CN115104609A - Oligosaccharins plant sterilization synergistic composition and preparation method thereof - Google Patents

Oligosaccharins plant sterilization synergistic composition and preparation method thereof Download PDF

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CN115104609A
CN115104609A CN202110979848.3A CN202110979848A CN115104609A CN 115104609 A CN115104609 A CN 115104609A CN 202110979848 A CN202110979848 A CN 202110979848A CN 115104609 A CN115104609 A CN 115104609A
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active ingredient
wetting agent
composition
synergistic composition
fatty acid
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CN115104609B (en
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郭元乾
王晓青
张超楠
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Ruyang Ziqiang Biotechnology Co ltd
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Ruyang Ziqiang Biotechnology Co ltd
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    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N43/00Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/02Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms
    • A01N43/04Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom
    • A01N43/14Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom six-membered rings
    • A01N43/16Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom six-membered rings with oxygen as the ring hetero atom
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N25/00Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/12Powders or granules
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N47/00Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
    • A01N47/08Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having one or more single bonds to nitrogen atoms
    • A01N47/10Carbamic acid derivatives, i.e. containing the group —O—CO—N<; Thio analogues thereof
    • A01N47/18Carbamic acid derivatives, i.e. containing the group —O—CO—N<; Thio analogues thereof containing a —O—CO—N< group, or a thio analogue thereof, directly attached to a heterocyclic or cycloaliphatic ring

Abstract

The invention relates to A01N, in particular to an oligosaccharins plant sterilization synergistic composition and a preparation method thereof. The preparation raw materials of the composition comprise active ingredients and auxiliaries, wherein the active ingredients comprise a first active ingredient and a second active ingredient; the first active ingredient is amino-oligosaccharin; the second active ingredient is at least one of zhongshengmycin and kasugamycin. The present invention is achieved by using amino-oligosaccharins; and at least one of zhongshengmycin and kasugamycin is used as an active ingredient, so that the sterilization effect can be promoted, the sterilization spectrum is expanded, the addition of a carrier ingredient and a wetting agent and an oil agent in an auxiliary agent is controlled, the heat storage stability of the active ingredient is promoted, and the granules with low moisture absorption and good fluidity are obtained.

Description

Oligosaccharide plant sterilization synergistic composition and preparation method thereof
Technical Field
The invention relates to A01N, in particular to an oligosaccharins plant sterilization synergistic composition and a preparation method thereof.
Background
The amino-oligosaccharin is oligosaccharide with glucosamine as a unit, and can be used as an efficient bactericidal component in various plants through the effects of promoting cell activation in crops such as fruits, vegetables and rice, inhibiting plant pathogenic bacteria and the like.
CN109221131A provides an aqueous solution containing amino-oligosaccharin and kasugamycin, which comprises amino-oligosaccharin, GENAPOL X150, polyoxyethylene castor oil, lauramidopropyl betaine, and water. Can be used for preventing and treating crop diseases.
Because the amino-oligosaccharin is water-soluble, generally prepared into a water aqua and difficult to be used for preparing granules and the like, and a single active ingredient is easy to cause drug resistance and influence the applicability of the amino-oligosaccharin, a new composition is required to be provided for synergy and promotion of sterilization.
Disclosure of Invention
In order to solve the problems, the invention provides a plant sterilization synergistic composition of oligosaccharins in a first aspect, which is prepared from raw materials comprising active ingredients and auxiliaries, wherein the active ingredients comprise a first active ingredient and a second active ingredient; the first active ingredient is amino-oligosaccharin; the second active ingredient is at least one of zhongshengmycin and kasugamycin.
The present invention is not particularly limited to the weight ratio of the first active ingredient to the second active ingredient, and there may be mentioned, for example, 1: (0.01 to 100) such as 1: 1. 2: 1. 1: 2.
as a preferable technical scheme, the active ingredients account for 0.5-20 wt% of the composition.
In a preferred embodiment of the present invention, the auxiliary agent is selected from one or more of a carrier, an oil agent, a wetting agent, a fatty acid salt, a stabilizer, a spreader, and a binder.
As a preferable technical scheme, the carrier comprises one or more of starch, sepiolite, trehalose, potassium chloride, urea, magnesium aluminum silicate, attapulgite and kaolin, and accounts for 50-90 wt% of the composition.
According to a preferable technical scheme of the invention, the fatty acid salt accounts for 10-20 wt% of the active ingredient, and is selected from one or more of calcium stearate, magnesium stearate, calcium palmitate and magnesium palmitate.
