is placed in a progressive microwave reaction chamber; 4) 300 g of oxalic acid are added with water to prepare a 10% oxalic acid solution; 5) 3 L of the oxalic acid solution from step 4) are added to the microwave reaction chamber mentioned above, and the mixer is sufficiently agitated to uniformly moisten the material; 6) The aforementioned mixer is irradiated at a continuous microwave power of 5 kW until the liquid begins to reflux, the organic acid solution is vaporized and then the microwave is switched to a pulsed microwave power operation, in which the service ratio is 5 seconds / 5 seconds (that is, the relationship between the on and off time), the peak power is 10 kW; after 15 min, aspiration is carried out (the working pressure in the reaction chamber is 20 mmHg) until no liquid is in the microwave reaction chamber; 7) 5 L of absolute ethanol are added to the microwave-treated astragalus in step 6), sufficiently agitated and filtered, where the filtrate is distilled to recover ethanol and oxalic acid and the filter residue after drying is the micro-treated astragalus -waves; 8) 100 g of microwave-treated astragalus from step 7) are placed in a 1 L beaker, 500 ml of distilled water is added to this and the mixer is placed in a hot water bath at 70 ° C for 40 min for extraction and then it is filtered. The above procedure is repeated once. The two filtrates are combined; 9) The filtrate, after being concentrated, is subjected to precipitation with alcohol, and the precipitate is dried to obtain the active polysaccharides; 10) Data including polysaccharide extraction yield, polysaccharide content, polysaccharide molecular weight distribution and amount of water used for extraction are listed in table 1. Example 2 1) 1.5 kg of red medlar dry is placed in an extraction vessel, 10 L of petroleum ether are added, the mixer is heated to reflux for extraction for 1 h and filtered; the filtration residue is added with 10 L of ethanol and heated to reflux for extraction for 1 h; 2) Filtration is carried out, the filtrate is distilled under reduced pressure to recover the ethanol, in order to obtain an alcohol extract rich in fat-soluble active components, including the color of the red medlar, and the filtration residue is dried 60 ° C to 80 ° C to be further processed; 3) The filtration residue dried in step 2) is placed in a microwave reaction chamber of progressive waves; 4) 2.4 L of pure formic acid are added with water to prepare the 70% formic acid solution; 5) 3 L of the formic acid solution from step 4) are added to the microwave reaction chamber mentioned above, and the mixer is sufficiently agitated to uniformly moisten the material; 6) The aforementioned mixer is irradiated at a continuous microwave power of 6 kW until the liquid begins to reflux, that is, the organic acid solution is vaporized and then the microwave is changed until a pulsed microwave power operation mode, in which the service ratio is 5 seconds / 5 seconds (that is, the relationship between the on and off time), the peak power is 8 kW; after 25 min, aspiration is performed (the working pressure in the reaction chamber is 20 mmHg) until no liquid is in the microwave reaction chamber; 7) 5 L of absolute ethanol are added to the microwave-treated red medlar in step 6), sufficiently stirred and filtered, where the filtrate is distilled to recover ethanol and the filter residue after drying is the treated red medlar by microwave; 8) 100 g of microwave-treated red medlar from step 7) are placed in a 1 L beaker, 500 ml of distilled water are added to it and the mixer is placed in a hot water bath at 70 ° C for 40 min for extraction and then it is filtered. The above procedure is repeated once. The two filtrates are combined; 9) The filtrate, after being concentrated, is subjected to precipitation with alcohol, and the precipitate is dried to obtain the active polysaccharides; 10) Data including polysaccharide extraction yield, polysaccharide content, polysaccharide molecular weight distribution and amount of water used for extraction are listed in table 1. Example 3 1) 1.5 kg of dry yam, clean and mechanically pulverized is placed in a progressive wave microwave reaction chamber; 2) 2.8 L of pure propionic acid are added with water to prepare the 90% propionic acid solution; 3) 3 L of the propionic acid solution from step 2) are added to the microwave reaction chamber mentioned above, and the mixer is sufficiently agitated to uniformly moisten the material; 4) The aforementioned mixer is irradiated at a continuous microwave power of 5 kW until the liquid begins to reflux, that is, the organic acid solution is vaporized and then the microwave is changed until a pulsed microwave power operation mode, in which the service ratio is 5 seconds / 5 seconds (that is, the relationship between the on and off time), the peak power is 8 kW; after 20 min, aspiration is carried out (the working pressure in the reaction chamber is 20 mmHg) until no liquid is in the microwave reaction chamber; 5) 5 L of absolute ethanol are added to the stirred and filtered yam, where the filtrate is distilled to recover ethanol and the filter residue after drying is the microwave-treated yam; 6) 100 g of the microwave-treated yam from step 7) are placed in a 1 L beaker, 800 ml of distilled water are added to this and the mixer is placed in a hot water bath at 70 ° C for 40 min for extraction and then it is filtered. The above procedure is repeated once. The two filtrates are combined; 7) The filtrate, after being concentrated, is subjected to precipitation with alcohol, and the precipitate is dried to obtain the active polysaccharides; 8) Data including polysaccharide extraction yield, polysaccharide content, polysaccharide molecular weight distribution and amount of water used for extraction are listed in table 1. Example 4 1) 1.5 kg of dry gingko, clean and mechanically pulverized is placed in an extraction vessel, 10 L of ethanol are added, the mixer is heated to reflux for extraction for 1 h and the above procedure is repeated once; 2) Filtration is carried out, the filtrate is distilled under reduced pressure to recover the ethanol, in order to obtain an alcohol extract rich in fat-soluble active components, including flavone and lactone, and the filter residue is dried at 60 ° C to 80 ° C to be further processed; 3) The dry filtration residue in step 2) is placed in a progressive microwave reaction chamber; 4) 2.8 L of pure formic acid are added with water to prepare the 30% formic acid solution; 5) 3 L of the formic acid solution from step 4) are added to the microwave reaction chamber mentioned above, and the mixer is sufficiently agitated to uniformly moisten the material; 6) The aforementioned mixer is irradiated at a continuous microwave power of, 4kW until the liquid starts to reflux, that is, the organic acid solution is vaporized and then the microwave is changed until a pulsed microwave power operation mode, in which the service ratio is 5 seconds / 5 seconds (that is, the relationship between the on and off time), the peak power is 6 kW; after 15 min, aspiration is carried out (the working pressure in the reaction chamber is 20 mmHg) until no liquid is in the microwave reaction chamber; 7) 5 L of absolute ethanol are added to the microwave treated gingko in step 6), sufficiently agitated and filtered, where the filtrate is distilled to recover ethanol and the filtration residue after drying is the microwave treated gingko ; 8) 100 g of gingko treated with microwave from step 7) are placed in a 1 liter beaker, 600 ml of distilled water is added to this and the mixer is placed in a hot water bath at 70 ° C for 40 min for extraction and then it is filtered. The above procedure is repeated once. The two filtrates are combined; 9) The filtrate, after being concentrated, is subjected to precipitation with alcohol, and the precipitate is dried to obtain the active polysaccharides; 10) Data including polysaccharide extraction yield, polysaccharide content, polysaccharide molecular weight distribution and amount of water used for extraction are listed in table 1. Example 5 1) 1.5 kg of dry pseudoginseng , cleaned and mechanically sprayed is placed in an extraction vessel, 10 L of ethanol are added, the mixer is heated to reflux for extraction for 1 h and the above procedure is repeated once; 2) Filtration is carried out, the filtrate is distilled under reduced pressure to recover the ethanol, in order to obtain an alcohol extract rich in fat-soluble active components, including triterpenoid saponin, and the filtration residue is dried at 60 ° C to 80 ° C to be further processed; 3) The dry filtration residue in step 2) is placed in a progressive microwave reaction chamber; 4) 2.8 L of pure acetic acid are added with water to prepare the 85% acetic acid solution; 5) 3 L of the acetic acid solution from step 4) are added to the microwave reaction chamber mentioned above, and the mixer is sufficiently agitated to uniformly moisten the material; 6) The aforementioned mixer is irradiated at a continuous microwave power of 6 kW until the liquid begins to reflux, that is, the organic acid solution is vaporized and then the microwave is changed until a pulsed microwave power operation mode, in which the service ratio is 5 seconds / 5 seconds (that is, the relationship between the on and off time), the peak power is 8 kW; after 15 min, aspiration is carried out (the working pressure in the reaction chamber is 20 mmHg) until no liquid is in the microwave reaction chamber; 7) 5 L of absolute ethanol are added to the panax pseudoginseng treated by microwave in step 6), sufficiently stirred and filtered, where the filtrate is distilled to recover ethanol and the filter residue after drying is the panax pseudoginseng treated by microwave ; 8) 100 g of panax pseudoginseng treated with microwaves from step 7) are placed in a 1 L beaker, 500 ml of distilled water are added to it and the mixer is placed in a hot water bath at 70 ° C for 40 min. extraction and then it is filtered. The above procedure is repeated once. The two filtrates are combined; 9) The filtrate, after being concentrated, is subjected to precipitation with alcohol, and the precipitate is dried to obtain the active polysaccharides; 10) Data including polysaccharide extraction yield, polysaccharide content, polysaccharide molecular weight distribution