CN109432141A - A kind of preparation method of Phellinus composition and the application in terms of medical treatment - Google Patents

A kind of preparation method of Phellinus composition and the application in terms of medical treatment Download PDF

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CN109432141A
CN109432141A CN201811317389.7A CN201811317389A CN109432141A CN 109432141 A CN109432141 A CN 109432141A CN 201811317389 A CN201811317389 A CN 201811317389A CN 109432141 A CN109432141 A CN 109432141A
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phellinus
water
tree extract
composition
dihydroquercetin
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丁传波
郑毅男
刘文丛
赵婷
郑冰
张伟
刘兴龙
陈雪燕
赵迎春
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    • A61K36/15Pinaceae (Pine family), e.g. pine or cedar
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    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
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    • A61K2236/30Extraction of the material
    • A61K2236/39Complex extraction schemes, e.g. fractionation or repeated extraction steps
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/50Methods involving additional extraction steps
    • A61K2236/53Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization

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Abstract

Fresh Phellinus fructification is by broken wall, the processing of high-pressure homogeneous and super-high-pressure homogenization; it is mixed with dihydroquercetin Larch tree extract, Arabic gum and resistant dextrin; it is placed in the superhigh-voltage homogenizing machine of 50-250 megapascal and handles; it is substantially reduced Phellinus Powder Particle Size; change the structure of contained macromolecular compound such as Phellinus polysaccharide in Phellinus; increase the water solubility of wherein small molecule compound, to be more convenient for being absorbed and utilized, improves bioavilability.Parasitic Phellinus and host's Larch tree extract passes through scientific disposal, and cooperates with Arabic gum and resistant dextrin, hence it is evident that the solubility of dihydroquercetin in enhancing Larch tree extract, hence it is evident that increase the antioxidation of Phellinus composition, enhance clinical effect effect.

Description

A kind of preparation method of Phellinus composition and the application in terms of medical treatment
Technical field
The present invention relates to the applications of the compatibility of Phellinus composition and extraction preparation method and anti-oxidant aspect, belong to biology Technical field.
Background technique
Wild Phellinus (Phellinus igniarius) be distributed in Changbaishan area, Phellinus is a kind of food full of nutrition Medicament dual-purpose type fungi, has no toxic side effect, and is known as the laudatory title of " forest gold ".Phellinus mildly bitter flavor, can relieving the five internal organs, softening hard masses, toxin expelling;Only Blood, promoting blood circulation;Stomach function regulating antidiarrheal.Modern pharmacology research shows that Phellinus has anti-inflammatory, anti-diabetic, and anti-oxidant, Immune-enhancing effect resists Mutagenesis, anticancer and antitumor action.Currently, Phellinus is efficient highest a kind of food in biology field for cancer generally acknowledged in the world Medicinal fungi, anticancer effect get well (Fu Haiqing, 2005) also it has been reported that " polyphenol extract thans ganoderma lucidum and Brazilian mushroom etc. Can be used for preventing ishemic stroke " (Papawee Suabjakyong, 2015);It is reported that Phellinus general flavone has significantly Effect for reducing blood fat and anti-aging effects (Li Shanji, 2015);It is obtained from phellinus igniarius mycelium fermentation liquid preparation Phellinus crude extract Cyclic dipeptides C4, this compound has been reported at present to be had the function of inhibiting Vibrio anguillarum breeding (103073550 A of CN);Phellinus bacterium is thick Extract carries out purification on normal-phase silica gel chromatography, is eluted using chloroform and methanol, followed by methanol gel chromatographs, and after HPLC is detected, carries out The preparation of high pressure reverse phase, is detected through HPLC, suitably merging eluent, is dried under reduced pressure to get Cyclic dipeptides C6, i.e. hexahydro-7-hydroxyl Base-3-(2-methyl-propyl) pyrrolo- [1,2- ɑ) pyrazine-Isosorbide-5-Nitrae-diketone, this compound has been reported anti-with wide spectrum at present Bacterium acts on (103145716 A of CN).A kind of method of Phellinus general flavone in enriching and purifying Phellinus, utilizes batch distillation-macropore to inhale The method (102078339 A of CN) of Phellinus general flavone in attached resin coupled method enriching and purifying Phellinus;ー kind extracts Phellinus polysaccharide Method, technique be Phellinus through sorting, cleaning, slice, immersion, ultra high pressure treatment, boiling, filtration sterilization and obtain Phellinus polysaccharide Stoste, slice time slice thickness are 0.3-0.5mm, impregnate there are about half an hour, ultra high pressure treatment 200-300MPa, are kept for 10-15 points Clock, then through boiling, boiled in 100 °C of boiling water 1-2 hours, the ratio of Phellinus and water is 1:40, takes out cooking liquid and goes out through Pasteur Bacterium handles and obtains (CN101463093);Phellinus polysaccharide is prepared with high performance countercurrent chromatography, using ultrasonic extraction method from Phellinus fructification The yield of middle extraction Phellinus Thick many candies, Phellinus Thick many candies is high, and generally 2%, this law is up to 6%(CN200810041120.0).
