CN108261418B - Preparation and drying method of pachyman powder - Google Patents
Preparation and drying method of pachyman powder Download PDFInfo
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Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/70—Carbohydrates; Sugars; Derivatives thereof
- A61K31/715—Polysaccharides, i.e. having more than five saccharide radicals attached to each other by glycosidic linkages; Derivatives thereof, e.g. ethers, esters
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/14—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/331—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation or decoction
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Medicinal Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- Pharmacology & Pharmacy (AREA)
- Engineering & Computer Science (AREA)
- Veterinary Medicine (AREA)
- Molecular Biology (AREA)
- Public Health (AREA)
- Animal Behavior & Ethology (AREA)
- Epidemiology (AREA)
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- Organic Chemistry (AREA)
- Polymers & Plastics (AREA)
- Sustainable Development (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Bioinformatics & Cheminformatics (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention belongs to the technical field of traditional Chinese medicine pharmacy, and particularly discloses a preparation and drying method of pachyman powder, which is a method for preparing and drying pachyman powder by taking poria as a raw material. The method comprises an extraction step, a desalination step and a drying step, adopts sodium hydroxide solution or sodium bicarbonate solution to stir and extract, greatly reduces the consumption and energy consumption of organic reagents, saves the production period and cost and is beneficial to environmental protection compared with the traditional ethanol precipitation method or ethanol reflux extraction method by water reflux extraction. In the drying step, a method of drying at normal pressure and then drying under reduced pressure to obtain the pachyman extract is adopted, so that the problems of low spray drying efficiency, poor product quality and the like caused by poor water solubility and difficulty in forming a homogeneous system in water of the pachyman are solved. The process is simple and easy to implement, and is beneficial to industrial production.
Description
Technical Field
The invention belongs to the technical field of traditional Chinese medicine pharmacy, and particularly relates to a method for preparing pachymaran powder by using poria as a raw material and drying the poria.
Background
In recent years, outbreaks of infectious diseases still occur after vaccination and the dosage of the vaccine is gradually increased to achieve an ideal treatment effect in animal husbandry. The phenomenon is largely due to the adverse effect caused by the reduction of the organism immune function of the livestock and poultry caused by the large amount of abused drugs and unreasonable vaccination for a long time. In animal production, how to improve the immunity of animals so as to reduce the morbidity of the animals and further improve the economic benefit of the animals becomes a problem which is concerned by relevant experts and farmers. Practice proves that effective means are adopted to activate an immune system, enhance the disease resistance of an organism, enable the livestock and poultry organism to obtain higher-level immune response after being inoculated with the vaccine, and enhance the immune effect of the vaccine.
The immunopotentiator can enhance the animal immune function, improve the animal disease resistance and the immune effect of the vaccine, thereby having wide prospect in preventing and controlling animal infectious diseases. At present, the research field of the chemical medicine immunopotentiator is greatly developed, and the chemical medicine immunopotentiator plays a positive role in the healthy development of the animal husbandry. However, the immunopotentiators of the chemical drugs have the problems of reducing the production performance of animals, even having toxic and side effects and drug residues to different degrees, and further harming the health of human beings, so the research on the immunopotentiators of the Chinese herbal medicines is increasingly concerned by people.
Poria Poriacos (Schw.) Wolf is a dry sclerotium of Poria cocos (a fungus in Polyporaceae), has a long history of clinical application, and is recorded in the classic medical book Shen nong Ben Cao Jing in China and the pharmacopoeia of the people's republic of China in the past edition. The traditional Chinese medicine considers that the tuckahoe can tonify qi, benefit vitality, eliminate pathogenic factors and strengthen body resistance.
Poria cocos Polysaccharides (PWP) is considered as a main active ingredient in a Poria cocos extract and has various biological activities of resisting tumors and viruses, enhancing immunity and the like, a large number of researches show that the total Polysaccharides of the Poria cocos extract have an immunoregulation effect on an immune system, the pachyman has wide influences on specific and non-specific immunity of organisms, humoral immunity and cellular immunity, the pachyman can increase the content of immunoglobulin IgG in the humoral immunity, and the pachyman can activate macrophages and enhance the phagocytic capacity of phagocytes in the aspect of cellular immunity.
The prior art develops and prepares pachyman powder based on various pharmacological activities of pachyman. And according to pharmacological and clinical results, the composition is used for enhancing the immune function of animals and improving the antibody level of vaccines.
At present, there are some published reports on extracting pachymaran from poria, but all have certain disadvantages, such as:
the wang school, in 2016, published under No. CN106046192A, entitled "a process for extracting polysaccharides from poria", selected poria raw materials, ultrafine-pulverized to obtain poria powder, ultrasonically extracted with water, centrifuged, separated by enzymatic hydrolysis with complex enzyme to obtain filtrate, removed protein, concentrated to obtain pachyman concentrate, spray-dried to obtain pachyman, ultrafiltered, subjected to column chromatography to obtain purified pachyman, and freeze-dried to obtain pachyman. However, the method adopts ultrasonic extraction, industrial amplification production is not easy to realize, and the obtained polysaccharide is hydrolyzed by using complex enzyme to obtain the micromolecule polysaccharide, but no relevant theory supports that the micromolecule pachyman has better biological activity.