and amount of water used for extraction are listed in table 1. Example 6 1) 1.5 kg of dry plantain is placed in an extraction vessel, 10 L of petroleum ether are added, the mixer is heated to reflux for extraction for 1 h and filtered; the filtration residue is added with 10 L of ethanol and heated to reflux for extraction for 1 h; 2) Filtration is performed, the filtrate is distilled under reduced pressure to recover ethanol, in order to obtain an alcohol extract rich in fat-soluble active components, including fatty acids, and the filtration residue is dried at 60 ° C to 80 ° C ° C to be further processed; 3) The dry filtration residue in step 2) is placed in a progressive microwave reaction chamber; 4) 3 L of pure propionic acid are added with water to prepare the 90% propionic acid solution; 5) 3 L of the propionic acid solution from step 4) are added to the microwave reaction chamber mentioned above, and the mixer is sufficiently agitated to uniformly moisten the material; 6) The aforementioned mixer is subjected to irradiation in the continuous microwave power of 5 kW until the liquid begins to reflux, that is, the organic acid solution is vaporized and then the microwave is changed until a pulsed microwave power operation mode, in which the service ratio is 5 seconds / 5 seconds (that is, the relationship between the on and off time), the peak power is 10 kW; after 20 min, aspiration is carried out (the working pressure in the reaction chamber is 20 mmHg) until no liquid is in the microwave reaction chamber; 7) 5 L of absolute ethanol are added to the plank treated by microwave in step 6), sufficiently agitated and filtered, where the filtrate is distilled to recover ethanol and the filter residue after drying is the plank treated by microwave ; 8) 100 g of plantain treated with microwave from step 7) are placed in a 1 L beaker, 500 ml of distilled water is added to this and the mixer is placed in a hot water bath at 70 ° C for 40 min for extraction and then it is filtered. The above procedure is repeated once. The two filtrates are combined; 9) The filtrate, after being concentrated, is subjected to precipitation with alcohol, and the precipitate is dried to obtain the active polysaccharides; 10) Data including polysaccharide extraction yield, polysaccharide content, polysaccharide molecular weight distribution and amount of water used for extraction are listed in table 1. Example 7 1) 1.5 Kg of dry elast gastronomy , clean and mechanically pulverized is placed in an extraction vessel, 10 L of ethanol are added, the mixer is heated to reflux for extraction for 1 h and the above procedure is repeated once; 2) Filtration is carried out, the filtrate is distilled under reduced pressure to recover the ethanol, in order to obtain an alcohol extract rich in fat-soluble active components, including phenolic acids, and the filtration residue is dried at 60 ° C to 80 ° C to be further processed; 3) The dry filtration residue in step 2) is placed in a progressive microwave reaction chamber; 4) 2.8 L of pure formic acid are added with 100 ml of concentrated hydrochloric acid 36% and water to prepare a mixture solution of formic acid — hydrochloric acid solution (0.5% hydrochloric acid and 75% formic acid ); 5) 3 L of the solution of the formic acid-hydrochloric acid mixture from step 4) are added to the microwave reaction chamber mentioned above, and the mixer is sufficiently agitated to uniformly moisten the material; 6) The aforementioned mixer is irradiated at a continuous microwave power of 6 kW until the liquid begins to reflux, that is, the organic acid solution is vaporized and then the microwave is changed until a pulsed microwave power operation mode, in which the service ratio is 5 seconds / 5 seconds (that is, the relationship between the on and off time), the peak power is 8 kW; after 15 min, aspiration is carried out (the working pressure in the reaction chamber is 20 mmHg) until no liquid is in the microwave reaction chamber; 7) 5 L of absolute ethanol are added to the microwave oven treated in microwave in step 6), sufficiently stirred and filtered, where the filtrate is distilled to recover ethanol and the filtration residue after drying is microwave oven treated by microwave. ; 8) 100 g of elated gastrodia treated with microwave from step 7) are placed in a 1 L beaker, 800 ml of distilled water are added to this and the mixer is placed in a hot water bath at 70 ° C for 40 min for extraction and then it is filtered. The above procedure is repeated once. The two filtrates are combined; 9) The filtrate, after being concentrated, is subjected to precipitation with alcohol, and the precipitate is dried to obtain the active polysaccharides; 10) Data including polysaccharide extraction yield, polysaccharide content, polysaccharide molecular weight distribution and amount of water used for extraction are listed in table 1. Example 8 1) 1.5 Kg of dry eucommia ulmoides , clean and mechanically pulverized is placed in an extraction vessel, 10 L of ethanol are added, the mixer is heated to reflux for extraction for 1 h and the above procedure is repeated once; 2) Filtration is carried out, the filtrate is distilled under reduced pressure to recover ethanol, in order to obtain an alcohol extract rich in fat-soluble active components, including lignans, and the filtration residue is dried from 60 ° C to 80 ° C to be further processed; 3) The dry filtration residue in step 2) is placed in a progressive microwave reaction chamber; 4) 2.8 L of pure formic acid are added with water to prepare the 80% formic acid solution; 5) 3 L of the formic acid solution from step 4) are added to the microwave reaction chamber mentioned above, and the mixer is sufficiently agitated to uniformly moisten the material; 6) The aforementioned mixer is irradiated at a continuous microwave power of 6 kW until the liquid begins to reflux, that is, the organic acid solution is vaporized and then the microwave is changed until a pulsed microwave power operation mode, in which the service ratio is 5 seconds / 5 seconds (that is, the relationship between the on and off time), the peak power is 8 kW; after 15 min, aspiration is carried out (the working pressure in the reaction chamber is 20 mmHg) until no liquid is in the microwave reaction chamber; 7) 5 L of absolute ethanol are added to the microwave-treated eucommia ulmoides in step 6), sufficiently stirred and filtered, where the filtrate is distilled to recover ethanol and the filtration residue after drying is micro-treated eucommia ulmoides waves; 8) 100 g of microwave-treated eucommia ulmoides from step 7) are placed in a 1 L beaker, 800 ml of distilled water are added to this and the mixer is placed in a hot water bath at 70 ° C for 40 min for extraction and then it is filtered. The above procedure is repeated once. The two filtrates are combined; 9) The filtrate, after being concentrated, is subjected to precipitation with alcohol, and the precipitate is dried to obtain the active polysaccharides; 10) Data including polysaccharide extraction yield, polysaccharide content, polysaccharide molecular weight distribution and amount of water used for extraction are listed in table 1. Example 9 1) 1.5 kg of dry sage, clean and mechanically pulverized is placed in an extraction vessel, 10 L of ethanol are added, the mixer is heated to reflux for extraction for 1 h and the above procedure is repeated once; 2) Filtration is carried out, the filtrate is distilled under reduced pressure to recover ethanol, in order to obtain an alcohol extract rich in fat-soluble active components, including salvianolic acid, and the filtration residue is dried at 60 ° C to 80 ° C ° C to be further processed; 3) The dry filtration residue in step 2) is placed in a progressive microwave reaction chamber; 4) 2.8 L of pure acetic acid are added with water to prepare the 85% acetic acid solution; 5) 3 L of the acetic acid solution from step 4) are added to the microwave reaction chamber mentioned above, and the mixer is sufficiently agitated to uniformly moisten the material; 6) The aforementioned mixer is irradiated at a continuous microwave power of 5 kW until the liquid begins to reflux, the organic acid solution is vaporized and then the microwave is switched to a pulsed microwave power operation, in which the service ratio is 5 seconds / 5 seconds (that is, the relationship between the on and off time), the peak power is 10 kW; after 20 min, aspiration is carried out (the working pressure in the reaction chamber is 20 mmHg) until no liquid is in the microwave reaction chamber; 7) 5 L of absolute ethanol are added to the microwave-treated salvia in step 6), sufficiently stirred and filtered, where the filtrate is distilled to recover ethanol and the filtration residue after drying is the microwave-treated salvia ; 8) 100 g of sage treated with microwaves from step 7) are placed in a 1 liter beaker, 600 ml of distilled water is added to this and the mixer is placed in a hot water bath at 70 ° C for 40 min for extraction and then it is filtered. The above procedure is repeated once. The two filtrates are combined; 9) The filtrate, after being concentrated, is subjected to precipitation with alcohol, and the precipitate is dried to obtain the active polysaccharides; 10) The data including polysaccharide extraction yield, polysaccharide content, polysaccharide molecular weight distribution and amount of water used for extraction are listed in table 1. Example 10 1) 1.5 Kg of dry kudzu, clean and mechanically pulverized is placed in an extraction vessel, 10 L ethanol is added, the mixer is heated to reflux for extraction for 1 h and the above procedure is repeated once; 2) Filtration is carried out, the filtrate is distilled under reduced pressure to recover ethanol, in order to obtain an alcohol extract rich in fat-soluble active components, including flavonoids and saponins, and the filtration residue is dried at 60 ° C to 80 ° C to be further processed; 3) The dry filtration residue in step 2) is placed in a progressive microwave reaction chamber; 4) 3.0 L of pure propionic acid are added with water to prepare the 90% propionic acid solution; 5) 3 L of the propionic acid solution from step 4) are added to the microwave reaction chamber mentioned above, and the mixer is sufficiently agitated to uniformly moisten the material; 6) The aforementioned