Recently research have indicated that the triterpene substance in Phellinus has the function of improving immunity rapidly, promotion lymph is shown Cell Proliferation improves macrophage, NK cell, the phagocytic activity of T cell and lethality, and directly or indirectly poisoning tumour is thin Born of the same parents, at the same can activated chemotherapy drug be difficult to the dormant period tumour cell killed, carry out individually and joint poisoning (CN 102628064 A).The active constituent of Phellinus, wherein based on polysaccharide (103059155 A of CN).
Research finds P. igniarius phenols rich in and polysaccharide, and has more higher than P. linteus SOD sample activity.P. igniarius ratio P. linteus more likely develops antioxidant and immunological regulation food.Edible mushroom Moisture and crude fiber content are respectively 90% and 1% [Nae-Cherng, etal, 2016].Due to P. igniarius and P. linteus is the higher hard mushroom of degree of lignification, and the water content (15%) of two kinds of mushrooms is less, and fiber content is higher (6% to 8%) is higher than other edible mushroom contents.P. igniarius and P. linteus fructification contains the nitrogen-free of high-content Soluble matter.In general, the nitrogen-free soluble matter in edible mushroom is lower than 10%, and the nothing in P. igniarius and P. linteus Nitrogen solubles content > 67%.This observation indicate that, the nutritional ingredient in the carbohydrate of Phellinus mushroom composition is obviously not It is same as other common mushrooms.In a word, it has been found that P. igniarius has higher phenolic compound, flavonoids and polysaccharide Content and higher SOD sample activity.These results indicate that P. igniarius has more than P. linteus in food The development potentiality (Nae-Cherng, etal, 2016) of high antioxidant and immunoloregulation function.
About Phellinus, mainly polysaccharide, followed by flavones, terpene, sterol etc. are had now been found that, also contain amino acid, fall The multiple nutritional components such as leaf pine acid, jervine, agaricin acid.Contain various trace elements in Phellinus bacterium, there is iron, zinc, calcium, magnesium etc.. These elements are all substances needed by human or beneficial to human body.It is believed that Phellinus is mainly based on polysaccharide, but Phellinus ingredient Complexity, effect extensively, actually still have many active constituents to fail to be disclosed, for example, thinking that crude fibre is always in the past It cannot be by human consumption and absorption.It has been generally acknowledged that crude fibre does not have trophism to human body, or even overeats and also will affect Human body is unfavorable to body especially to the absorption of microelement to nutrient in food, is not taken seriously always.Hereafter, Ren Menfa It is existing, and recognize those " non-nutritive " substances that cannot be digested, it is but closely related with human health, and pre- Anti- human body certain diseases such as coronary heart disease, diabetes, colon cancer and constipation etc. play an important role, and at the same time, also recognize It has been not suitable for " crude fibre " word concept, thus has been discarded and be changed to dietary fiber.Phellinus contains volume fiber, therefore having must To carry out science processing to it and improve its bioavilability, especially whole development to utilize, rather than just with its polysaccharide or The preparation of the ingredients such as flavones terpene.The especially addition of Larch tree extract, the bioactivity and clinic for more enhancing Phellinus are answered With value.Larch is also the host of Phellinus (P.laricid), and the two symbiosis has been doomed them in Changbaishan area, heaven-made match Rare effect.The dihydroquercetin contained in larch is best one of natural.Dihydroquercetin because With antitumor, anti-oxidant, anti-radiation, antiviral, anti-disease of cardiovascular system, improve capillary microcirculation, improvement brain The effects of blood circulation, anti-platelet aggregation, for treating the diseases such as cerebral infarction and its sequelae, cerebral thrombosis, heart coronary artery, So being developed is the Related products such as food additives, health food and drug, there is very high potentiality to be exploited.