Liu Zhi means applies in 2015 patent publication No. CN105639617A entitled "a comprehensive development and application method of Poria and its new use" to crush Poria sclerotium, add water to soak, reflux, extract, filter, concentrate the extract and dry to obtain water-soluble pachyman; extracting filter residue with sodium hydroxide solution, vacuum filtering, washing filter residue with water to neutral to prepare dietary fiber, adjusting pH of filtrate to weak acidity, filtering, drying to obtain Poria total triterpene and alkali soluble pachyman mixture, drying, adding into ethanol water solution, dissolving, and filtering to obtain Poria total triterpene alcohol solution and alkali soluble pachyman solid; washing alkali soluble pachyman with water and drying to obtain the final product; concentrating and drying the alcoholic solution of the total triterpene of Poria cocos to obtain the total triterpene of Poria cocos. The method considers each effective component in Poria, but is not beneficial to actual production operation, and has complicated process and high energy consumption.
In patent application No. CN105132491A published in 2015 in Wanan, entitled "a pachyman extraction method", Poria is crushed, expanded by adding water, fermented by adding yeast and lactobacillus, mixed uniformly, hydrolyzed by adding complex enzyme preparation, precipitated by alcohol, and spray-dried to obtain the final product. The method adopts fermentation, enzyme hydrolysis and other methods to hydrolyze pachyman, the process is complicated, and due to the fact that a large amount of enzyme hydrolysis is carried out, polysaccharide components are hydrolyzed into monosaccharide, disaccharide and other components to a great extent, pharmacological activity of the polysaccharide is lost, and therefore biological activity of the pachyman obtained by the method has a certain question.
Extracting Poria cocos wolf with ethanol, extracting residue with water, collecting filtrate, concentrating the filtrate into extract, precipitating with ethanol, and centrifuging to obtain precipitate; washing the precipitate with absolute ethyl alcohol and acetone in sequence, dissolving the washed precipitate with distilled water, passing through a hollow fiber membrane with the molecular weight cutoff of 6 ten thousand, collecting the concentrated solution, passing the concentrated solution through a hollow fiber membrane with the molecular weight cutoff of 10 ten thousand, collecting the permeate, centrifuging, filtering, and taking the filtrate for later use; spray drying the filtrate to obtain pachyman. The method has the advantages of relatively complicated process, high process cost due to the adoption of ethanol extraction and membrane filtration, and relatively low yield in the spray drying process due to poor water solubility of the obtained macromolecular polysaccharide.
Yuan 2014 is prepared by pulverizing Poria, sieving, and mixing with ethanol at a certain ratio in patent application with publication No. CN104208107A entitled Poria extract and its preparation method and application; placing the mixture in microwave extraction equipment for microwave extraction; filtering with microporous membrane, discarding residue, mixing filtrates to obtain liquid Poria extract, or concentrating the filtrate, and drying to obtain solid Poria extract. The processes of microwave extraction, filtration by an air filter membrane and the like adopted in the method are difficult to be produced in an enlarged mode, and the process cost and the equipment investment are high.
The method of the patent application with publication number CN101757045A and name "a preparation method of pachyman" in songdeng of 2008 is: weighing Poria, slicing, pulverizing, adding water, extracting under reflux, concentrating under reduced pressure, precipitating with ethanol, and collecting precipitate to obtain pachyman. Although the water extraction and ethanol precipitation method is a conventional method for extracting macromolecular substances such as polysaccharide, the water-soluble pachyman only accounts for about 4 percent of the weight of the polysaccharide, and most of the water-insoluble polysaccharide is used, so the resource utilization rate of the pachyman prepared by the method is extremely low.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a preparation and drying method of pachyman powder, which solves the problems of high consumption and high energy consumption of organic reagents in the existing water reflux extraction ethanol precipitation method or ethanol reflux extraction method, and solves the problem that the existing ultrasonic extraction and enzyme extraction are not easy to realize industrial production. The method for obtaining the pachyman extract by drying at normal pressure and then drying under reduced pressure solves the problems of low efficiency, poor product quality and the like of the existing spray drying, has simple and easy process, and is beneficial to industrial production.
The invention relates to a preparation and drying method of pachyman powder, which comprises the following steps:
(1) the extraction step comprises: taking poria cocos blocks, crushing, sieving with a 14-80-mesh sieve to obtain poria cocos powder, adding an alkali solution, stirring and extracting, centrifuging at 800-2400 rpm to obtain a supernatant, adjusting the pH value of the supernatant with an acid, standing for 30-90 min, and centrifuging at 800-2400 rpm to obtain a precipitate;
(2) a desalting step: adding water into the precipitate obtained in the step (1), stirring, standing, centrifuging at 800-2400 rpm to obtain a precipitate as a polysaccharide desalting product, and repeating the desalting process for 2-4 times;
(3) and (3) drying: and (3) taking the polysaccharide desalted product obtained in the desalting step (2), drying at normal pressure, then drying at reduced pressure to obtain a pachyman extract, and crushing the pachyman extract and sieving with a 40-100-mesh sieve to obtain the pachyman powder.