mixer is subjected to irradiation in the continuous microwave power of 5 kW until the liquid begins to reflux, that is, the organic acid solution is vaporized and then the microwave is changed until a pulsed microwave power operation mode, in which the service ratio is 5 seconds / 5 seconds (ie, the relationship between the on and off time), the peak power is 8 kW; after 25 min, the aspiration is carried out (the working pressure in the reaction chamber is 20 mmHg) until no liquid is in the microwave reaction chamber; 7) 5 L of absolute ethanol are added to the microwave-treated kudzu in step 6), sufficiently stirred and filtered, where the filtrate is distilled to recover ethanol and the filter residue after drying is the microwave-treated kudzu ; 8) 100 g of microwave-treated kudzu from step 7) are placed in a 1 L beaker, 800 ml of distilled water are added to this and the mixer is placed in a hot water bath at 70 ° C for 40 min for extraction and then it is filtered. The above procedure is repeated once. The two filtrates are combined; 9) The filtrate, after being concentrated, is subjected to precipitation with alcohol, and the precipitate is dried to obtain the active polysaccharides; 10) Data including polysaccharide extraction yield, polysaccharide content, polysaccharide molecular weight distribution and amount of water used for extraction are listed in table 1. Example 11 1) 1.5 kg of ganoderma sporocarp dry, clean and mechanically pulverized lucid is placed in an extraction vessel, 10 L of ethanol are added, the mixer is heated to reflux for extraction for 1 h and the above procedure is repeated once; 2) Filtration is performed, the filtrate is distilled under reduced pressure to recover ethanol, in order to obtain an alcohol extract rich in fat-soluble active components, including triterpene, and the filtration residue is dried from 60 ° C to 80 ° C to be further processed; 3) The dry filtration residue in step 2) is placed in a progressive microwave reaction chamber; 4) 300 g of oxalic acid are added with water to prepare a 10% oxalic acid solution; 5) 3 L of the oxalic acid solution from step 4) are added to the microwave reaction chamber mentioned above, and the mixer is sufficiently agitated to uniformly moisten the material; 6) The aforementioned mixer is irradiated at a continuous microwave power of 6 kW until the liquid begins to reflux, that is, the organic acid solution is vaporized and then the microwave is changed until a pulsed microwave power operation mode, in which the service ratio is 5 seconds / 5 seconds (that is, the relationship between the on and off time), the peak power is 8 kW; after 15 min, aspiration is carried out (the working pressure in the reaction chamber is 20 mmHg) until no liquid is in the microwave reaction chamber; 7) 5 L of absolute ethanol are added to the sporocarp of lucid ganoderma treated by microwave in step 6), sufficiently stirred and filtered, where the filtrate is distilled to recover ethanol and the filtration residue after drying is sporocarp of lucid ganoderma microwave-treated; 8) 100 g of sporocarp of lucid ganoderma treated with microwave from step 7) are placed in a 1 L beaker, 800 ml of distilled water are added to this and the mixer is placed in a hot water bath at 70 ° C for 40 min for extraction and then it is filtered. The above procedure is repeated once. The two filtrates are combined; 9) The filtrate, after being concentrated, is subjected to precipitation with alcohol, and the precipitate is dried to obtain the crude active polysaccharides; 10) 5 g of crude active polysaccharides obtained in step 9) are placed in a 100 mL beaker; 11) 50 ml of distilled water are added to the beaker in step 10) and stirred for 30 minutes; 12) The solution obtained in step 11) is centrifuged at 5000r / min RPM, the precipitate is discarded and the supernatant is maintained; 13) The supernatant obtained in step 12) is added to a dialysis bag (cut at 3000 pm and dialyzed in distilled water for 24 h; 14) The solution in the dialysis bag from step 13) is removed and is lyophilized in a lyophilizer to obtain refined polysaccharides; 15) Data including polysaccharide extraction yield, polysaccharide content, polysaccharide molecular weight distribution and amount of water used for extraction are listed in table 1. Example 12 1) 1.5 kg dry pore, clean and mechanically pulverized is placed in an extraction vessel, 10 L of ethanol are added, the mixer is heated to reflux for extraction for 1 h and the above procedure is repeated once; 2) Filtration is performed, the filtrate is distilled under reduced pressure to recover ethanol, in order to obtain an alcohol extract rich in fat-soluble active components, including triterpene, and the filtration residue is dried from 60 ° C to 80 ° C to be further processed; 3) The dry filtration residue in step 2) is placed in a progressive microwave reaction chamber; 4) 2.8 L of pure formic acid are added with water to prepare the 80% formic acid solution; 5) 3 L of the formic acid solution from step 4) are added to the microwave reaction chamber mentioned above, and the mixer is sufficiently agitated to uniformly moisten the material; 6) The aforementioned mixer is irradiated at a continuous microwave power of 6 kW until the liquid begins to reflux, that is, the organic acid solution is vaporized and then the microwave is changed until a pulsed microwave power operation mode, in which the service ratio is 5 seconds / 5 seconds (that is, the relationship between the on and off time), the peak power is 10 kW; after 20 min, aspiration is carried out (the working pressure in the reaction chamber is 20 mmHg) until no liquid is in the microwave reaction chamber; 7) 5 L of absolute ethanol are added to the microwave-treated pore in step 6), sufficiently agitated and filtered, where the filtrate is distilled to recover ethanol and the filtration residue after drying is the microwave-treated pore ; 8) 100 g of the microwave-treated pore from step 7) are placed in a 1 L beaker, 800 ml of distilled water are added to this and the mixer is placed in a hot water bath at 70 ° C for 40 min for extraction and then it is filtered. The above procedure is repeated once. The two filtrates are combined; 9) The filtrate, after being concentrated, is subjected to precipitation with alcohol, and the precipitate is dried to obtain the active polysaccharides; 10) Data including polysaccharide extraction yield, polysaccharide content, polysaccharide molecular weight distribution and amount of water used for extraction are listed in table 1. Example 13 1) exidia auricula judae dry, clean and mechanically sprayed is placed in an extraction container; 2) 2.8 L of acetic acid are added with water to prepare the 85% acetic acid solution; 3) 3 L of the acetic acid solution from step 2) are added to the microwave reaction chamber mentioned above, and the mixer is sufficiently agitated to uniformly moisten the material; 4) The aforementioned mixer is irradiated at a continuous microwave power of, 4kW until the liquid begins to reflux, that is, the organic acid solution is vaporized and then the microwave is changed until a pulsed microwave power operation mode, where the service ratio is 5 seconds / 5 seconds (that is, the relationship between the on and off time), the peak power is 6 kW; after 15 min, the aspiration is carried out (the working pressure in the reaction chamber is 20 mmHg) until no liquid is in the microwave reaction chamber; 5) 5 L of absolute ethanol are added to the exidia auricula judae treated by microwave in step 4), sufficiently agitated and filtered, where the filtrate is distilled to recover ethanol and the filter residue after drying is exidia auricula judae treated microwave; 6) 100 g of exidia auricula judae treated with microwaves from step 5) are placed in a 1 L beaker, 500 ml of distilled water is added to this and the mixer is placed in a hot water bath at 70 ° C for 40 min for extraction and then it is filtered. The above procedure is repeated once. The two filtrates are combined; 7) The filtrate, after being concentrated, is subjected to precipitation with alcohol, and the precipitate is dried to obtain the active polysaccharides; 8) Data including polysaccharide extraction yield, polysaccharide content, polysaccharide molecular weight distribution and amount of water used for extraction are listed in table 1. Example 14 1) clean, mechanically dried mushroom sporocarp sprayed is placed in an extraction container; 2) 3 L of propionic acid are added with water to prepare the 90% propionic acid solution; 3) 3 L of the propionic acid solution from step 2) are added to the microwave reaction chamber mentioned above, and the mixer is sufficiently agitated to uniformly moisten the material; 4) The aforementioned mixer is irradiated at a continuous microwave power of 6 kW until the liquid begins to reflux, that is, the organic acid solution is vaporized and then the microwave is changed until a pulsed microwave power operation mode, in which the service ratio is 5 seconds / 5 seconds (that is, the relationship between the on and off time), the peak power is 8 kW; after 20 min, aspiration is carried out (the working pressure in the reaction chamber is 20 mmHg) until no liquid is in the microwave reaction chamber; 5) 5 L of absolute ethanol are added to the microwave-treated mushroom sporocarp in step 4), sufficiently stirred and filtered, where the filtrate is distilled to recover ethanol and the filtration residue after drying is mushroom sporocarp treated by microwave; 6) 100 g of sporocarp treated with microwave from step 5) are placed in a 1 liter beaker, 600 ml of distilled water is added to this and the mixer is placed in a hot water bath at 70 ° C for 40 min for extraction and then it is filtered. The above procedure is repeated once. The two filtrates are combined; 7) The filtrate, after being concentrated, is subjected to precipitation with alcohol, and the precipitate is dried to obtain the active polysaccharides; 8) Data including polysaccharide extraction yield, polysaccharide content, polysaccharide molecular weight distribution and amount of water used for extraction are listed in table 1.
[073] Table 1. Extraction yield of the polysaccharide product, polysaccharide content and amount of water used for the polysaccharide extraction in Examples 1 to 14.


