CN113318187A - Product for activating immune phagocyte and promoting arteriosclerosis plaque ablation, and preparation method and application thereof - Google Patents
Product for activating immune phagocyte and promoting arteriosclerosis plaque ablation, and preparation method and application thereof Download PDFInfo
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- CN113318187A CN113318187A CN202110500395.1A CN202110500395A CN113318187A CN 113318187 A CN113318187 A CN 113318187A CN 202110500395 A CN202110500395 A CN 202110500395A CN 113318187 A CN113318187 A CN 113318187A
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- 238000002679 ablation Methods 0.000 title claims abstract description 33
- 230000001737 promoting effect Effects 0.000 title claims abstract description 32
- 230000003213 activating effect Effects 0.000 title claims abstract description 30
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- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/06—Fungi, e.g. yeasts
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- A23L31/00—Edible extracts or preparations of fungi; Preparation or treatment thereof
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- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/33—Heterocyclic compounds
- A61K31/335—Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin
- A61K31/35—Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin having six-membered rings with one oxygen as the only ring hetero atom
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Abstract
The invention provides a product for activating immune phagocyte and promoting arteriosclerosis plaque ablation, which comprises cordyceps militaris powder, ginseng powder, rhizoma polygonati powder, cistanche tubulosa powder, grifola frondosa powder, poria cocos powder and epigallocatechin gallate powder, wherein the weight ratio of the components is 1-5: 1-5: 1-10: 1-5: 1-5: 1-5: 1-5, the seven medicinal and edible components are scientifically matched according to the dispensing principle of Chinese traditional medicine monarch, minister, assistant and guide, can repair arterial blood vessel granulocytes, prevent cholesterol from depositing in the arterial blood vessel wall, activate immune phagocytic cells, enhance the phagocytic activity of the immune phagocytic cells to phagocytize plaque components in the hardened arterial wall, promote the remodeling of the hardened arterial wall structure, ablate the plaque in the arterial wall, and restore the elasticity of the blood vessel wall.
Description
Technical Field
The invention relates to the technical field of biological products, in particular to a product for activating immune phagocyte and promoting the ablation of arteriosclerosis plaques, and a preparation method and application thereof.
Background
Arteriosclerotic plaques can grow in arteries throughout the body, and have the causes of hypertension, hyperglycemia, hyperlipidemia, homocysteine, high blood toxicity, high pressure and the like, which can damage the skin of blood vessels, resulting in the formation of arteriosclerotic plaques. Arteriosclerotic plaques can be classified according to their properties: lipid plaques, fibrous plaques, calcified plaques, mixed plaques. At present, the treatment aiming at the arteriosclerosis plaque only stays in the treatment of relieving symptoms by western medicines and traditional Chinese medicines of reducing blood fat, reducing blood viscosity, resisting blood coagulation, expanding arterial smooth muscle and the like, the blood flow is kept smooth, and when the plaque is too large and blocks a blood vessel to cause ischemia, an operation method such as an arterial stent, coronary bypass and the like is used for recovering the blood flow. All of these treatments are directed to maintaining blood flow, merely relieving ischemic symptoms, and not to therapeutic agents that promote plaque ablation in the plaque itself, restoring the natural smooth full elastic state of the arterial wall.
The traditional Chinese medicine and western medicine, health food and functional food in the prior art can only relieve vasospasm and poor blood flow, and no medicine or food capable of promoting arteriosclerosis ablation and promoting vascular transformation exists.
The Chinese patent application with the publication number of CN111773355A discloses a traditional Chinese medicine formula which is composed of the following medicinal materials in parts by weight: 3-9 parts of dragon's blood, 9-20 parts of ligusticum wallichii, 10-20 parts of radix pseudostellariae, 3-6 parts of rhizoma sparganii and 3-6 parts of curcuma zedoary. Soaking the other medicinal materials except for the dragon blood according to the required weight parts, decocting the medicinal materials with strong fire and then slow fire, concentrating the decoction into fluid extract, and preparing the fluid extract and the dragon blood raw powder into corresponding dosage forms for three times a day. The invention has simple compatibility and composition and wide medicine source; the efficacy is clear, and the arteriosclerosis plaque can be obviously reduced. Although the invention has simple compatibility and composition, the preparation process of the traditional Chinese medicine is complex and the curative effect is unstable.