Preferably, in the extraction step (1), the aqueous alkali is 0.1-1.5 mol/L sodium hydroxide solution or 0.2-2.0 mol/L sodium bicarbonate solution, the mass ratio of the added aqueous alkali to the tuckahoe powder is 10-30 m L: 1g, the stirring extraction is carried out at the stirring speed of 40-100 rpm and at the temperature of 25-70 ℃ for 20-60 min, the pH value of the supernatant is adjusted by acid, and the pH value of the supernatant is adjusted to 6.5-9.0 by adding one of 4-10 mol/L hydrochloric acid solution or 6-12 mol/L sulfuric acid solution;
preferably, in the desalting step (2), the water is added, wherein the volume ratio of the added water to the mass of the precipitate obtained in the extracting step is 3-6L: 1kg, and the stirring and standing process comprises the steps of adding water, stirring at 25-60 ℃ for 20-40 min, stirring at the rotating speed of 40-100 rpm, and standing for 20-60 min;
preferably, in the drying step (3), the atmospheric drying is: drying at 60-90 ℃ for 2-5 hours; the reduced pressure drying comprises the following steps: the drying vacuum degree is-0.06 to-0.1 Mpa, the drying temperature is 50 to 80 ℃, and the drying time is 1.5 to 3 hours.
Compared with the prior art, the invention has the advantages and beneficial effects that:
the invention discloses a method for preparing pachymaran powder by taking poria as a raw material and drying the poria. Compared with the traditional ethanol precipitation method or ethanol reflux extraction method by water reflux extraction, the method greatly reduces the consumption and energy consumption of organic reagents, saves the production period and cost, is beneficial to environmental protection, and also solves the problem that the existing ultrasonic extraction and enzyme extraction are not easy to realize industrial production.
Common drying methods for the traditional Chinese medicine extract concentrated solution mainly comprise normal-pressure drying, reduced-pressure drying, spray drying and the like, in the earlier research, the pachyman extract is respectively dried by three modes (see examples 7, 8 and 9 for details), and the result shows that the spray drying time is shortest, but the yield is lowest, and the serious wall hanging phenomenon can occur in the spraying process due to poor dispersibility of the pachyman in water, so that the yield is low; the drying time under normal pressure is relatively short, the yield of the finished product is high, but the situation of 'boiling tuckahoe' can occur due to long-time high temperature, so that the finished product has dark gray color, hardness and incomplete crushing; the yield of the finished product dried under reduced pressure is high, the quality is good, but the drying speed is reduced probably because the moisture content of the poria cocos is high at the beginning of drying, even though the vacuum pump continuously pumps air, water drops are hung on the wall of the drying box, the humidity in the drying box is too high, and the situation is in a non-complete vacuum state, and the drying is not thorough because the moisture content of the surface of the material is high.
In summary of the above results, the method of drying under normal pressure and then drying under reduced pressure to obtain pachyman extract of the present invention solves the problems of low spray drying efficiency, poor product quality during normal pressure drying, incomplete drying during reduced pressure drying, etc. due to poor water solubility of pachyman and difficulty in forming a homogeneous system in water. The process is simple and easy to implement and is beneficial to industrial production.
Detailed Description
The applicant below further elaborates the technical solution of the present invention with reference to specific embodiments.
Example 1a method for preparing and drying pachyman powder, comprising the steps of:
(1) the extraction step comprises the steps of taking poria cocos blocks, crushing and sieving the poria cocos blocks through a sieve of 80 meshes to obtain 500g of poria cocos powder, adding 1.5 mol/L of sodium hydroxide solution 15L, adding the poria cocos powder with the volume of 30m L: 1g, stirring at 50 ℃ for 60min, stirring at the rotating speed of 100rpm, after stirring and extraction are finished, centrifuging at 2400rpm to obtain a supernatant, adding 6 mol/L of hydrochloric acid solution into the supernatant, adjusting the pH value to 9.0, standing for 90min, and centrifuging at 800rpm to obtain 3.15kg of precipitate;
(2) desalting, namely adding 18.9L water into 3.15kg of the precipitate obtained in the extraction step (1), wherein the volume ratio of the added water to the precipitate obtained in the extraction step is 6L: 1kg, stirring at 60 ℃ for 20min, stirring at the rotating speed of 100rpm, standing for 20min after stirring, and centrifuging at 800rpm to obtain the precipitate;
precipitating, repeating the above desalting process with water (each time adding water amount is 18.9L) for 2 times to obtain 2.85kg of polysaccharide desalted product;
(3) and (3) drying: taking 2.85kg of polysaccharide desalted product obtained in the desalting step (2), and drying for 5 hours at normal pressure and the drying temperature of 60 ℃; drying under vacuum degree of-0.085 Mpa for 3 hr at 50 deg.C to obtain pachyman extract, pulverizing, and sieving with 100 mesh sieve to obtain pachyman powder 225 g.