As a preferable technical scheme, the wetting agent accounts for 0.5-15 wt% of the composition.
In a preferred embodiment of the present invention, the wetting agent comprises an anionic wetting agent.
As a preferred technical solution of the present invention, the anionic wetting agent is selected from one or more of sodium dodecyl sulfonate, calcium dodecyl benzene sulfonate, sodium dodecyl sulfate, lignosulfonate, alkyl ethyl sulfonate, fatty alcohol sulfate, and sodium dodecyl diphenyl oxide disulfonate.
The present invention provides a method for producing a protein by using amino-oligosaccharin; and at least one of zhongshengmycin and kasugamycin as an active ingredient, can promote the sterilization effect and expand the sterilization spectrum through synergistic effects such as contact killing, penetration and the like with pathogenic bacteria and the like, and the inventor finds that in order to promote the heat storage stability of the active ingredient, when preparing a preparation such as granules, a stable environment needs to be provided, and the inventor finds that by controlling the carrier ingredient and the addition of a wetting agent and an oil agent in an auxiliary agent, the adsorption of the carrier ingredient in a sepiolite fiber structure can be promoted to obtain a composition with high storage stability.
This is probably because the oil agent and the active ingredient are insoluble, and when mixing and grinding, wetting agents such as anionic wetting agent and stearate etc. are adsorbed on the surface of the active ingredient, so that when adsorption occurs, the active ingredient is promoted to enter into the channels and pores of sepiolite along with the anionic wetting agent and stearate because of the structure of many cations in sepiolite, and the fixation of the active ingredient is also promoted because of the exchange of metal ions in sepiolite, anionic wetting agent and stearate, providing a stable environment, thereby promoting the problem of mutual decomposition of the active ingredient, etc., and improving the storage stability of the active ingredient.
In a preferred embodiment of the present invention, the wetting agent further comprises a nonionic wetting agent.
As a preferable technical scheme, the weight ratio of the nonionic wetting agent to the anionic wetting agent is (0.2-0.5): 1. the non-ionic wetting agent is selected from one or more of nonylphenol polyoxyethylene (2) ether, sorbitan monooleate, sorbitan stearate and octadecylamine polyoxyethylene (2) ether.
In a preferred embodiment of the present invention, the oil agent includes a fatty acid ester selected from one or more of isopropyl palmitate, methyl oleate, methyl laurate and ethyl laurate. The oil agent accounts for 0.5-20 wt% of the composition.
However, the inventors have also found that the carrier components used, such as sepiolite and the like, suffer from problems such as moisture absorption and the like, affecting the presence of the composition, and the present invention improves the moisture absorption properties of the resulting composition by controlling the structure of the oil agent and using a suitable nonionic wetting agent.
This is probably because, by adding a nonionic wetting agent, particularly sorbitan monooleate, sorbitan stearate, octadecylamine polyoxyethylene (2) ether, etc., which have a good compatibility with the oil agent, in the process of adsorption with the carrier, the polar substance of the fatty acid ester is adsorbed to the pore passage of the sepiolite, so that excessive adsorption of water is avoided, and the hydroxyl group of the structure such as sorbitan or octadecylamine in the nonionic wetting agent and the surface of the sepiolite are used to promote the partial attachment of the fatty acid ester and the wetting agent to the surface of the sepiolite, so that the contact between water and the sepiolite is reduced while the water penetration is reduced, and the stability in a humid environment is promoted.
In a preferred embodiment of the present invention, the carrier further comprises at least one of organobentonite, microcrystalline cellulose, and attapulgite. Preferably, the sepiolite/organobentonite mixture is organic bentonite, and the weight ratio of the sepiolite to the organobentonite is 1: (0.05-0.1).
According to a preferable technical scheme of the invention, the binder accounts for 0.5-10 wt% of the composition, and is selected from one or more of xanthan gum, polyvinyl alcohol and sodium acrylate.
And the inventors found that when a binder is added to obtain composition granules having different particle diameters of 500 to 2000. mu.m, problems such as binding may occur at higher temperatures, which may be caused by the fatty acid ester falling off from the inside of the carrier at higher temperatures, while the inventors found that when a suitable organic bentonite is added and the binder is controlled, the occurrence of binding at high temperatures can be reduced.