Disclosure of Invention
In order to solve the problems in the prior art, the invention utilizes medicinal and edible Chinese herbal medicines to form a compound product through scientific combination, and the compound product can repair arterial vessel granulocytes, prevent cholesterol from depositing in the arterial vessel wall, activate immune phagocytic cells, enhance the phagocytic activity of the immune phagocytic cells to phagocytize plaque components in a hardened arterial wall, promote the remodeling of the hardened arterial wall structure, ablate the plaque in the arterial wall and restore the elasticity of the vessel wall.
The invention provides a product for activating immune phagocyte and promoting arteriosclerosis plaque ablation, which comprises cordyceps militaris powder, ginseng powder, rhizoma polygonati powder, cistanche tubulosa powder, grifola frondosa powder, poria cocos powder and epigallocatechin gallate powder, wherein the weight ratio of the components is 1-5: 1-5: 1-10: 1-5: 1-5: 1-5: 1-5, the seven medicinal and edible components are matched according to the dispensing principle of Chinese traditional medicine monarch, minister, assistant and guide.
Preferably, the feed comprises cordyceps militaris powder, ginseng powder, yellow fine powder, cistanche tubulosa powder, grifola frondosa powder, poria cocos powder and epigallocatechin gallate powder, wherein the weight ratio of each component is 1-4: 1-4: 1-8: 1-4: 1-4: 1-4: 1-4.
The preferable one of the schemes comprises cordyceps militaris powder, ginseng powder, rhizoma polygonati powder, cistanche tubulosa powder, ash tree pollen, tuckahoe powder and epigallocatechin gallate powder, wherein the weight ratio of each component is 1-3: 1-3: 1-7: 1-3: 2-4: 2-4: 1-4.
The preferable one of the schemes comprises cordyceps militaris powder, ginseng powder, rhizoma polygonati powder, cistanche tubulosa powder, ash tree pollen, tuckahoe powder and epigallocatechin gallate powder, wherein the weight ratio of each component is 1-2: 2-3: 2-6: 1-3: 3-4: 3-4: 2-3.
The preferable selection of any scheme comprises cordyceps militaris powder, ginseng powder, rhizoma polygonati powder, cistanche tubulosa powder, ash tree pollen, poria cocos powder and epigallocatechin gallate powder, wherein the weight ratio of each component is 2: 3: 5: 2: 4: 4: 3.
the invention also provides a preparation method of the product for activating immune phagocyte and promoting the ablation of the arteriosclerotic plaque, which comprises the following steps:
the method comprises the following steps: carrying out ultraviolet disinfection on a mixing chamber and related equipment for 2 hours;
step two: accurately weighing various raw materials according to a product formula, and uniformly mixing in a mixer;
step three: spraying purified water according to the weight ratio of 30-40% to moisten the raw materials;
step four: slowly adding the raw materials sprayed with the purified water into an extrusion granulator for granulation;
step five: kneading and sieving the prepared granules to form uniform small granules;
step six: placing the screened uniform particles in an oven for drying, detecting after the drying, and collecting qualified particles;
step seven: sieving again after drying to keep uniformity of the granules, barreling, sterilizing by irradiation, detecting microorganism, subpackaging and packaging after being qualified.
In any of the above embodiments, the mixing time in the mixer is preferably 35 minutes.
In any of the above embodiments, the sieve mesh number is preferably: 10 meshes.
Preferably, in any of the above schemes, the drying conditions are as follows: baking at 70 deg.C for 10 hr.
The invention also provides a beverage prepared from the product for activating the immune phagocyte and promoting the ablation of the arteriosclerotic plaque.
The invention also provides a food prepared from the product for activating the immune phagocyte and promoting the ablation of the arteriosclerotic plaque.
Cordyceps militaris powder: cordyceps polysaccharide in Cordyceps militaris powder can activate the activity of immune phagocyte of organism, remarkably improve phagocytic function of immune phagocyte, promote immune phagocyte to phagocytose plaque ingredient abnormally deposited in arterial blood vessel, and promote artery wall softening; cordycepic acid in Cordyceps militaris can remove free radicals of human body, obviously antagonize tissue homogenate to generate lipid peroxide, remarkably increase cell energy charge value, lower blood pressure, dilate cardiovascular and cerebrovascular vessels, regulate blood viscosity, and inhibit lipid deposition on vessel wall.