The polysaccharide content, yield and pharmacological activity of the pachymaran powder obtained in the embodiment are determined, the polysaccharide content is 85.3%, the yield is 45.0%, the activity of the pachymaran powder on the immune inhibition mice is determined by 40 SPF grade healthy Kunming mice, half female and half male mice, 18-22g, 10 mice are randomly divided into 4 groups, 14 days are continuously administered, a blank group is a blank group, 0.9% of physiological saline is perfused into stomach, 0.3ml/d is injected into stomach, 14d is continuously administered into stomach, a model group (a hydrocortisone group) is a group, 0.9% of physiological saline is administered into a front 4d and a rear 4d group, 0.3ml/d is phagocytosis of hydrocortisone is subcutaneously injected into 5-10d, 0.3ml/d is subcutaneously injected into each mouse, the dosage is 50 pg/kg, 0.9% of physiological saline is administered into each, 0.3ml/d is administered into a positive control group, the front 4d and the rear 4d and 4d is a group, 0.3 mg macrophage phagocytosis group (a mice) is a 10 mg phagocytosis promoting group, the mouse is a mouse phagocytosis promoting mouse, the mouse is a mouse, the mouse is a mouse, the mouse is a mouse, the mouse is a mouse, the mouse is a mouse, the mouse is a mouse, the mouse is a mouse, the mouse is a mouse, the mouse is a mouse, the mouse is a mouse, the.
Embodiment 2a method for preparing and drying pachyman powder, comprising the steps of:
(1) the extraction step comprises the steps of taking poria cocos blocks, crushing and sieving the poria cocos blocks through a 14-mesh sieve to obtain 1000g of poria cocos powder, adding 0.1 mol/L of sodium hydroxide solution 10L, adding the poria cocos powder with the volume ratio of 10m L: 1g, stirring at 25 ℃ for 40min, and stirring at the rotating speed of 40rpm, after stirring and extraction are finished, centrifuging at 800rpm to obtain a supernatant, adding 10 mol/L of hydrochloric acid solution into the supernatant, adjusting the pH value to 6.5, standing for 30min, and centrifuging at 2400rpm to obtain 5.95kg of precipitate;
(2) desalting, namely taking 5.95kg of precipitate obtained in the extraction step (1), adding 17.85L of water, wherein the volume ratio of the added precipitate to the mass ratio of the precipitate obtained in the extraction step is 3L: 1kg, stirring at 25 ℃ for 40min, stirring at the rotating speed of 40rpm, standing for 60min after stirring, and centrifuging at 2400rpm to obtain precipitate;
precipitating, repeating the desalting process with water (17.85L for each time) for 4 times to obtain desalted polysaccharide product 5.20 kg;
(3) and (3) drying: taking 5.20kg of polysaccharide desalted product obtained in the desalting step (2), and drying for 2 hours at normal pressure and the drying temperature of 90 ℃; then drying under vacuum degree of-0.1 Mpa for 2 hr at 70 deg.C to obtain pachyman extract, pulverizing, and sieving with 40 mesh sieve to obtain pachyman powder 433 g.
The content, yield and pharmacological activity of the pachymaran powder obtained in the example are respectively 83.5% and 43.3%, the influence of the pachymaran powder on the chicken red blood cell phagocytizing capacity of phagocytic cells of immunosuppressed mice, immune factors and immune organs is measured, and animal experiments and test methods are as in example 1. the experimental results show that compared with a hydrocortisone model group (the phagocytosis rate is 30.20%, the spleen index is 0.25, the thymus index is 0.16, the content of I L-2 is 7.62pg/m L- α is 6.03pg/m L.), the pachymaran powder can effectively promote the phagocytic capacity of phagocytic cells, the phagocytic rate is 48.13%, effectively promote the increase of the spleen index and the thymus index, the spleen index is 0.29, the thymus index is 0.18, and effectively promote the secretion of I2-2 and TNF- α, and the content of mouse serum is I L-211.59/m L and TNF- α.21pg/m L respectively.