This is probably because when a small amount of organobentonite is added to sepiolite as a carrier, when adsorption with an auxiliary agent or an active ingredient occurs, a trace amount of gel is formed due to the action of organic substances and fatty acid esters in lamellar structures in the organobentonite, so that in the course of kneading and granulating with a binder such as xanthan gum or the like, the xanthan gum and the organobentonite lamellar structures in the surface of sepiolite are gelled to form an organic-inorganic crosslinked structure, thereby avoiding problems such as sticking at higher temperatures, and the inventors also found that this crosslinked structure is also advantageous in reducing problems such as moisture absorption and promoting storage stability of the composition.
The second aspect of the invention provides a preparation method of the oligosaccharins plant bactericidal synergistic composition, which comprises the following steps: mixing the active ingredients and the auxiliary agent, and granulating to obtain the composition.
As a preferred technical solution of the present invention, the preparation method of the composition comprises: grinding the active ingredients, the oil agent, the wetting agent and the fatty acid salt, adding the carrier for adsorption, adding the binder, and granulating to obtain the composition.
The granules are generally used by means of broadcasting and the like, active ingredients are released by utilizing moisture and the like in soil, and the active ingredients can be promoted to exert the synergistic sterilization effect by utilizing contact of water, a carrier and the like while reducing hygroscopicity by controlling the use amount of raw materials of the composition.
Compared with the prior art, the invention has the following beneficial effects: the present invention is achieved by using amino-oligosaccharins; and at least one of zhongshengmycin and kasugamycin is used as an active ingredient, so that the sterilization effect can be promoted, the sterilization spectrum is expanded, the addition of a carrier ingredient and a wetting agent and an oil agent in an auxiliary agent is controlled, the heat storage stability of the active ingredient is promoted, and the granules with low moisture absorption and good fluidity are obtained.
Detailed Description
Examples
Example 1
The embodiment provides a composition, which is prepared from raw materials comprising an active ingredient and an auxiliary agent, wherein the active ingredient comprises a first active ingredient and a second active ingredient; the first active ingredient is amino-oligosaccharin; the second active ingredient is zhongshengmycin, and the weight ratio of the first active ingredient to the second active ingredient is 1: 1, the active ingredient accounts for 10 wt% of the composition, the auxiliary agent comprises a carrier, an oil agent, a wetting agent, a fatty acid salt and a binder, the carrier comprises sepiolite and organic bentonite, and the weight ratio of the sepiolite to the organic bentonite is 1: 0.1, the balance being the weight percentage of the carrier in the composition, the fatty acid salt accounting for 20 wt% of the active ingredient, the calcium stearate being the fatty acid salt, the wetting agent accounting for 8 wt% of the composition, the wetting agent comprising an anionic wetting agent, the anionic wetting agent being calcium dodecylbenzenesulfonate, the wetting agent further comprising a nonionic wetting agent, the nonionic wetting agent being sorbitan monooleate, the weight ratio of the nonionic wetting agent to the anionic wetting agent being 0.5: the oil agent comprises fatty acid ester, the fatty acid ester is isopropyl palmitate, the oil agent accounts for 15 wt% of the composition, the binder accounts for 6 wt% of the composition, and the binder is xanthan gum.
This example also provides a method of preparing a composition as described above comprising: grinding the active ingredients, the oil agent, the wetting agent and the fatty acid salt, adding the carrier for adsorption, adding the binder, and granulating to obtain the composition.
Example 2
The embodiment provides a composition, which is prepared from raw materials comprising an active ingredient and an auxiliary agent, wherein the active ingredient comprises a first active ingredient and a second active ingredient; the first active ingredient is amino-oligosaccharin; the second active ingredient is zhongshengmycin, and the weight ratio of the first active ingredient to the second active ingredient is 2: 1, the active ingredient accounts for 8 wt% of the composition, the auxiliary agent comprises a carrier, an oil agent, a wetting agent, a fatty acid salt and a binder, the carrier comprises sepiolite and organic bentonite, and the weight ratio of the sepiolite to the organic bentonite is 1: 0.08, the weight percentage of the carrier in the composition is the balance, the fatty acid salt accounts for 15 wt% of the active ingredient, the fatty acid salt is magnesium stearate, and the wetting agent accounts for 5 wt% of the composition, wherein the wetting agent comprises an anionic wetting agent, the anionic wetting agent is calcium dodecylbenzene sulfonate, the wetting agent further comprises a nonionic wetting agent, the nonionic wetting agent is sorbitan stearate, and the weight ratio of the nonionic wetting agent to the anionic wetting agent is 0.4: the oil agent comprises fatty acid ester, the fatty acid ester is methyl oleate, the oil agent accounts for 10 wt% of the composition, the binder accounts for 4 wt% of the composition, and the binder is xanthan gum.