[074] Experiment 1 Anti-tumor pharmaceutical efficacy of the active ingredient of lucid ganoderma polysaccharides
[075] Experimental materials: lucid ganoderma polysaccharides, 78% crude polysaccharides and 94% purified polysaccharides, prepared in example11.
[076] Experimental animals: male Kunming mice, weighing (22 ± 2) g, supplied by Experimental Animal Center of Military Medical Sciences, Beijing
[077] Tumor lines: Lewis lung tumor lines and S180 sarcoma tumor lines, purchased from the Shanghai Institutes for Biological Sciences.
[078] Main Instruments: DSX-280A autoclave, produced by Shanghai Shen An Med Instrument; LD5-2A low speed centrifuge, produced by Beijing Medical Centrifuge Company; 14ZQ-F160 thermostatic oscillator, produced by Harbin Donglian Electronic Technology Development Co., Ltd.
[079] Experimental method: well-developed tumor mice were sacrificed 7 days after being inoculated with Lewis lung tumor and S180 sarcoma tumor. Well-developed tumor tissues are selected to prepare the cell suspension, which is inoculated in the axilla of the test mice, the amount of inoculation is 0.2 mL / mouse, in order to prepare the models of focal solid tumor. The inoculated mice are randomly divided into control groups, in the positive control group, in the polysaccharide dose group, to 10 mice / group. The mice are administered drugs 24 hours after being inoculated with the tumor cell, the drugs are injected intraperitoneally in a chronic manner for 9 days, the mice are weighed 24 hours after the last administration and sacrificed by cervical dislocation, and the tumor is removed and weighed .
[080] The tumor inhibition rate is calculated as: tumor inhibition rate (%) = (average tumor weight of the model group - average tumor weight of the drug-administered group) / average tumor weight of the model group x 100 .
[081] The results are in the table below:

[082] It has been found that lucid ganoderma polysaccharides can effectively inhibit tumor growth.
[083] The results of the experiment showed that the present invention uses the chemical microwave method to treat flowers, leaves, fruits, seeds, barks, roots or tubers of common higher plants and mycelium or sporocarp of common fungi, then applies aqueous extraction and alcohol precipitation methods to obtain water-soluble polysaccharides and overcomes deficiencies in the prior art, such as consumption of large amounts of water, high energy consumption, low product yield, etc. Higher plants and fungi contain active polysaccharides, as well as many other active components, including triterpenes, flavonoids, saponins, etc. which can be extracted with alcohol or extracted with water, respectively before or after microwave treatment according to their differences in polysaccharide solubility, in order to achieve the comprehensive use of active ingredients in higher plants and fungi.

权利要求:
Claims (15)
[0001]
1.PROCESSING EXTRACTION OF POLYSACARIDES FROM UPPER PLANTS OR FUNGI based on a chemical treatment with microwave, characterized by the fact that it comprises the following steps: 1) treating top plants or sprayed fungi with an organic solvent to remove their fat-soluble components to obtain residue from higher plants or fungi; or directly use higher plants or sprayed fungi; 2) place residue or the top plants or pulverized fungi obtained in step 1) in a microwave reaction chamber, add an acid solution of a mass concentration of 5% to 99%, perform the mixer reaction for 5 to 120 min at a microwave power mass power density of 1 kW per kilogram of material - 10 kilowatts per kilogram of material under a working pressure of 20 mmHg to 760 mmHg; optionally, perform the concentration and then wash with an organic solvent to remove excess acid; 3) perform the extraction by adding an aqueous solution 5 to 15 times in volume in the product obtained from step 2), subject the extraction solution after concentration to precipitation with alcohol, separate the precipitates, that is, the polysaccharides .
[0002]
2. PROCESS, according to claim 1, characterized by the fact that the method of applying microwave power in step 2) is a continuous microwave mode or a combination of continuous microwave mode and pulsed microwave; where, in the case of using the combination of continuous microwave and pulsed microwave, continuous microwave irradiation is first used until the acid solution is refluxed and then it is switched to pulsed microwave for 5 min to 120 min.
[0003]
3. PROCESS, according to claim 1, characterized by the fact that, in said step 2), when the acid solution used is of a non-volatile acid, the removal of the acid by concentration is not carried out; when a volatile acid is used, the concentration is first carried out to remove the acid, preferably by distillation under reduced pressure under microwave heating.
[0004]
4. PROCESS, according to claim 2, characterized by the fact that, in said step 2), in the case of continuous microwave, the mass power density is 1 kW per kilogram of material at 5 kilowatts per kilogram of material; in the case of pulsed microwaves, the mass power density is from 2 kilowatts per kilogram of material to 10 kilowatts per kilogram of material, the service ratio is A / B, where A = 1 s to 100 s, B = 1 to 100 s.
[0005]
5. PROCESS, according to claim 2, characterized by the fact that the acid solution in said step 2) is an organic acid or a mixed solution of an organic acid and an inorganic acid.
[0006]
6. PROCESS, according to claim 5, characterized by the fact that the organic acid solution in said step 2) is selected from oxalic acid, formic acid, acetic acid or propionic acid.
[0007]
7. PROCESS, according to claim 6, characterized by the fact that, in said step 2), a percentage concentration by weight of oxalic acid is from 5% to 50%, preferably from 10% to 35%; a weight percent formic acid concentration is 10% to 99%, preferably 30 to 85%; a weight percent concentration of acetic acid is 10% to 99%, preferably 60 to 95%; or a weight percent concentration of propionic acid is 10% to 99%, preferably 70 to 95%.
[0008]
8. PROCESS, according to claim 5, characterized by the fact that, in the mixed solution of an organic acid and an inorganic acid used in said step 2), the mass percentage concentration of the inorganic acid in the mixed solution is 0, 1% to 15%.
[0009]
9. PROCESS, according to claim 8, characterized by the fact that the inorganic acid in step 2) is selected from hydrochloric acid, sulfuric acid, nitric acid or phosphoric acid.
[0010]
10. PROCESS, according to claim 1, characterized by the fact that, in step 2), the ratio of the residue or higher plants or pulverized fungi obtained in step 1) in relation to the amount of acid solution is 5/1 to 1/5.
[0011]
11. PROCESS, according to claim 1, characterized by the fact that the organic solvent used in said step 2) is selected from methanol, ethanol, propanol or acetone.
[0012]
12. PROCESS, according to claim 1, characterized by the fact that the organic solvent used in said step 1) is petroleum ether, methanol, ethanol, propanol or ethyl acetate; and / or that the fat-soluble component in step 1) is volatile oils, flavonoids, triterpenoids or saponins; and / or that the alcohol used in said step 3) is ethanol.
[0013]
13. PROCESS, according to claim 1, characterized by the fact that the upper plants are selected from flowers, leaves, seeds, barks, fruits, roots or tubers of astragalus, medlar-red, gingko leaf, papaya, honeysuckle, chinese angelica, orange peel, ephedra sinica, ligusticum chuanxiong hort, acorus gramineus, garlic, galangal fruits with strong leaves, angelica, Chinese sagebrush leaves, asarum, cystanche, elaeagnus angustifolia, eucalyptus leaf, cordata, ligustrum lucidum, notopterygium, ginseng, panax pseudoginseng, sarcandra glabra, plantain, oriental polygonum fruit, lilac daphne, bergamot, white mulberry root, mistletoe, scutellaria baicalensis, tared goat seed, tea leaf, pine herb, aloe, oats, konjac, yam, gastrodia elata, radix bupleuri or acanthopanax; fungi are selected from sporocarp or fungal mycelium of lucid ganoderma, exidia auricula judae, mushrooms, polyporus, tremela, maitake, poria, rainbow conk, hericium erinaceus or cordyceps sinensis; in which the upper plants are preferably astragalus, red medlar, yam, gingko leaves, panax pseudoginseng, plantain, gastrodia elata, eucommia ulmoides, sage or kudzu; and fungi are preferably lucid ganoderma, poria, exidia auricula judae or mushrooms.
[0014]
14. PROCESS, according to any one of claims 1 to 13, characterized by the fact that the process is a process for preparing astragalus polysaccharides which comprises: placing astragalus after being sprayed and degreased with ethanol in a micro-extraction chamber waves, add 10% to 35% oxalic acid solution of 1.5 to 2.5 times the weight of the same, in a microwave power density of 1 to 2 kW / kg, under pressure of 500 mmHg at 760 mmHg, maintaining the reflux of the oxalic acid solution for 15 to 30 min and then evaporating the liquid in the microwave extraction chamber under reduced pressure until dry; add an ethanol solution of 3 to 5 times the weight of astragalus in the reaction chamber, shake and wash for 40 to 60 minutes and perform the filtration; extract the filtration residue after being dried twice with water, in which each time, the amount of water is 6 to 8 times the weight of the residue, the extraction temperature is 70 ° C, and the extraction time is about 40 minutes; perform filtration, combining the two filtrate solutions and concentrating the filtrate solution to 1/5 of the volume of the original extraction solution; then, add ethanol for precipitation and dry the precipitates to obtain astragalus polysaccharides; the process is a process of preparing red medlar polysaccharides which comprises: placing red medlar after being defatted with petroleum ether and ethanol in a microwave extraction chamber, adding 30% to 85% formic acid solution from 1 to 2.5 times its weight, in a microwave power density of 1 to 2 kW / Kg under pressure of 500 mmHg to 760 mmHg maintaining the reflux of the formic acid solution for 15 to 25 min and, then, evaporate