Ginseng powder: the panaxatriol saponins in Ginseng radix can exert endothelium-dominated vasodilation effect by increasing NO amount released from endothelial cells, and the panaxatriol saponins can increase cyclooxygenase gene expression of vascular wall cells, and has arteriosclerosis resisting effect.
Fine yellow powder: the polygonatum polysaccharide in the polygonatum can improve the macrophage function, reduce foam cells in arteriosclerosis plaques, promote the reduction of arteriosclerosis plaques and promote the ablation of arteriosclerosis plaques.
Cistanche tubulosa powder: the cistanche polysaccharide in cistanche can obviously improve the phagocytic and secretory functions of macrophages, so that the macrophages are activated, the macrophages are promoted to phagocytose arteriosclerosis plaques, and the remodeling of arterial wall structures is promoted.
Ash tree pollen: the grifolan in the grifola frondosa can obviously increase the phagocytosis percentage and the phagocytosis index of macrophages, enhance the phagocytosis function of the macrophages and promote the phagocytosis of immune phagocytes on arteriosclerosis plaques.
Poria cocos powder: pachyman in Poria can obviously enhance phagocytic function of macrophage, and promote phagocytosis of arteriosclerosis plaque by immune phagocyte
Epigallocatechin gallate powder: the gallocatechin gallate can inhibit cholesterol absorption, promote cholesterol excretion from intestinal tract, reduce total cholesterol and low density lipoprotein in blood, and increase high density lipoprotein in blood, so as to promote cholesterol in arterial plaque to dissolve out from plaque, and gradually reduce plaque.
Compared with the prior art, the product for activating immune phagocyte and promoting arteriosclerosis plaque ablation comprises cordyceps militaris powder, ginseng powder, rhizoma polygonati powder, cistanche tubulosa powder, grifola frondosa powder, poria cocos powder and epigallocatechin gallate powder, wherein the weight ratio of the components is 1-5: 1-5: 1-10: 1-5: 1-5: 1-5: 1-5. The seven components are medicinal and edible components, are scientifically matched according to the dispensing principle of Chinese traditional medicine, namely monarch, minister, assistant and guide, can repair arterial blood vessel granulocytes, prevent cholesterol from depositing in the arterial blood vessel wall, activate immune phagocytic cells, enhance phagocytic activity of the immune phagocytic cells to phagocytize plaque components in a hardened arterial wall, promote the structure of the hardened arterial wall to be remolded, ablate plaque in the arterial wall and restore the elasticity of the blood vessel wall.
Detailed Description
In order that the present invention may be more clearly understood, the following description and the accompanying drawings are provided for illustrative purposes.
Example 1
A product for activating immune phagocyte and promoting arteriosclerosis plaque ablation is composed of cordyceps militaris powder, ginseng powder, rhizoma polygonati powder, cistanche tubulosa powder, grifola frondosa powder, poria cocos powder and epigallocatechin gallate powder, wherein the weight ratio of each component is 5: 5: 9: 5: 5: 5: and 5, the seven medicinal and edible components are matched according to the dispensing principle of Chinese traditional medicine monarch, minister, assistant and guide.
The preparation method comprises the following steps:
the method comprises the following steps: carrying out ultraviolet disinfection on a mixing chamber and related equipment for 2 hours;
step two: accurately weighing various raw materials according to the formula, and uniformly mixing in a mixer for 35 minutes;
step three: spraying purified water according to the weight ratio of 30-40% to moisten the raw materials;
step four: slowly adding the raw materials sprayed with the purified water into an extrusion granulator for granulation;
step five: kneading the prepared granules, and sieving the granules by a sieve with 10 meshes to form uniform small granules;
step six: placing the screened uniform particles in a drying oven, setting the temperature of 70 ℃ for drying for 10 hours, detecting after the drying is finished, and collecting qualified particles;
step seven: sieving again after drying to keep uniformity of the granules, barreling, sterilizing by irradiation, detecting microorganism, subpackaging and packaging after being qualified.