Embodiment 3 a method for preparing and drying pachyman powder, comprising the steps of:
(1) the extraction step comprises the steps of taking poria cocos blocks, crushing and sieving the poria cocos blocks through a 60-mesh sieve to obtain 500g of poria cocos powder, adding 1.0 mol/L of sodium hydroxide solution 10L, adding the poria cocos powder with the volume ratio of 20m L: 1g, stirring at 70 ℃ for 20min, and stirring at the rotating speed of 80rpm, after stirring and extraction are finished, centrifuging at 1200rpm to obtain a supernatant, adding 4 mol/L of hydrochloric acid solution into the supernatant, adjusting the pH value to 7.5, standing for 60min, and centrifuging at 1200rpm to obtain 3.00kg of precipitate;
(2) desalting, namely extracting 3.00kg of the precipitate obtained in the step (1), adding 15.0L of water, wherein the mass ratio of the added volume to the precipitate obtained in the step (1) is 5L: 1kg, stirring at 40 ℃ for 30min, stirring at the rotating speed of 80rpm, standing for 40min after stirring, and centrifuging at 1200rpm to obtain the precipitate;
precipitating, repeating the above desalting process with water (15.0L per time) for 3 times to obtain 2.80kg desalted polysaccharide product;
(3) and (3) drying: taking 2.80kg of polysaccharide desalted product obtained in the desalting step (2), and drying for 4 hours at normal pressure and the drying temperature of 80 ℃; then drying under vacuum degree of-0.06 Mpa for 1.5 hr at 80 deg.C to obtain pachyman extract, pulverizing, and sieving with 80 mesh sieve to obtain pachyman powder 210 g.
The content, yield and pharmacological activity of the pachymaran powder obtained in the example are measured, the content and yield of the polysaccharide are 87.1% and 42.0%, the influence on the chicken red blood cell phagocytizing capacity of phagocytic cells of immunosuppressed mice, immune factors and immune organs is measured, animal experiments and a test method are the same as those in example 1, and the experimental results show that compared with a hydrocortisone model group (the phagocytosis rate is 30.20%, the spleen index is 0.25, the thymus index is 0.16, the content of I L-2 is 7.62pg/m L- α is 6.03pg/m L.), the pachymaran powder can effectively promote the phagocytic capacity of phagocytic cells, the phagocytic rate is 48.13%, the spleen index and the thymus index are effectively promoted to be increased, the spleen index is 0.29, the thymus index is 0.19, the secretion of I2-2 and TNF- α is effectively promoted, and the content of the mouse serum is I L-214.21/m L and TNF- α.72pg/m L respectively.
Embodiment 4 a method for preparing and drying pachyman powder, comprising the steps of:
(1) the extraction step comprises the steps of taking poria cocos blocks, crushing and sieving the poria cocos blocks through a 24-mesh sieve to obtain 1000g of poria cocos powder, adding 2.0 mol/L of sodium bicarbonate solution 25L, adding the poria cocos powder with the volume ratio of 25m L: 1g, stirring at 25 ℃ for 60min, and stirring at the rotating speed of 60rpm, after stirring and extraction are finished, centrifuging at 1200rpm to obtain a supernatant, adding 12 mol/L of sulfuric acid solution into the supernatant, adjusting the pH value to 9.0, standing for 30min, and centrifuging at 1200rpm to obtain 6.30kg of precipitate;
(2) desalting, namely taking 6.30kg of the precipitate obtained in the extraction step (1), adding 31.50L of water, wherein the volume ratio of the added water to the precipitate obtained in the extraction step is 5L: 1kg, stirring at 25 ℃ for 20min, stirring at the rotating speed of 60rpm, standing for 30min after stirring, and centrifuging at 1200rpm to obtain the precipitate;
precipitating, repeating the above desalting process with water (31.50L per time) for 3 times to obtain 5.65kg desalted polysaccharide product;
(3) and (3) drying: taking 5.65kg of polysaccharide desalted product obtained in the desalting step (2), drying for 5 hours under normal pressure, wherein the drying temperature is 85 ℃; then drying under vacuum degree of-0.09 Mpa for 3 hr at 70 deg.C to obtain pachyman extract, pulverizing, and sieving with 60 mesh sieve to obtain pachyman powder 465 g.
The content, yield and pharmacological activity of the polysaccharide of the pachymaran powder obtained in the embodiment are determined, the content and yield of the polysaccharide are 84.2% and 46.5%, the influence of the polysaccharide on the chicken red blood cell phagocytizing capacity of a phagocyte of an immunosuppressed mouse, an immune factor and an immune organ is determined, and an animal test and a test method are as in example 1. the test result shows that compared with a hydrocortisone model group (the phagocytosis rate is 30.20%, the spleen index is 0.25, the thymus index is 0.16, the content of I L-2 is 7.62pg/m L- α is 6.03pg/m L.), the phagocytic capacity of the phagocyte can be effectively promoted, the phagocyte rate is 48.51%, the spleen index and the thymus index are effectively promoted to be increased, the spleen index is 0.27, the thymus index is 0.17, the secretion of I L-2 and TNF- α can be effectively promoted, and the content of the mouse serum is I L-213.25/m L and TNF- α 44.33.33 pg/m L respectively.