under reduced pressure the formic acid to dryness; add an ethanol solution of 3 to 5 times the weight of the red medlar to the reaction chamber, shake and wash for 40 to 60 minutes and perform the filtration; extract the filtration residue after being dried twice with water, each time the amount of water is 6 to 8 times the weight of the residue, the extraction temperature is 70 ° C and the extraction time is about 40 minutes; perform filtration, combine the two filtrate solutions and concentrate the filtrate solution to 1/5 the volume of the original extraction solution; then, add ethanol for precipitation and dry the precipitates to obtain red medlar polysaccharides; the process is a process for preparing yam polysaccharides which comprises: placing yam, after being sprayed in a microwave extraction chamber, adding 70% to 95% propionic acid solution 1.5 to 2.5 times its weight, at a microwave power density of 1 to 2 kW / kg under pressure of 500 mmHg to 760 mmHg, maintaining the reflux of the propionic acid solution for 15 to 25 min and then evaporating under reduced pressure propionic acid to dryness; add an ethanol solution of 3 to 5 times the weight of yam in the reaction chamber, shake and wash for 40 to 60 minutes and perform the filtration; extract the filtration residue after being dried twice with water, in which each time, the amount of water is 6 to 8 times the weight of the residue, the extraction temperature is 70 ° C and the extraction time is about 40 minutes; perform filtration, combine the two filtrate solutions and concentrate the filtrate solution to 1/5 the volume of the original extraction solution; then, add ethanol for precipitation and dry the precipitates to obtain yam polysaccharides; the process is a process for preparing gingko polysaccharides which comprises: placing gingko after being sprayed and degreased by ethanol in a microwave extraction chamber, adding 30% to 85% formic acid solution from 1.5 to 2 , 5 times its weight, in a microwave power density of 1 to 2 kW / Kg under pressure of 500 mmHg to 760 mmHg, maintaining the reflux of the formic acid solution for 15 to 25 min and then , evaporate under reduced pressure the formic acid to dryness; add an ethanol solution of 4 to 6 times the weight of ginko in the reaction chamber, shake and wash for 40 to 60 minutes and perform the filtration; extract the filtration residue after being dried twice with water, in which each time, the amount of water is 6 to 8 times the weight of the residue, the extraction temperature is 70 ° C and the extraction time is about 40 minutes; perform filtration, combine the two filtrate solutions and concentrate the filtrate solution to 1/5 the volume of the original extraction solution; then, add ethanol for precipitation and dry the precipitates to obtain gingko polysaccharides; the process is a process of preparing panax pseudoginseng polysaccharides which comprises: placing panax pseudoginseng after being sprayed and degreased by ethanol in a microwave extraction chamber, adding 60% to 95% acetic acid solution of 1.5 at 2.5 times its weight, at a microwave power density of 1 to 2 kW / kg under pressure of 500 mmHg to 760 mmHg, maintaining the reflux of the acetic acid solution for 15 to 25 min and, then, evaporate the acetic acid under reduced pressure to dryness; add an ethanol solution of 3 to 5 times the weight of panax pseudoginseng in the reaction chamber, shake and wash for 40 to 60 minutes and perform the filtration; extract the filtration residue after being dried twice with water, where each time, the amount of water is 6 to 8 times the weight of the residue, the extraction temperature is 70 ° C and the extraction time is about 40 minutes; perform filtration, combine the two filtrate solutions and concentrate the filtrate solution to 1/5 the volume of the original extraction solution; then, add ethanol for precipitation and dry the precipitates to obtain panax pseudoginseng polysaccharides; the process is a process for preparing plantain polysaccharides which comprises: placing plantain after being defatted by petroleum ether, ethanol in a microwave extraction chamber, adding 80% to 95% propionic acid solution from 1.5 to 2 , 5 times its weight, in a microwave power density of 1 to 2 kW / Kg under pressure of 500 mmHg to 760 mmHg, maintaining the reflux of the propionic acid solution for 15 to 25 min and then , evaporate propionic acid under reduced pressure to dryness; add an ethanol solution of 3 to 5 times the plantain weight in the reaction chamber, shake and wash for 40 to 60 minutes and perform the filtration; extract the filtration residue after being dried twice with water, in which each time, the amount of water is 6 to 8 times the weight of the residue, the extraction temperature is 70 ° C and the extraction time is about 40 minutes; perform filtration, combine the two filtrate solutions and concentrate the filtrate solution to 1/5 the volume of the original extraction solution; then, add ethanol for precipitation and dry the precipitates to obtain plantain polysaccharides; the process is a process for preparing polysaccharides of gastrodia elata which comprises: placing gastrodia elata after being sprayed and defatted by ethanol in a microwave extraction chamber, adding a mixed solution of 0.3% formic acid-hydrochloric acid 0.6% hydrochloric acid and 30% to 85% formic acid, 1.5 to 2.5 times the weight of the same, in a microwave power density of 1 to 2 kW / kg under pressure from 500 mmHg to 760 mmHg, maintaining the reflux of the mixed acid solution for 15 to 25 min and then evaporating the mixed acid solution to dryness under reduced pressure; add an ethanol solution of 3 to 5 times the weight of the gastrodia elata in the reaction chamber, shake and wash for 40 to 60 minutes and perform the filtration; extract the filtration residue after being dried twice with water, where each time the amount of water is 6 to 8 times the weight of the residue, the extraction temperature is 70 ° C and the extraction time is about 40 minutes; perform filtration, combine two filtrate solutions and concentrate the filtrate solution to 1/5 the volume of the original extraction solution; then, add ethanol for precipitation and dry the precipitates to obtain polysaccharides of gastrodia elata; the process is a process for preparing eucommia ulmoides polysaccharides which comprises: placing eucommia ulmoides, after being sprayed and degreased by ethanol in a microwave extraction chamber, adding 30% to 85% formic acid solution 1, 5 to 2.5 times its weight, in a microwave power density of 1 to 2 kW / Kg under pressure of 500 mmHg to 760 mmHg, maintaining the reflux of the formic acid solution for 15 to 25 min and then, evaporate the formic acid under reduced pressure to dryness; add an ethanol solution of 3 to 5 times the weight of eucommia ulmoides in the reaction chamber, shake and wash for 40 to 60 minutes to perform filtration; extract filtration residue after being dried twice with water, in which each time, the amount of water is 6 to 8 times the weight of the residue, the extraction temperature is 70 ° C and the extraction time is about 40 minutes; perform filtration and combine the two filtrate solutions and concentrate the filtrate solution to 1/5 of the volume of the original extraction solution; then, add ethanol for precipitation and dry the precipitates to obtain polysaccharides from eucommia ulmoides; the process is a process of preparing sage polysaccharides which comprises: placing sage after being sprayed and defatted by ethanol in a microwave extraction chamber, adding 60% to 95% acetic acid solution from 1.5 to 2 , 5 times its weight, in a microwave power density of 1 to 2 kW / Kg under pressure of 500 mmHg to 760 mmHg, maintaining the reflux of the acetic acid solution for 15 to 25 min and then , evaporate the acetic acid under reduced pressure to dryness; add an ethanol solution of 3 to 5 times the weight of sage in the reaction chamber, shake and wash for 40 to 60 minutes and perform the filtration; extract the filtration residue after being dried twice with water, in which each time, the amount of water is 6 to 8 times the weight of the residue, the extraction temperature is 70 ° C and the extraction time