The granules prepared by the preparation method are bagged and supplied to patients with plaques in the arteries of the head and neck, the coronary arteries or the arteries of the limbs.
Example 2
A product for activating immune phagocyte and promoting arteriosclerosis plaque ablation is composed of cordyceps militaris powder, ginseng powder, rhizoma polygonati powder, cistanche tubulosa powder, grifola frondosa powder, poria cocos powder and epigallocatechin gallate powder, wherein the weight ratio of each component is 4: 5: 9: 4: 4: 3: 3, the seven medicinal and edible components are matched according to the dispensing principle of Chinese traditional medicine monarch, minister, assistant and guide.
The specific preparation method is shown in example 1.
Example 3
A product for activating immune phagocyte and promoting arteriosclerosis plaque ablation is composed of cordyceps militaris powder, ginseng powder, rhizoma polygonati powder, cistanche tubulosa powder, grifola frondosa powder, poria cocos powder and epigallocatechin gallate powder, wherein the weight ratio of each component is 3: 5: 8: 3: 3: 3: 3, the seven medicinal and edible components are matched according to the dispensing principle of Chinese traditional medicine monarch, minister, assistant and guide.
The specific preparation method is shown in example 1.
Example 4
A product for activating immune phagocyte and promoting arteriosclerosis plaque ablation is composed of cordyceps militaris powder, ginseng powder, rhizoma polygonati powder, cistanche tubulosa powder, grifola frondosa powder, poria cocos powder and epigallocatechin gallate powder, wherein the weight ratio of each component is 2: 3: 7: 2: 3: 3: 3, the seven medicinal and edible components are matched according to the dispensing principle of Chinese traditional medicine monarch, minister, assistant and guide.
The specific preparation method is shown in example 1.
Example 5
A product for activating immune phagocyte and promoting arteriosclerosis plaque ablation is composed of cordyceps militaris powder, ginseng powder, rhizoma polygonati powder, cistanche tubulosa powder, grifola frondosa powder, poria cocos powder and epigallocatechin gallate powder, wherein the weight ratio of each component is 2: 3: 5: 2: 4: 4: 3, the seven medicinal and edible components are matched according to the dispensing principle of Chinese traditional medicine monarch, minister, assistant and guide.
The specific preparation method is shown in example 1.
Example 6
A product for activating immune phagocyte and promoting arteriosclerosis plaque ablation is prepared from cordyceps militaris powder, ginseng powder, rhizoma polygonati powder, cistanche tubulosa powder, grifola frondosa powder, poria cocos powder and epigallocatechin gallate powder, wherein the weight ratio of each component is 1: 2: 3: 2: 3: 3: 3, the seven medicinal and edible components are matched according to the dispensing principle of Chinese traditional medicine monarch, minister, assistant and guide.
The specific preparation method is shown in example 1.
Example 7
A product for activating immune phagocyte and promoting arteriosclerosis plaque ablation is prepared from cordyceps militaris powder, ginseng powder, rhizoma polygonati powder, cistanche tubulosa powder, grifola frondosa powder, poria cocos powder and epigallocatechin gallate powder, wherein the weight ratio of each component is 1: 2: 2: 2: 1: 1: 1, the seven medicinal and edible components are matched according to the dispensing principle of Chinese traditional medicine monarch, minister, assistant and guide.
The specific preparation method is shown in example 1.
Comparative example 1
A product for activating immune phagocyte and promoting arteriosclerosis plaque ablation is composed of cordyceps militaris powder, ginseng powder, rhizoma polygonati powder, cistanche tubulosa powder, ash tree pollen and poria cocos powder, wherein the weight ratio of each component is 2: 3: 5: 2: 4: 4.
the specific preparation method is shown in example 1.
Comparative example 2
A product for activating immune phagocyte and promoting arteriosclerosis plaque ablation is composed of Cordyceps militaris powder, Ginseng radix powder, rhizoma Polygonati powder, Cistanchis herba powder, Grifola Frondosa powder, and epigallocatechin gallate powder, wherein the weight ratio of each component is 2: 3: 5: 2: 4: 3, the seven medicinal and edible components are matched according to the dispensing principle of Chinese traditional medicine monarch, minister, assistant and guide.