Example 5a method for preparing and drying pachyman powder, comprising the steps of:
(1) the extraction step comprises the steps of taking poria cocos blocks, crushing and sieving the poria cocos blocks through a 60-mesh sieve to obtain 1000g of poria cocos powder, adding 0.2 mol/L of sodium bicarbonate solution 20L, adding the poria cocos powder with the volume ratio of 20m L: 1g, stirring at 60 ℃ for 40min, and stirring at the rotating speed of 100rpm, after stirring and extraction are finished, centrifuging at 2400rpm to obtain a supernatant, adding 6 mol/L of sulfuric acid solution into the supernatant, adjusting the pH value to 7.0, standing for 45min, and centrifuging at 2400rpm to obtain 5.80kg of precipitate;
(2) desalting, namely taking 5.80kg of the precipitate obtained in the extraction step (1), adding 34.80L of water, wherein the volume ratio of the added water to the precipitate obtained in the extraction step is 6L: 1kg, stirring at 25 ℃ for 40min, stirring at the rotating speed of 100rpm, standing for 60min after stirring, and centrifuging at 800rpm to obtain the precipitate;
precipitating, repeating the above desalting process with water (34.80L per time) for 2 times to obtain 5.50kg desalted polysaccharide product;
(3) and (3) drying: taking 5.50kg of polysaccharide desalted product obtained in the desalting step (2), and drying for 4 hours at normal pressure and the drying temperature of 80 ℃; then drying under vacuum degree of-0.09 Mpa for 1.5 hr at 80 deg.C to obtain pachyman extract, pulverizing, and sieving with 80 mesh sieve to obtain pachyman powder 440 g.
The content, yield and pharmacological activity of the pachymaran powder obtained in the example are respectively 82.5% and 44.0%, the influence of the pachymaran powder on the chicken red blood cell phagocytizing capacity of phagocytic cells of immunosuppressed mice, immune factors and immune organs is measured, animal experiments and a test method are as in example 1, and the experimental results show that compared with a hydrocortisone model group (the phagocytosis rate is 30.20%, the spleen index is 0.25, the thymus index is 0.16, the content of I L-2 is 7.62pg/m L- α is 6.03pg/m L.), the pachymaran powder can effectively promote the phagocytic capacity of phagocytic cells, the phagocytic rate is 47.32%, effectively promote the increase of the spleen index and the thymus index, the spleen index is 0.28, the thymus index is 0.18, and effectively promote the secretion of I2-2 and TNF- α, and the content of mouse serum is I L-212.81/m L and TNF- α.12pg/m L respectively.
Embodiment 6 a method for preparing and drying pachyman powder, comprising the steps of:
(1) the extraction step comprises the steps of taking poria cocos blocks, crushing and sieving the poria cocos blocks through a 80-mesh sieve to obtain 500g of poria cocos powder, adding 1.0 mol/L of sodium bicarbonate solution 10L, adding the poria cocos powder with the volume ratio of 20m L: 1g, stirring at 25 ℃ for 60min, and stirring at the rotating speed of 80rpm, after stirring and extraction are finished, centrifuging at 1200rpm to obtain a supernatant, adding 10 mol/L of sulfuric acid solution into the supernatant, adjusting the pH value to 9.0, standing for 20min, and centrifuging at 1200rpm to obtain 3.20kg of precipitate;
(2) desalting, namely adding 16.0L of water into 3.20kg of the precipitate obtained in the extraction step (1), wherein the volume ratio of the added water to the precipitate obtained in the extraction step is 5L: 1kg, stirring the mixture at 25 ℃ for 30min at a stirring speed of 80rpm, standing the mixture for 30min after stirring, and centrifuging the mixture at 1200rpm to obtain a precipitate;
precipitating, repeating the above desalting process with water (16.0L for each time) for 3 times to obtain 2.85kg desalted polysaccharide product;
(3) and (3) drying: taking 2.85kg of polysaccharide desalted product obtained in the desalting step (2), and drying for 5 hours under normal pressure at the drying temperature of 90 ℃; then drying under vacuum degree of-0.09 Mpa for 3 hr at 70 deg.C to obtain pachyman extract, pulverizing, and sieving with 100 mesh sieve to obtain pachyman powder 232 g.
The content, yield and pharmacological activity of the polysaccharide of the pachymaran powder obtained in the embodiment are respectively 85.8% and 46.4%, the influence of the polysaccharide on the chicken red blood cell phagocytizing capacity of a phagocyte of an immunosuppressed mouse, an immune factor and an immune organ is measured, and an animal test and a test method are as in example 1. the test result shows that compared with a hydrocortisone model group (the phagocytosis rate is 30.20%, the spleen index is 0.25, the thymus index is 0.16, the content of I L-2 is 7.62pg/m L- α is 6.03pg/m L.), the pachymaran powder can effectively promote the phagocytic capacity of the phagocyte, the phagocyte rate is 48.02%, the spleen index and the thymus index are effectively promoted to be increased, the spleen index is 0.28, the thymus index is 0.19, the secretion of I L-2 and TNF- α is effectively promoted, and the content of the mouse serum is respectively I L-213.44/m L and TNF-36 α 46.28pg/m L.