This example also provides a method of preparing a composition as described above comprising: grinding the active ingredients, the oil agent, the wetting agent and the fatty acid salt, adding the carrier for adsorption, adding the binder, and granulating to obtain the composition.
Example 3
The embodiment provides a composition, which is prepared from raw materials comprising an active ingredient and an auxiliary agent, wherein the active ingredient comprises a first active ingredient and a second active ingredient; the first active ingredient is amino-oligosaccharin; the second active ingredient is kasugamycin, and the weight ratio of the first active ingredient to the second active ingredient is 1: 2, the active ingredient accounts for 3 wt% of the composition, the auxiliary agent comprises a carrier, an oil agent, a wetting agent, a fatty acid salt and a binder, the carrier comprises sepiolite and organic bentonite, and the weight ratio of the sepiolite to the organic bentonite is 1: 0.05, the balance being the weight percentage of the carrier in the composition, 10 wt% of the fatty acid salt, magnesium stearate being the fatty acid salt, 3 wt% of the composition being the wetting agent, wherein the wetting agent comprises an anionic wetting agent, the anionic wetting agent is sodium dodecyl diphenyl ether disulfonate, the wetting agent further comprises a nonionic wetting agent, the nonionic wetting agent is octadecylamine polyoxyethylene (2) ether, and the weight ratio of the nonionic wetting agent to the anionic wetting agent is 0.2: the oil agent comprises fatty acid ester, the fatty acid ester is methyl oleate, the oil agent accounts for 8 wt% of the composition, the binder accounts for 2 wt% of the composition, and the binder is xanthan gum.
This example also provides a method of preparing a composition as described above comprising: grinding the active ingredients, the oil agent, the wetting agent and the fatty acid salt, adding the carrier for adsorption, adding the binder, and granulating to obtain the composition.
Example 4
The embodiment provides a composition, which is prepared from raw materials comprising an active ingredient and an auxiliary agent, wherein the active ingredient comprises a first active ingredient and a second active ingredient; the first active ingredient is amino-oligosaccharin; the second active ingredient is zhongshengmycin, and the weight ratio of the first active ingredient to the second active ingredient is 2: 1, the active ingredient accounts for 8 wt% of the composition, the auxiliary agent comprises a carrier, an oil agent, a wetting agent, a fatty acid salt and a binder, the carrier comprises sepiolite and organic bentonite, and the weight ratio of the sepiolite to the organic bentonite is 1: 0.08, the balance being the weight percentage of the carrier in the composition, the fatty acid salt accounting for 15 wt% of the active ingredient, the magnesium stearate being the fatty acid salt, and the 5 wt% of the wetting agent accounting for the wetting agent, wherein the wetting agent comprises an anionic wetting agent, the anionic wetting agent is calcium dodecylbenzene sulfonate, the wetting agent further comprises a nonionic wetting agent, the nonionic wetting agent is sorbitan stearate, and the weight ratio of the nonionic wetting agent to the anionic wetting agent is 0.05: the oil agent comprises fatty acid ester, the fatty acid ester is methyl oleate, the oil agent accounts for 10 wt% of the composition, the binder accounts for 4 wt% of the composition, and the binder is xanthan gum.
This example also provides a method of making a composition as described above comprising: grinding the active ingredients, the oil agent, the wetting agent and the fatty acid salt, adding the carrier for adsorption, adding the binder, and granulating to obtain the composition.
Example 5
The embodiment provides a composition, which is prepared from raw materials comprising an active ingredient and an auxiliary agent, wherein the active ingredient comprises a first active ingredient and a second active ingredient; the first active ingredient is amino-oligosaccharin; the second active ingredient is zhongshengmycin, and the weight ratio of the first active ingredient to the second active ingredient is 2: the active ingredient accounts for 8 wt% of the composition, the auxiliary agent comprises a carrier, an oil agent, a wetting agent, a fatty acid salt and a binder, the carrier comprises sepiolite, the weight percentage of the carrier in the composition is the balance, the fatty acid salt accounts for 15 wt% of the active ingredient, the fatty acid salt is magnesium stearate, the wetting agent accounts for 5 wt% of the composition, the wetting agent comprises an anionic wetting agent, the anionic wetting agent is calcium dodecylbenzene sulfonate, the wetting agent further comprises a nonionic wetting agent, the nonionic wetting agent is sorbitan stearate, and the weight ratio of the nonionic wetting agent to the anionic wetting agent is 0.4: the oil agent comprises fatty acid ester, the fatty acid ester is methyl oleate, the oil agent accounts for 10 wt% of the composition, the binder accounts for 4 wt% of the composition, and the binder is xanthan gum.