The specific preparation method is shown in example 1.
Comparative example 3
A product for activating immune phagocyte and promoting arteriosclerosis plaque ablation is prepared from Cordyceps militaris powder, Ginseng radix powder, rhizoma Polygonati powder, Cistanchis herba powder, Poria powder, and epigallocatechin gallate powder, wherein the weight ratio of each component is 2: 3: 5: 2: 4: 3.
the specific preparation method is shown in example 1.
Comparative example 4
A product for activating immune phagocyte and promoting arteriosclerosis plaque ablation is prepared from ginseng powder, rhizoma polygonati powder, cistanche tubulosa powder, grifola frondosa powder, poria cocos powder and epigallocatechin gallate powder, wherein the weight ratio of the components is 3: 5: 2: 4: 4: 3.
the specific preparation method is shown in example 1.
Comparative example 5
A product for activating immune phagocyte and promoting arteriosclerosis plaque ablation is composed of Cordyceps militaris powder, rhizoma Polygonati powder, cistanche tubulosa powder, Grifola frondosa powder, Poria cocos powder and epigallocatechin gallate powder, wherein the weight ratio of each component is 2: 5: 2: 4: 4: 3.
the specific preparation method is shown in example 1.
Comparative example 6
A product for activating immune phagocyte and promoting arteriosclerosis plaque ablation is prepared from Cordyceps militaris powder, Ginseng radix powder, Cistanchis herba powder, Grifola Frondosa powder, Poria powder, and epigallocatechin gallate powder, wherein the weight ratio of each component is 2: 3: 2: 4: 4: 3, the seven medicinal and edible components are matched according to the dispensing principle of Chinese traditional medicine monarch, minister, assistant and guide.
Comparative example 7
A product for activating immune phagocyte and promoting arteriosclerosis plaque ablation is prepared from cordyceps militaris powder, ginseng powder, rhizoma polygonati powder, cistanche tubulosa powder and ash tree pollen in a weight ratio of 2: 3: 5: 2: 4, the seven medicinal and edible components are matched according to the dispensing principle of Chinese traditional medicine monarch, minister, assistant and guide.
The specific preparation method is shown in example 1.
Comparative example 8
A product for activating immune phagocyte and promoting arteriosclerosis plaque ablation is prepared from cordyceps militaris powder, ginseng powder, rhizoma polygonati powder and cistanche tubulosa powder in a weight ratio of 2: 3: 5: 2, the seven medicinal and edible components are matched according to the dispensing principle of Chinese traditional medicine monarch, minister, assistant and guide.
The specific preparation method is shown in example 1.
Comparative example 9
A product for activating immune phagocyte and promoting arteriosclerosis plaque ablation is prepared from ginseng powder, rhizoma polygonati powder and cistanche tubulosa powder in a weight ratio of 3: 5: 2, the seven medicinal and edible components are matched according to the dispensing principle of Chinese traditional medicine monarch, minister, assistant and guide.
The specific preparation method is shown in example 1.
Comparative example 10
A product for activating immune phagocyte and promoting arteriosclerosis plaque ablation is prepared from cordyceps militaris powder, rhizoma polygonati powder and cistanche tubulosa powder in a weight ratio of 2: 5: 2, the seven medicinal and edible components are matched according to the dispensing principle of Chinese traditional medicine monarch, minister, assistant and guide.
The specific preparation method is shown in example 1.
The results of the efficacy test of example 5 are shown below, as the results of the efficacy comparison of example 5 show the best results.
And (3) curative effect test:
the method comprises the steps of selecting 35 patients with coronary heart diseases meeting diagnosis standards, carrying out contrast examination or coronary artery CTA examination on the coronary arteries of all the patients, displaying that 3-5 lipid plaques exist in the coronary artery wall of each patient, carrying out stent interventional operation treatment on more than 75% of plaques, carrying out minimum 25% and maximum 65% of the remaining plaques, adopting case-by-case contrast treatment, orally taking two bags of the product of the embodiment 5 of the invention by the patients in the morning and the evening, wherein each bag contains 2 g of the product of the invention, and 6 months is a treatment course.
