CN110754476A - Soluble solution for improving stability of 6-benzylaminopurine preparation and preparation method thereof - Google Patents
Soluble solution for improving stability of 6-benzylaminopurine preparation and preparation method thereof Download PDFInfo
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION 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
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/90—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having two or more relevant hetero rings, condensed among themselves or with a common carbocyclic ring system
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION 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
- A01N25/00—Biocides, 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
- A01N25/02—Biocides, 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 containing liquids as carriers, diluents or solvents
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Abstract
The invention discloses a soluble solution for improving the stability of a 6-benzylaminopurine preparation and a preparation method thereof, wherein the soluble solution comprises the following components in parts by weight: 0.1-30 parts of 6-benzylaminopurine, 0.1-30 parts of cosolvent, 1-60 parts of solvent and 1-60 parts of stabilizer; the cosolvent is a strong acid weak base salt or a strong acid lipid compound; the solvent is a polar high flash point solvent; the stabilizer is an acid compound. The invention adopts strong acid weak base salt or strong acid lipid compound to dissolve 6-BA to prepare 6-BA soluble solution, which can improve the solubility of benzylaminopurine, ensure the storage stability, improve the product quality, improve the production safety and reduce the production cost.
Description
Technical Field
The invention relates to the technical field of production of 6-benzylaminopurine preparations, and in particular relates to a soluble solution for improving the stability of a 6-benzylaminopurine preparation and a preparation method thereof.
Background
6-benzylaminopurine (6-BA) is a plant growth regulator, is a first artificially synthesized cytokinin, can promote plant cell growth, inhibit the degradation of plant chlorophyll, improve the content of amino acid, delay leaf senescence, induce bud differentiation, promote lateral bud growth, promote cell division, reduce the decomposition of chlorophyll in plants, and has the effects of inhibiting senescence and keeping green; meanwhile, the fertilizer has various effects of transferring amino acid, auxin, inorganic salt and the like to a treatment part and the like, and is widely applied to various stages from germination to harvest of agricultural, fruit trees and horticultural crops. 6-BA is white crystalline powder, is insoluble in water, slightly soluble in ethanol, and stable in acid and alkali.
According to the physicochemical properties of the raw benayl aminopurine, the characteristics of pesticide formulations are followed, and the 6-BA is developed into a soluble solution or a suspending agent ideally. However, the modern pesticide is a future development trend, and the suspending agent is added with a thickening agent to improve the stability in order to ensure less water precipitation, no layering and no bottom formation in the storage process, but the high viscosity is not beneficial to airplane spraying; meanwhile, the suspending agent is an unstable system, and when the suspending agent is mixed with other pesticides, particularly mixed with a fly spray auxiliary agent used in combination with fly spray, the flocculation phenomenon is easy to occur due to the improvement of wettability, the spray head can be blocked, or the chemical injury is easy to occur due to the non-uniform liquid medicine; the soluble solution is a true solution, is much more stable than a suspending agent, has simple processing technology and simple processing equipment, and better conforms to the future development trend. It is therefore more desirable to develop 6-BA as a soluble agent.
The 6-BA is processed into soluble solution, and because the 6-BA is difficult to dissolve in water, the 6-BA is very easy to separate out once diluted by water and cannot meet the dilution stability index of the soluble solution, the prior preparation of the 6-BA soluble solution mainly adopts the steps of adding acid or alkali for compounding, so that the 6-BA and the acid or alkali are salified to improve the solubility of the soluble solution, but the reaction process is a reversible reaction, and the salified compound reacts in the hydrolysis direction along with the change of the external environment, so that the original medicine is separated out, and the product quality is unstable; if strong acid or strong base is adopted for salifying, the formed salt is relatively more stable, and the product quality requirement can be met; however, strong acids (sulfuric acid, hydrochloric acid, nitric acid, methanesulfonic acid, benzenesulfonic acid, trichloroacetic acid and the like) and strong bases (sodium hydroxide, potassium hydroxide, sodium methoxide, potassium ethoxide and the like) belong to dangerous chemicals and are not small hidden dangers for the life safety and health of operators; the country has increasingly strict control on hazardous chemicals; the requirements on hazardous chemical use manufacturers are increasingly strict, and the processing cost and the management cost are increased in the process of invisibility.