Example 7a method for preparing and drying pachyman powder, comprising the steps of:
(1) the extraction step comprises the steps of taking poria cocos blocks, crushing and sieving the poria cocos blocks through a 60-mesh sieve to obtain 500g of poria cocos powder, adding 1.0 mol/L of sodium hydroxide solution 10L, adding the poria cocos powder with the volume ratio of 20m L: 1g, stirring at 70 ℃ for 20min, and stirring at the rotating speed of 80rpm, after stirring and extraction are finished, centrifuging at 1200rpm to obtain a supernatant, adding 4 mol/L of hydrochloric acid solution into the supernatant, adjusting the pH value to 7.5, standing for 60min, and centrifuging at 1200rpm to obtain 3.00kg of precipitate;
(2) desalting, namely taking 3.00kg of the precipitate obtained in the extraction step (1), adding 15.0L of water, wherein the volume ratio of the added water to the precipitate obtained in the extraction step is 5L: 1kg, stirring at 40 ℃ for 30min, stirring at the rotating speed of 80rpm, standing for 40min after stirring, and centrifuging at 1200rpm to obtain the precipitate;
precipitating, repeating the above desalting process with water (15.0L per time) for 3 times to obtain 2.80kg desalted polysaccharide product;
(3) and (3) drying: and (3) taking 2.80kg of polysaccharide desalted product obtained in the desalting step (2), drying for 8 hours under normal pressure at the drying temperature of 80 ℃ to obtain pachyman extract, and crushing the pachyman extract and sieving the pachyman extract by a sieve of 80 meshes to obtain 95g of pachyman powder.
The content, yield and pharmacological activity of the polysaccharide of the pachymaran powder obtained in the example are determined, the content and yield of the polysaccharide are 81.7 percent and 19.0 percent, the influence of the polysaccharide on the chicken red blood cell phagocytizing capacity of a phagocyte of an immunosuppressed mouse, an immune factor and an immune organ is determined, and an animal test and a test method are the same as those in example 1. the test result shows that compared with a hydrocortisone model group (the phagocytosis rate is 30.20 percent, the spleen index is 0.25, the thymus index is 0.16, the content of I L-2 is 7.62pg/m L- α is 6.03pg/m L.), the phagocytic capacity of the phagocyte can be effectively promoted, the phagocytic rate is 38.32 percent, the spleen index and the thymus index are effectively promoted to be increased, the spleen index is 0.26, the thymus index is 0.17, the secretion of I L-2 and the secretion of TNF- α can be effectively promoted, and the content of the mouse serum is respectively I L-210.59/m L and TNF- α 28.72.72 pg/m L.
Embodiment 8 a method for preparing and drying pachyman powder, comprising the steps of:
(1) the extraction step comprises the steps of taking poria cocos blocks, crushing and sieving the poria cocos blocks through a 60-mesh sieve to obtain 500g of poria cocos powder, adding 1.0 mol/L of sodium hydroxide solution 10L, adding the poria cocos powder with the volume ratio of 20m L: 1g, stirring at 70 ℃ for 20min, and stirring at the rotating speed of 80rpm, after stirring and extraction are finished, centrifuging at 1200rpm to obtain a supernatant, adding 4 mol/L of hydrochloric acid solution into the supernatant, adjusting the pH value to 7.5, standing for 60min, and centrifuging at 1200rpm to obtain 3.00kg of precipitate;
(2) desalting, namely taking 3.00kg of the precipitate obtained in the extraction step (1), adding 15.0L of water, wherein the volume ratio of the added water to the precipitate obtained in the extraction step is 5L: 1kg, stirring at 40 ℃ for 30min, stirring at the rotating speed of 80rpm, standing for 40min after stirring, and centrifuging at 1200rpm to obtain the precipitate;
precipitating, repeating the above desalting process with water (15.0L per time) for 3 times to obtain 2.80kg desalted polysaccharide product;
(3) and (3) drying: taking 2.80kg of polysaccharide desalted product obtained in the desalting step (2), drying under reduced pressure for 10 hours at 65 ℃ and under vacuum degree of-0.09 Mpa to obtain pachyman extract, pulverizing, and sieving with 80 mesh sieve to obtain pachyman powder 105 g.
The content, yield and pharmacological activity of the polysaccharide of the pachymaran powder obtained in the embodiment are respectively 82.3 percent and 21.0 percent, the influence of the polysaccharide on the chicken red blood cell phagocytizing capacity of a phagocyte of an immunosuppressed mouse, an immune factor and an immune organ is measured, and an animal test and a test method are as in example 1. the test result shows that compared with a hydrocortisone model group (the phagocytosis rate is 30.20 percent, the spleen index is 0.25, the thymus index is 0.16, and the content of I L-2 is 7.62pg/m L- α is 6.03pg/m L.), the pachymaran powder can effectively promote the phagocytic capacity of the phagocyte and the phagocyte rate is 40.63 percent, effectively promote the increase of the spleen index and the thymus index, the spleen index is 0.27, and the thymus index is 0.17, and can also effectively promote the secretion of I L-2 and TNF- α, and the content of the mouse serum is I L-211.49-L and TNF- α 35.62.62 pg/m L respectively.