Resistant dextrin is a kind of Low Caloric Polydextrose being process by starch, belongs to low molecule water-soluble dietary fiber. As a kind of soluble food raw material low in calories, the vast potential for future development having in the food industry.Resistant dextrin can picture Granulated sugar or carbohydrate equally simply add, and will not influence the original flavor of food, so that it is strong to be applied to production food fiber Changing in the milk beverage of dairy products or supplement food fiber, since resistant dextrin and fat have similar mouthfeel, heat is low, can also As matched with flavor of dairy products maltodextrin low in calories appropriate carry out addition using, resistant dextrin so that resistant dextrin and The biological function of the enterals beneficial bacterium such as lactic acid bacteria, Bifidobacterium is more fully brought into play, to produce great phase Multiply effect prebiotics product to be characterized in: the drop of the increase of " beneficial bacteria " and/or the reduction of " harmful bacteria ", gut pH The variation of low, short chain fatty acids generations and bacterium enzyme concentration.Studies have shown that resistant dextrin is to show institute by colon fermentation There are these prebiotic functions.Resistant dextrin has excellent physiological function: resistant dextrin helps to maintain normal, healthy Blood glucose level and insulin level delay and inhibit digestion and absorption of the small intestine to carbohydrate, and improve distal tissues to insulin Sensitivity reduces the demand to insulin.Resistant dextrin can also change the secretion and the digested enzymatic activity of enteron aisle of intestinal hormone, Inhibit the digestion and absorption of carbohydrate, to play the role of reducing blood glucose;
It can reach reducing blood lipid, improve the effect of the lipid metabolism of various types hyperlipemia.Resistant dextrin small enteral not It is absorbed, large intestine can be directly entered, growth, the breeding of intestine beneficial bacteria colony can be promoted, while inhibiting harmful intestinal tract microorganism Growth and breeding;Resistant dextrin ferments in big enteral generates short chain fatty acids, produces acid and measures, these short chain rouge more compared with same dietary fiber Fat acid can prevent the growth and breeding of cancer cell.The water swelling of resistant dextrin can increase faecal volume, promote intestines peristalsis, right There is certain effect in constipation, hemorrhoid.
Diet functional component of the resistant dextrin as food, can be added in acidified milk or lactic acid drink, can not only mention Board fiber, and the biological function for the enterals beneficial bacterium such as can make lactic acid bacteria, Bifidobacterium fully plays, and generates great Multiplication effect can be used as diet food and constipation Crowded health protection food.
Arabic gum is a kind of natural plant, is derived from the tree of entitled Acacia a kind of, is Mimosaceae, Acacia, Acacia A. senegal (L.) Willd. and catechu A. catechu (L.f.) Willd. can extract Arabic gum It is condensed by the juice set.It can on bark self-assembling formation nodule, referred to as gummosis.
Arabic gum is a kind of carbohydrate polymer, can be in large intestine by Partial digestion.It can be supplemented for human body Cellulose, compared with starch and maltodextrin, energy value is less than half.More specifically, Arabic gum is Arabic half The mixture of lactose oligosaccharides, polysaccharide and protein sugar.D- galactolipin (Arabic tree according to source difference, in polysaccharide component Glue) and L- pectinose ratio it is also not identical.Compared with wattle, gum arabic contains more 4-O- methyl Ds- Glucuronic acid, and the amount of L- rhamnose and irreplaceable D-Glucose aldehydic acid is less.Resolvability with height is put down The colloid that normal glue class is only capable of at most adding during molten water about 5-8% reaches saturation, and the mixing ratio of Arabic gum and water It then may be up to 60%, can there is very high viscosity to show in high-content.Because it is water-base cement, therefore it will not be dissolved in oil and alcohol, If but alcohol content be lower than 15% when, can dissolve.In nutrition, Arabic gum does not generate heat substantially, is good water Soluble dietary fiber is used for health care product candy and beverage.