is about 40 minutes; perform filtration, combine the two filtrate solutions and concentrate the filtrate solution to 1/5 the volume of the original extraction solution; then, add ethanol for precipitation and dry the precipitates to obtain sage polysaccharides; the process is a process of preparing kudzu polysaccharides which comprises: placing kudzu, after being sprayed and degreased by ethanol in a microwave extraction chamber, adding 70% to 95% propionic acid solution from 1.5 to 2.5 times its weight, in a microwave power density of 1 to 2 kW / Kg under pressure of 500 mmHg to 760 mmHg, maintaining the reflux of the propionic acid solution for 15 to 25 min and, in then, evaporate the propionic acid under reduced pressure until dryness; add an ethanol solution of 3 to 5 times the weight of kudzu in the reaction chamber, shake and wash for 40 to 60 minutes and perform the filtration; extract the filtration residue after being dried twice with water, in which each time, the amount of water is 6 to 8 times the weight of the residue, the extraction temperature is 70 ° C and the extraction time is about 40 minutes; perform filtration, combine the two filtrate solutions and concentrate the filtrate solution to 1/5 the volume of the original extraction solution; then, add ethanol for precipitation and dry the precipitates to obtain kudzu polysaccharides; the process is a process for preparing lucid ganoderma polysaccharides which comprises: placing sporocarp of ganoderma lucid after being sprayed and degreased by ethanol in a microwave extraction chamber, adding 10% to 35% oxalic acid solution 1 , 5 to 2.5 times its weight, in a microwave power density of 1 to 2 kW / Kg under pressure of 500 mmHg to 760 mmHg, maintaining the reflux of the oxalic acid solution for 15 to 25 min and then evaporate the liquid a under reduced pressure to dryness; add an ethanol solution of 3 to 5 times the weight of sporocarp of lucid ganoderma in the reaction chamber, shake and wash for 40 to 60 minutes and perform the filtration; extract the filtration residue after being dried twice with water, in which each time, the amount of water is 6 to 8 times the weight of the residue, the extraction temperature is 70 ° C and the extraction time is about 40 minutes; perform filtration and combine the two filtrate solutions and concentrate the filtrate solution to 1/5 the volume of the original extraction solution; then, add ethanol for precipitation and dry the precipitates to obtain the lucid ganoderma polysaccharides; poria polysaccharides comprising: placing poria, after being sprayed and degreased by ethanol in a microwave extraction chamber, add 30% to 85% formic acid solution from 1.5 to 2.5 times the weight of at a microwave power density of 1 to 2 kW / kg under pressure from 500 mmHg to 760 mmHg, maintaining the reflux of the formic acid solution for 15 to 25 min and then evaporating under reduced pressure formic acid to dryness; add an ethanol solution of 3 to 5 times the pore weight in the reaction chamber, shake and wash for 40 to 60 minutes and perform the filtration; extract the filtration residue after being dried twice with water, in which each time, the amount of water is 6 to 8 times the weight of the residue, the extraction temperature is 70 ° C and the extraction time is about 40 minutes; perform filtration, combine the two filtrate solutions and concentrate the filtrate solution to 1/5 the volume of the original extraction solution; then, add ethanol for precipitation and dry the precipitates to obtain porous polysaccharides; the process is a process of preparing polysaccharides from exidia auricula judae which comprises: placing exidia auricula judae after being sprayed in a microwave extraction chamber, adding 60% to 95% acetic acid solution from 1.5 to 2 , 5 times its weight, in a microwave power density of 1 to 2 kW / Kg under pressure of 500 mmHg to 760 mmHg, maintaining the reflux of the acetic acid solution for 15 to 25 min and then , evaporate the acetic acid under reduced pressure to dryness; add an ethanol solution of 3 to 5 times the weight of exidia auricula judae in the reaction chamber, shake and wash for 40 to 60 minutes and perform the filtration; extract the filtration residue after being dried twice with water, in which each time, the amount of water is 6 to 8 times the weight of the residue, the extraction temperature is 70 ° C and the extraction time is about 40 minutes; perform filtration, combine the two filtrate solutions and concentrate the filtrate solution to 1/5 the volume of the original extraction solution; then, add ethanol for precipitation and dry the precipitates to obtain polysaccharides of exidia auricula judae; or the process is a mushroom polysaccharide preparation process that comprises: placing mushroom sporocarp after being sprayed in a microwave extraction chamber, adding 70% to 95% propionic acid solution from 1.5 to 2 , 5 times its weight, in a microwave power density of 1 to 2 kW / Kg under pressure of 500 mmHg to 760 mmHg, maintaining the reflux of the propionic acid solution for 15 to 25 min and then , evaporate propionic acid under reduced pressure to dryness; add an ethanol solution of 3 to 5 times the weight of the mushroom in the reaction chamber, shake and wash for 40 to 60 minutes and perform the filtration; extract the filtration residue after being dried twice with water, in which each time, the amount of water is 6 to 8 times the weight of the residue, the extraction temperature is 70 ° C and the extraction time is about 40 minutes; perform filtration, combine the two filtrate solutions and concentrate the filtrate solution to 1/5 the volume of the original extraction solution; then, add ethanol for precipitation and dry the precipitates to obtain mushroom polysaccharides.
[0015]
15. Astragalus polysaccharide, prepared using the process according to claim 14, characterized by the fact that the molecular weight distribution of said astragalus polysaccharide is from 3000 to 40,000; red medlar polysaccharide prepared using the process according to claim 14, wherein the molecular weight distribution of said red medlar polysaccharide is from 3000 to 20000; yam polysaccharides prepared using the process according to claim 14, wherein the molecular weight distribution of said yam polysaccharide is 3000 to 20000; gingko polysaccharide prepared using the process according to claim 14, wherein the molecular weight distribution of said gingko polysaccharide is 5000 to 12000; panax pseudoginseng polysaccharide, prepared using the process according to claim 14, wherein the molecular weight distribution of the panax pseudoginseng polysaccharide is 4000 to 20000; plantain polysaccharide, prepared using the process according to claim 14, wherein the molecular weight distribution of said plantain polysaccharide is 4000 to 30000; gastrodia elata polysaccharide prepared using the process according to claim 14, wherein the molecular weight distribution of said gastrodia elata polysaccharides is from 3000 to 20000; eucommia ulmoides polysaccharide prepared using the process according to claim 14, wherein the molecular weight distribution of said eucommia ulmoides polysaccharide is from 3000 to 20000; sage polysaccharides prepared using the process according to claim 14, wherein the molecular weight distribution of said sage polysaccharides is 5000 to 25000; kudzu polysaccharides prepared using the process according to claim 14, wherein the molecular weight distribution of said kudzu polysaccharide is from 3000 to 25000; lucid ganoderma polysaccharide prepared using the process according to claim 14, wherein the molecular weight distribution of the lucid ganoderma polysaccharide is from 3000 to 12000; poria polysaccharide prepared using the process according to claim 14, wherein the molecular weight distribution of said poria polysaccharides is from 2000 to 8000; exidia auricula judae polysaccharides prepared using the process according to claim 14, wherein the molecular weight distribution of the exidia auricula judae polysaccharide is 5000 to 40,000; or mushroom polysaccharide prepared using the process according to claim 14, wherein the molecular weight distribution of said mushroom polysaccharide is from 3000 to 15000.