Example 9 a method for preparing and drying pachyman powder, comprising the steps of:
(1) the extraction step comprises the steps of taking poria cocos blocks, crushing and sieving the poria cocos blocks through a 60-mesh sieve to obtain 500g of poria cocos powder, adding 1.0 mol/L of sodium hydroxide solution 10L, adding the poria cocos powder with the volume ratio of 20m L: 1g, stirring at 70 ℃ for 20min, and stirring at the rotating speed of 80rpm, after stirring and extraction are finished, centrifuging at 1200rpm to obtain a supernatant, adding 4 mol/L of hydrochloric acid solution into the supernatant, adjusting the pH value to 7.5, standing for 60min, and centrifuging at 1200rpm to obtain 3.00kg of precipitate;
(2) desalting, namely taking 3.00kg of the precipitate obtained in the extraction step (1), adding 15.0L of water, wherein the volume ratio of the added water to the precipitate obtained in the extraction step is 5L: 1kg, stirring at 40 ℃ for 30min, stirring at the rotating speed of 80rpm, standing for 40min after stirring, and centrifuging at 1200rpm to obtain the precipitate;
precipitating, repeating the above desalting process with water (15.0L per time) for 3 times to obtain 2.80kg desalted polysaccharide product;
(3) and (3) drying: and (3) taking 2.80kg of polysaccharide desalted product obtained in the desalting step (2), adding 1 time of water by mass, uniformly stirring in a water bath at 60 ℃, spray-drying for 4 hours, wherein the air inlet temperature is 170 ℃, the air outlet temperature is 90 ℃, the feeding speed is 1.3kg/h, and the rotation speed of a centrifugal disc is 29000rpm to obtain 20g of pachyman powder.
The content, yield and pharmacological activity of the polysaccharide of the pachymaran powder obtained in the example are respectively 83.2 percent and 4.0 percent, the influence of the polysaccharide on the chicken red blood cell phagocytizing capacity of a phagocyte of an immunosuppressed mouse, an immune factor and an immune organ is measured, and an animal test and a test method are as in example 1. the test result shows that compared with a hydrocortisone model group (the phagocytosis rate is 30.20 percent, the spleen index is 0.25, the thymus index is 0.16, the content of I L-2 is 7.62pg/m L- α is 6.03pg/m L.), the phagocytic capacity of the phagocyte can be effectively promoted, the phagocyte rate is 42.45 percent, the spleen index and the thymus index are effectively promoted to be increased, the spleen index is 0.26, the thymus index is 0.17, the secretion of I L-2 and TNF- α can be effectively promoted, and the content of the mouse serum is respectively I L-210.35/m L and TNF- α 37.54.54 pg/m L.
Claims (3)
1. A method for preparing pachyman powder comprises:
(1) an extraction step; taking poria cocos blocks, crushing, sieving with a 14-80-mesh sieve to obtain poria cocos powder, adding an alkali solution, stirring and extracting, centrifuging at 800-2400 rpm to obtain a supernatant, adjusting the pH value of the supernatant with an acid, standing for 30-90 min, and centrifuging at 800-2400 rpm to obtain a precipitate;
(2) a desalting step; adding water into the precipitate obtained in the step (1), stirring, standing, and centrifuging at 800-2400 rpm to obtain a precipitate as a polysaccharide desalination product, which is a primary desalination process; the desalting process is repeated for 2-4 times;
(3) a drying step; drying the polysaccharide desalted product obtained in the step (2) at normal pressure, and then drying at reduced pressure to obtain pachyman extract;
(4) pulverizing the pachymaran extract obtained in the step (3), and sieving with a 40-100-mesh sieve to obtain pachymaran powder;
in the drying step (3), the normal pressure drying process comprises the following steps: drying at 60-90 ℃ for 2-5 hours; the process of reduced pressure drying is as follows: the drying vacuum degree is-0.06 to-0.1 Mpa, the drying temperature is 50 to 80 ℃, and the drying time is 1.5 to 3 hours.
2. The method for preparing pachyman powder according to claim 1, wherein in the step (1), the aqueous alkali is added in an amount of 0.1-1.5 mol/L sodium hydroxide solution or 0.2-2.0 mol/L sodium bicarbonate solution, the volume of the aqueous alkali and the weight ratio of the Poria cocos powder are 10-30 m L: 1g, the stirring and extraction process is that the aqueous alkali is stirred at a rotating speed of 40-100 rpm for 20-60 min at a temperature of 25-70 ℃, and the pH value of the supernatant is adjusted by adding 4-10 mol/L hydrochloric acid solution or 6-12 mol/L sulfuric acid solution into the supernatant, and the pH value is adjusted to 6.5-9.0.
3. The method for preparing pachymaran powder according to claim 1, wherein in each desalting step (2), the weight ratio of the volume of water added to the precipitate obtained in the extraction step is 3-6L: 1kg, and the stirring and standing process comprises adding water, stirring at a rotation speed of 40-100 rpm for 20-40 min at 25-60 ℃, and standing for 20-60 min.
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