The present invention is characterized in that: due to using fresh Phellinus, drying course is saved, protects some of which physiology living Property substance such as SOD and some vitamin substances, such as vitamin C;Secondly, Phellinus through broken wall, is especially passed through at super-pressure It manages, by means such as shearing, friction, impact, extruding in homogenizing process, mechanical energy is applied to condensed state matters such as solid, liquid, It induces its structure and physicochemical properties to change, and induced chemical reaction, changes the more of macromolecular compound in Phellinus The structure of sugar, there are also the structures of Arabic gum and resistant dextrin, and make the small molecule compound in Phellinus, for example, flavonoids, polyphenol The ingredients such as class, terpene and sterols.The polysaccharide and Arabic gum in dihydroquercetin and Phellinus in Larch tree extract Embedding is formed by means such as shearing, friction, impact, extruding in homogenizing process with resistant dextrin, improves these small molecules Water solubility especially improves their bioavilability, enhances effect, thus reduces dosage, reduces side effect.
The features of the present invention: using 3 years raw fresh Phellinus fructifications, cleaning, fritter be made, water is added to mix, through broken wall, With Larch tree extract (90% or more element containing dihydroquercetin), Arabic gum, resistant dextrin mixing is placed in 150-250 megapascal It handles, is then placed in vacuum freeze drier in superhigh-voltage homogenizing machine, be freeze-dried, larch Phellinus powder is made.
Summary of the invention
The present invention provides the preparation methods of Phellinus composition, it is characterised in that: component in the Phellinus composition and Each component weight percent are as follows: fresh Phellinus fructification 85%, Larch tree extract (containing 90% or more dihydromyricetin) 3% are Arabic Glue 5%, resistant dextrin 7%;
Fallen leaves pine stump wood dust is broken into diameter 0.5mm-10mm little particle, and with hexamethylene static immersing 10-24h, filtering must be filtered Liquid, residue impregnates 10h with hexamethylene again, same to operate, and 2 filtrates are merged, solvent is recovered under reduced pressure, dries, obtains larch and mentions Take object;Phellinus and Larch tree extract, Arabic gum and resistant dextrin are collectively disposed to the superhigh-voltage homogenizing machine of 30-250 megapascal Middle processing, is then placed in vacuum freeze drier, is freeze-dried to get Phellinus composition.
The positive effect of the present invention is: due to using fresh Phellinus, saving high temperature drying course, protects therein one A little physiological activator such as SOD and some vitamin substances, such as vitamin C;Secondly, Phellinus is especially passed through through broken wall Super-high-pressure homogenization is handled, by means such as shearing, friction, impact, extruding in homogenizing process, to the condensed states object such as solid, liquid Matter applies mechanical energy, induces its structure and physicochemical properties to change, and induced chemical reaction, changes in Phellinus and divide greatly The structure of the polysaccharide of sub- compound, especially water-soluble polysaccharide molecule, there are also the structures of Arabic gum and resistant dextrin.Fallen leaves Polysaccharide in dihydroquercetin and Phellinus and Arabic gum and resistant dextrin in loose extract are in homogenizing process by cutting It the means such as cuts, rub, impacting, squeezing and forming embedding, improving these small molecule water dissolubilities, especially improving their biology benefit Expenditure enhances effect, thus reduces dosage, reduces side effect.
The positive effect of the present invention is: containing in the cooperation of Phellinus and Larch tree extract, especially Larch tree extract There is dihydroquercetin, hence it is evident that increase the antioxidation of Phellinus composition.
The present invention can be administered orally mode in the form of single or composition and be suitable for health or patient.
1 Phellinus composition antioxidation of experimental example
Experimental method
The preparation of 1.1 sample solutions
Example 4,5,6 and 7 Phellinus larch composition 1g respectively are extracted 1 hour with 10 times of 70% alcohol refluxs of amount, are extracted Liquid centrifugal filtration is concentrated certain volume, adds second alcohol and water that solution ethanol concentration is made to reach 70%, be settled in 50ml volumetric flask, supplies Examination.