Disclosure of Invention
In view of the above, the present invention aims to provide a soluble solution for improving the stability of 6-benzylaminopurine preparation and a preparation method thereof, so as to solve the problems of safety and cost in the preparation process of the 6-BA soluble solution proposed in the above background art.
In order to achieve the above object, the present invention provides a soluble solution for improving the stability of a 6-benzylaminopurine preparation, wherein the soluble solution comprises the following components by weight:
0.1-30 parts of 6-benzylaminopurine, 0.1-30 parts of cosolvent, 1-60 parts of stabilizer and 1-60 parts of solvent;
the cosolvent is a strong acid weak base salt or a strong acid lipid compound; further, the cosolvent is selected from formate, sulfate, chloride and phosphate compounds; the formate is aluminum formate or magnesium formate, and the sulfate is aluminum sulfate or ferric sulfate. The addition of the cosolvent can improve the solubility of the 6-BA in the soluble agent and improve the quality of the product.
The stabilizer is an acid compound; further, the stabilizer is selected from lactic acid, citric acid, malic acid, tartaric acid and phytic acid.
The solvent is a high flash point polar solvent; further, the high flash point polar solvent is a polar solvent having a flash point higher than 60 ℃, and the kinds of the polar solvent include, but are not limited to, alcohol, dialkyl ketone, alkylene carbonate, alkyl ester, aryl ester, and sulfone-based solvents.
The material existing in liquid state at normal temperature and having flash point below 60 deg.c is inflammable and has the features of easy burning, high heat expansibility, easy electrostatic aggregation, high flowability, strong oxidizing acid and oxidant action, different toxicity, etc. And the polar solvent with the flash point higher than 60 ℃ does not belong to flammable liquid and dangerous chemical management, so that the danger is reduced, and the management cost is reduced.
Further, the soluble agent also comprises 1-20 parts by weight of a synergist according to different required efficacies of the soluble agent. The synergist is selected from tween, glucoside, alkyl polyglycoside, alkyl polyether and sugar.
The Tween can promote the absorption of plant into water insoluble macromolecule, and also can help water to permeate into lipid-rich biological membrane. The glucoside, alkyl polyglycoside, alkyl polyether and sugar are all surfactants, have strong broad-spectrum antibacterial activity and obvious synergistic effect, and can greatly improve the performance of the 6-BA soluble agent when used as a synergist.
The invention also provides a preparation method of the soluble solution for improving the stability of the 6-benzylaminopurine preparation, which comprises the following steps:
weighing the following raw materials in parts by weight: 0.1-30 parts of 6-benzylaminopurine, 0.1-30 parts of cosolvent, 1-60 parts of stabilizer and 1-60 parts of solvent, wherein the solvent, the cosolvent and the stabilizer are uniformly mixed, and 6-benzylaminopurine is added to completely dissolve the mixture to obtain the 6-benzylaminopurine soluble agent; the cosolvent is a strong acid weak base salt or a strong acid lipid compound; the solvent is a polar high flash point solvent; the stabilizer is an acid compound.
Further, the 6-benzylaminopurine soluble solution also comprises 1-20 parts by weight of a synergist, wherein the 6-benzylaminopurine soluble solution is obtained by uniformly mixing a solvent, a cosolvent and a stabilizer, adding 6-benzylaminopurine to dissolve completely, and adding the synergist; the synergist is selected from tween, glucoside, alkyl polyglycoside, alkyl polyether and sugar.
Compared with the prior art, the method adopts the strong acid weak base salt or the strong acid ester compound as the cosolvent to dissolve the 6-benzylaminopurine, the strong acid weak base salt or the strong acid ester compound can hydrolyze out strong acid or medium strong acid, so that the salt forming reaction can be better carried out with 6-BA, the reaction is prevented from being carried out in the reverse direction, the solubility of the 6-BA is improved, and the strong acid weak base salt is easy to generate precipitate in the hydrolysis process to influence the transparency of the preparation and influence the judgment of the quality standard of the subsequent preparation.