As a result: the effective rate is 100 percent, namely, the lipid plaque in the coronary artery wall of all patients is reduced; the plaque is reduced by more than 25%, namely the minimum plaque reduction degree is 25%, and the maximum plaque reduction degree is 50%.
Selecting 50 patients with carotid plaques, wherein all patients are subjected to carotid color ultrasound examination, and the carotid plaques of all patients are more than 1, the carotid plaques of the patients are at least 1, the carotid plaques of the patients are 5, the carotid plaques of 40 patients are less than 25%, one of the carotid plaques of 9 patients is 25-50%, and 1 of the carotid plaques of 1 patient is 50-75%. The medicine is treated by adopting the control before and after the case, two bags of the product are orally taken in the morning and at night, each bag contains 2 g of the product, and 6 months are a course of treatment.
As a result: 100% effective, 40 carotid plaques less than 25% of patients all disappeared, and the largest plaque among the other 10 patients decreased by more than 20%.
It should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. A product for activating immune phagocyte and promoting arteriosclerosis plaque ablation comprises cordyceps militaris powder, ginseng powder, rhizoma polygonati powder, cistanche tubulosa powder, grifola frondosa powder, poria cocos powder and epigallocatechin gallate powder, wherein the weight ratio of each component is 1-5: 1-5: 1-10: 1-5: 1-5: 1-5: 1-5.
2. The product of claim 1, comprising cordyceps militaris powder, ginseng powder, rhizoma polygonati powder, cistanche tubulosa powder, grifola frondosa powder, poria cocos powder and epigallocatechin gallate powder, wherein the weight ratio of the components is 1-4: 1-4: 1-8: 1-4: 1-4: 1-4: 1-4.
3. The product of claim 1, comprising cordyceps militaris powder, ginseng powder, rhizoma polygonati powder, cistanche tubulosa powder, grifola frondosa powder, poria cocos powder and epigallocatechin gallate powder, wherein the weight ratio of the components is 1-3: 1-3: 1-7: 1-3: 2-4: 2-4: 1-4.
4. The product of claim 1, comprising cordyceps militaris powder, ginseng powder, rhizoma polygonati powder, cistanche tubulosa powder, grifola frondosa powder, poria cocos powder and epigallocatechin gallate powder, wherein the weight ratio of the components is 1-2: 2-3: 2-6: 1-3: 3-4: 3-4: 2-3.
5. The product of claim 1, comprising cordyceps militaris powder, ginseng powder, rhizoma polygonati powder, cistanche tubulosa powder, grifola frondosa powder, poria cocos powder and epigallocatechin gallate powder, wherein the weight ratio of each component is 2: 3: 5: 2: 4: 4: 3.
6. a beverage made of the preparation for activating immune phagocyte and promoting ablation of arteriosclerotic plaque according to any one of claims 1 to 5.
7. A food product comprising the preparation for activating immunophagocytic cells and promoting ablation of arteriosclerotic plaque according to any one of claims 1 to 5.
8. A preparation method of a preparation for activating immune phagocyte and promoting the ablation of arteriosclerotic plaque comprises the following steps:
the method comprises the following steps: carrying out ultraviolet disinfection on a mixing chamber and related equipment for 2 hours;
step two: accurately weighing the raw materials according to the formula of the product, and uniformly mixing in a mixer;
step three: spraying purified water according to the weight ratio of 30-40% to moisten the raw materials;
step four: slowly adding the raw materials sprayed with the purified water into an extrusion granulator for granulation;
step five: kneading and sieving the prepared granules to form uniform small granules;
step six: placing the screened uniform particles in an oven for drying, detecting after the drying, and collecting qualified particles;
step seven: sieving again after drying to keep uniformity of the granules, barreling, sterilizing by irradiation, detecting microorganism, subpackaging and packaging after being qualified.
9. The method of claim 8, wherein the mixing time in the mixer of step two is 35 minutes.
10. The method for preparing the preparation of claim 9, wherein the mesh number of the five-mesh screen is 10 meshes; the drying conditions in the sixth step are as follows: baking at 70 deg.C for 10 hr.
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