1.2 Phellinus compositions act on DPPH radicals scavenging
The experiment of DPPH radicals scavenging effect is most common, because it is simple with antioxidant, directly, is rapidly reacted. It weighs 0.0128 g of DPPH and is dissolved in it surely in 50 mL volumetric flasks with dehydrated alcohol, 10mL solution is then taken to be dissolved in 50 mL surely It in volumetric flask, is protected from light, ultimate density is 1.3 × 10-4 mol/L。
With reference to the method for Luo etc., and make it is suitably modified, 96 orifice plates be used to quickly measurement sample absorbance value.It inhales respectively Take 80 μ L of sample and positive reference substance prepare liquid, be added 80 μ L of DPPH solution, at 37 DEG C it is dark stand 30 minutes after, with nothing Water-ethanol zeroing, measure 517nm wavelength at absorbance (ASample), each sample is measured in parallel 3 times;Take sample prepare liquid 80 μ L and 70% ethyl alcohol, 80 μ L mixed liquor at 517nm absorbance (A 1 ), then measure 80 μ LDPPH solution and 80 μ L70% ethyl alcohol At 517nm wavelength absorbance (A 0 ).DPPH clearance rate is calculated by following formula.
DPPH clearance rate/%=(1-)× 100
As a result see embodiment 4-7.
Embodiment 1
3 years fresh Phellinus fructification 100g of life are cleaned, fritter are made, adds water, is placed in wall-breaking machine, under the conditions of 4 °C, broken wall 3 minutes, Phellinus aqueous suspension liquid is obtained, is handled with high pressure homogenizer, then use superhigh-voltage homogenizing machine, the processing of 200 megapascal obtains Phellinus Water slurry, spray drying, obtains Phellinus xeraphium.
Embodiment 2
Fallen leaves pine stump wood dust is broken into diameter 0.5mm-5mm particle, and with hexamethylene static immersing 14h, filtering obtains filtrate, residue 10h is impregnated with hexamethylene again, it is same to operate, 2 filtrates are merged, solvent is recovered under reduced pressure, dries, obtains Larch tree extract 1(bis- Hydrogen quercetin content 49%), hot water is added, removes water-insoluble impurity while hot, is concentrated into certain volume, it is cooling, it is placed at room temperature for, Crystallization is collected in filtering, is re-dissolved in water, is repeated 3 times to get Larch tree extract 2(dihydroquercetin content >=90%).
Embodiment 3
The phellinus linteus extract dry powder 85g of Example 1, add embodiment 2 Larch tree extract (dihydroquercetin content >= 90%) 3g, Arabic gum 5g, resistant dextrin 7g add water 1000ml, are placed in common homogenizer, mix, and Phellinus composition is made, Wherein dihydroquercetin solubility in the suspension reaches 1.29g.
Embodiment 4
The phellinus linteus extract dry powder 85g of Example 1, add embodiment 2 Larch tree extract (dihydroquercetin content >= 90%) 3g, Arabic gum 5g, resistant dextrin 7g add appropriate amount of water, are placed in common homogenizer, mix, are placed in the high pressure of 50 megapascal It mixes, is then placed in vacuum freeze drier in homogenizer, be freeze-dried, larch Phellinus powder is made.Powder 10g is taken to add water 100ml, wherein dihydroquercetin solubility reaches 3.38g/L, to DPPH radicals scavenging exercising result: clearance rate is 88.51%。
Embodiment 5
The phellinus linteus extract dry powder 85g of Example 1, add embodiment 2 Larch tree extract (dihydroquercetin content >= 90%) 3g, Arabic gum 5g, resistant dextrin 7g add appropriate amount of water, are placed in common homogenizer, mix, are placed in the high pressure of 100 megapascal It mixes, is then placed in vacuum freeze drier in homogenizer, be freeze-dried, larch Phellinus powder is made.Powder 10g is taken to add water 100ml, wherein dihydroquercetin solubility reaches 4.10g/L, and to DPPH radicals scavenging exercising result, clearance rate is 90.68%。
Embodiment 6
The phellinus linteus extract dry powder 85g of Example 1, add embodiment 2 Larch tree extract (dihydroquercetin content >= 90%) 3g, Arabic gum 5g, resistant dextrin 7g add appropriate amount of water, are placed in common homogenizer, mix, are placed in the high pressure of 150 megapascal It mixes, is then placed in vacuum freeze drier in homogenizer, be freeze-dried, larch Phellinus powder is made.Powder 10g is taken to add water 100ml, wherein dihydroquercetin solubility reaches 5.64g/L, and to DPPH radicals scavenging exercising result, clearance rate is 92.71%。
Embodiment 7
The phellinus linteus extract dry powder 85g of Example 1, add embodiment 2 Larch tree extract (dihydroquercetin content >= 90%) 3g, Arabic gum 5g, resistant dextrin 7g add appropriate amount of water, are placed in common homogenizer, mix, are placed in the high pressure of 250 megapascal It mixes, is then placed in vacuum freeze drier in homogenizer, be freeze-dried, larch Phellinus powder is made.Powder 10g is taken to add water 100ml, wherein dihydroquercetin solubility reaches 5.11g/L, is 91.25% to DPPH radicals scavenging exercising result clearance rate.