The invention adopts strong acid weak base salt or strong acid lipid compound to dissolve 6-BA to prepare 6-BA soluble solution, thereby not only solving the danger caused by adopting strong acid or strong base as solvent to improve the solubility and stability of 6-BA, but also greatly improving the solubility and storage stability of 6-benzylaminopurine compared with adopting weak acid to dissolve 6-BA, the invention improves the product quality of 6-benzylaminopurine preparation, improves the production safety and reduces the production cost.
Detailed Description
In order to make those skilled in the art better understand the technical solution of the present invention, the following detailed description of the present invention is provided with reference to specific embodiments. It is to be understood that the described embodiments are merely some embodiments of the invention and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention firstly provides a soluble solution for improving the stability of a 6-benzylaminopurine preparation, which comprises the following components in parts by weight:
0.1-30 parts of 6-benzylaminopurine, 0.1-30 parts of cosolvent, 1-60 parts of stabilizer and 1-60 parts of solvent;
the cosolvent is a strong acid weak base salt or a strong acid lipid compound; further, the cosolvent is selected from formate, sulfate, chloride and phosphate compounds; the formate is aluminum formate or magnesium formate, and the sulfate is aluminum sulfate or ferric sulfate.
The stabilizer is an acid compound; further, the stabilizer is selected from lactic acid, citric acid, malic acid, tartaric acid and phytic acid.
The solvent is a polar high flash point solvent; further, the high flash point polar solvent is a polar solvent having a flash point higher than 60 ℃, and the kinds of the polar solvent include, but are not limited to, alcohol, dialkyl ketone, alkylene carbonate, alkyl ester, aryl ester, and sulfone-based solvents.
Further, the soluble agent also comprises 1-20 parts by weight of a synergist according to different required efficacies of the soluble agent. The synergist is selected from tween, glucoside, alkyl polyglycoside, alkyl polyether and sugar.
The invention also provides a preparation method of the soluble solution for improving the stability of the 6-benzylaminopurine preparation, which comprises the following steps:
weighing the following raw materials in parts by weight: 0.1-30 parts of 6-benzylaminopurine, 0.1-30 parts of cosolvent, 1-60 parts of stabilizer, 1-60 parts of solvent and 1-20 parts of synergist, wherein the solvent, the cosolvent and the stabilizer are uniformly mixed, and the 6-benzylaminopurine is added to be completely dissolved, and then the synergist is added to obtain the 6-benzylaminopurine soluble solution; the cosolvent is a strong acid weak base salt or a strong acid lipid compound; the solvent is a polar high flash point solvent; the stabilizer is an acid compound.
Further, the 6-benzylaminopurine soluble solution also comprises 1-20 parts by weight of a synergist, wherein the 6-benzylaminopurine soluble solution is obtained by uniformly mixing a solvent, a cosolvent and a stabilizer, adding 6-benzylaminopurine to dissolve completely, and adding the synergist; the synergist is selected from tween, glucoside, alkyl polyglycoside, alkyl polyether and sugar.
The stability of the 6-BA solubles prepared by the process of the present invention is illustrated below by means of specific examples. The cosolvent in examples 1 to 5 is a strong acid weak base salt, the cosolvent in example 6 is a strong acid lipid compound, and the cosolvent in comparative examples 1 and 2 is a medium strong acid.
Example 1:
30% benzylaminopurine soluble agent, production method and determination of various quality indexes
After 30.6g of benayl aminopurine is completely dissolved by 8.0g of aluminum sulfate and 60g of malic acid, 1g of synergist Tween-20 is added, and then 100g of water is used for complementing; thus obtaining 30% benzylaminopurine soluble agent.
The benzylaminopurine soluble solution is detected by referring to the enterprise standard Q/91510185MA68HDG804 & 71-2018, and the detection results of all quality indexes are shown in the following table.