This example also provides a method of preparing a composition as described above comprising: grinding the active ingredients, the oil agent, the wetting agent and the fatty acid salt, adding the carrier for adsorption, adding the binder, and granulating to obtain the composition.
Evaluation of Performance
1. Moisture absorption rate: the granules provided in examples 1 to 5 were left at 28 ℃ under a 70% relative humidity environment for 12 hours, and the moisture absorption rate (post-moisture weight-pre-moisture weight)/pre-moisture weight of 100% and the moisture absorption rate of less than 0.5 wt% were observed, and the results are shown in table 1.
2. Heat storage stability:
(1) decomposition rate: after the granules provided in examples 1 to 3 were stored at 54 ℃ for 2 weeks, the decomposition rates of the active ingredients were measured, and it was found that all of the amino-oligosaccharin, zhongshengmycin, and kasugamycin were 3% or less in decomposition rate.
(2) Adhesion: the granules provided in examples 1 to 5 were stored at 54 ℃ for 2 weeks, 3 weeks, and 4 weeks, and then, whether or not adhesion occurred between the granules was observed, wherein no adhesion was represented by O and the occurrence of adhesion was represented by X, and the results are shown in Table 1.
3. Fluidity: examples 1-3 provide granules having an angle of repose less than 30 °.
Table 1 performance characterization test
Figure BDA0003228649960000061
Figure BDA0003228649960000071
The test result shows that the composition provided by the invention has high synergistic bactericidal action, can be used for preparing formulations such as granules and the like, and is used for preventing and treating diseases of various crops and fruits and vegetables.

Claims (10)

1. The oligosaccharins plant sterilization synergistic composition is characterized in that raw materials for preparing the composition comprise active ingredients and auxiliaries, wherein the active ingredients comprise a first active ingredient and a second active ingredient; the first active ingredient is amino-oligosaccharin; the second active ingredient is at least one of zhongshengmycin and kasugamycin.
2. The oligosaccharide plant sterilization synergistic composition as claimed in claim 1, wherein the active ingredient accounts for 0.5-20 wt% of the composition.
3. The oligosaccharin plant bactericidal synergistic composition according to claim 1 or 2, wherein the auxiliary agent is selected from one or more of a carrier, an oil agent, a wetting agent, a fatty acid salt, a stabilizer, a spreader and a binder.
4. The oligosaccharins plant bactericidal synergistic composition of claim 3, wherein the carrier comprises one or more of starch, sepiolite, trehalose, potassium chloride, urea, magnesium aluminum silicate, attapulgite, kaolin.
5. The oligosaccharide plant bactericidal synergistic composition of claim 3 wherein the fatty acid salt is selected from one or more of calcium stearate, magnesium stearate, calcium palmitate and magnesium palmitate.
6. The oligosaccharin plant bactericidal synergistic composition of claim 3, wherein the wetting agent comprises an anionic wetting agent selected from one or more of sodium dodecyl sulfate, calcium dodecyl benzene sulfonate, sodium dodecyl sulfate, lignosulfonate, alkyl ethyl sulfonate, fatty alcohol sulfate, sodium dodecyl diphenyl oxide disulfonate.
7. The oligosaccharin plant bactericidal synergistic composition of claim 6, wherein the wetting agent further comprises a non-ionic wetting agent selected from one or more of nonylphenol polyoxyethylene (2) ether, sorbitan monooleate, sorbitan stearate, and octadecylamine polyoxyethylene (2) ether.
8. The oligosaccharin plant bactericidal synergistic composition of claim 3, wherein the fatty acid ester is selected from one or more of isopropyl palmitate, methyl oleate, methyl laurate and ethyl laurate.
9. The oligosaccharins plant bactericidal synergistic composition of claim 3, wherein the binder is selected from one or more of xanthan gum, polyvinyl alcohol, and sodium acrylate.
10. A method for preparing the oligosaccharide plant bactericidal synergistic composition according to any one of claims 1 to 9, which comprises the following steps: mixing the active ingredients and the auxiliary agents, and granulating to obtain the composition.
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