Embodiment 8
It takes the dihydroquercetin extract of unprocessed mistake and is rich in dihydro Mongolian oak through what the invention patent claim 5 was prepared The Larch tree extract of Pi Su carries out soluble test, the results show that untreated dihydroquercetin is in water after solution saturation Middle biological solubility is 0.45g/L, and through the invention patent treated product, the highest solubility of dihydroquercetin is 5.11g/ L。

Claims (6)

1. a kind of Phellinus composition, it is characterised in that: component and each component weight percent in the Phellinus composition are as follows: fresh Phellinus fructification 60-85%, Larch tree extract 3-20% contain 90% or more dihydroquercetin, Arabic gum in Larch tree extract 5-20%, resistant dextrin 7-15%.
2. the Phellinus composition according to claim 1, wherein the water content of fresh Phellinus is 15-40%.
3. the Phellinus composition according to claim 1, it is characterised in that: wherein fresh Phellinus the preparation method is as follows: 3 years Raw fresh Phellinus fructification 100g, cleans, fritter is made, adds water, is placed in wall-breaking machine, under the conditions of 4 °C, broken wall 3 minutes, obtains Suspension high pressure homogenizer is handled 20 minutes, ultra high pressure extraction equipment is then used, at 200 megapascal by fresh Phellinus water slurry Reason 20 minutes obtains Phellinus water slurry, freeze-drying or spray drying, obtains Phellinus xeraphium.
4. the Phellinus composition according to claim 1, the wherein preparation method of Larch tree extract, it is characterised in that: fall Leaf pine stump sawdust is ground into diameter 0.5mm-5mm particle, and with hexamethylene static immersing 14h, filtering obtains filtrate, residue uses ring again Hexane impregnates 10h, same to operate, and 2 filtrates are merged, solvent is recovered under reduced pressure, dries, and obtains larch and slightly takes object, hot water is added, Water-insoluble impurity is removed while hot, is concentrated into certain volume, it is cooling, it is placed at room temperature for, crystallization is collected in filtering, is re-dissolved in water, repeatedly 3 times are carried out to get dihydroquercetin content >=90% in Larch tree extract wherein Larch tree extract.
5. the resulting Phellinus powder of preparation method according to claim 3, it is characterised in that Phellinus dried powder 85g is added as weighed Benefit requires 4 gained Larch tree extract 3-20g and Arabic gum 5-15g, resistant dextrin 7-15g to add appropriate amount of water, is placed in common It in homogenizer, mixes, obtains Phellinus composition aqueous suspension, suspension is placed in superhigh-voltage homogenizing machine, pressure is 200-800 million Pa is handled 2-5 times, is taken out whole liquid and is put into vacuum freeze drier, is freeze-dried, Phellinus composition powder is made.
6. preparing Phellinus composition powder according to claim 5, it is characterised in that wherein solubility increases dihydroquercetin in water 5-10 times.
CN201811317389.7A 2018-11-07 2018-11-07 A kind of preparation method of Phellinus composition and the application in terms of medical treatment Pending CN109432141A (en)

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Application publication date: 20190308