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同族专利:

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公开号 | 公开日

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HUE031545T2|2017-07-28|

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PT2778177T|2017-02-17|

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ES2615752T3|2017-06-08|

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HRP20170118T1|2017-03-24|

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BR112014010924A2|2017-05-16|

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US20140309414A1|2014-10-16|

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RS55745B1|2017-07-31|

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DK2778177T3|2017-03-06|

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US9447198B2|2016-09-20|

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LT2778177T|2017-03-10|

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CY1118683T1|2017-07-12|

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JP5795444B2|2015-10-14|

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WO2013067897A1|2013-05-16|

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KR101605068B1|2016-03-21|

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CN102391387A|2012-03-28|

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SI2778177T1|2017-05-31|

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EP2778177B1|2017-01-04|

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SMT201700096B|2017-03-08|

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EP2778177A4|2015-07-29|

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CN102391387B|2013-02-27|

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PL2778177T3|2017-07-31|

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KR20140087051A|2014-07-08|

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EP2778177A1|2014-09-17|

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JP2014532788A|2014-12-08|

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法律状态:
2018-03-27| B06F| Objections, documents and/or translations needed after an examination request according art. 34 industrial property law|

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2020-09-01| B09A| Decision: intention to grant|

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2020-12-15| B16A| Patent or certificate of addition of invention granted|Free format text: PRAZO DE VALIDADE: 20 (VINTE) ANOS CONTADOS A PARTIR DE 01/11/2012, OBSERVADAS AS CONDICOES LEGAIS. |

优先权:

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申请号 | 申请日 | 专利标题

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CN201110348823XA|CN102391387B|2011-11-07|2011-11-07|Microwave chemical extraction method of active polysaccharide in higher plants or edible and medicinal fungi|

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CN201110348823.X|2011-11-07|

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PCT/CN2012/083934|WO2013067897A1|2011-11-07|2012-11-01|Method for extracting polysaccharides from higher plants and fungi through microwave chemical treatment|

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