Example 2:
0.1% benzylaminopurine soluble agent, production method and determination of various quality indexes
After 0.1g of benzylaminopurine is completely dissolved by 0.05g of ferric sulfate and 1g of phytic acid, 5g of synergist alkylpolyglycoside synergist and 5g of dimethyl sulfoxide solvent are added, and then 100g of water is used for complementing; thus obtaining 0.1 percent benayl aminopurine soluble agent.
The benzylaminopurine soluble solution is detected by referring to the enterprise standard Q/91510185MA68HDG804 & 71-2018, and the detection results of all quality indexes are shown in the following table.
Example 3:
2% benzylaminopurine soluble agent, production method and determination of various quality indexes
After 2g of benzylaminopurine is completely dissolved by 1g of aluminum formate and 6g of lactic acid, 5g of alkylpolyglycoside synergist and 50g of propylene glycol solvent are added, and then 100g of water is used for supplementing; thus obtaining the 2% benzylaminopurine soluble agent.
The benzylaminopurine soluble solution is detected by referring to the enterprise standard Q/91510185MA68HDG804 & 71-2018, and the detection results of all quality indexes are shown in the following table.
Example 4:
1% benzylaminopurine soluble agent, production method and determination of various quality indexes
After 1.0 benzylaminopurine is completely dissolved by 1g of calcium chloride and 2g of lactic acid, 5g of alkyl polyether synergist and 60g of glycol solvent are added, and then 100g of water is used for complementing; thus obtaining the 1% benzylaminopurine soluble agent.
The benzylaminopurine soluble solution is detected by referring to the enterprise standard Q/91510185MA68HDG804 & 71-2018, and the detection results of all quality indexes are shown in the following table.
Example 5:
5% benzylaminopurine soluble agent, production method and determination of various quality indexes
After 5.1g of benzylaminopurine is completely dissolved by 2g of magnesium formate and 10g of tartaric acid, 15g of carbohydrate synergist and 60g of glycol solvent are added, and then 100g of water is used for supplementing; thus obtaining 5% benzylaminopurine soluble agent.
The benzylaminopurine soluble solution is detected by referring to the enterprise standard Q/91510185MA68HDG804 & 71-2018, and the detection results of all quality indexes are shown in the following table.
Example 6:
2% benzylaminopurine soluble agent, production method and determination of various quality indexes
After 2.1g of benzylaminopurine is completely dissolved by 2g of trimethyl phosphate and 4g of lactic acid, 5g of glycoside synergist and 60g of glycol solvent are added, and then 100g of water is used for supplementing; thus obtaining the 2% benzylaminopurine soluble agent.
The benzylaminopurine soluble solution is detected by referring to the enterprise standard Q/91510185MA68HDG804 & 71-2018, and the detection results of all quality indexes are shown in the following table.
Comparative example 1:
5% benzylaminopurine soluble agent, production method and determination of various quality indexes
After 5.1g of benzylaminopurine is completely dissolved by 16.0g of lactic acid, 10g of synergist Tween-20 is added, and then 100g of propylene glycol is used for supplementing; thus obtaining 5% benzylaminopurine soluble agent.
The benzylaminopurine soluble solution is detected by referring to the enterprise standard Q/91510185MA68HDG804 & 71-2018, and the detection results of all quality indexes are shown in the following table.
Comparative example 2:
2% benzylaminopurine soluble agent, production method and determination of various quality indexes
Dissolving 2.0g benzylaminopurine with 6g citric acid and a small amount of water completely, adding 10g glycoside synergist, and supplementing 100g with propylene carbonate; thus obtaining the 2% benzylaminopurine soluble agent.
The benzylaminopurine soluble solution is detected by referring to the enterprise standard Q/91510185MA68HDG804 & 71-2018, and the detection results of all quality indexes are shown in the following table.
As can be seen from the above examples, the quality of the 6-BA soluble solution prepared by the method provided by the invention is obviously better than that of the soluble solution prepared by dissolving 6-BA by using medium-strong acid, the solubility of benzylaminopurine is better, and the storage stability is stronger.
The solubility of 6-BA in the 6-BA solubles prepared by the process of the present invention is greatly improved as will be described below with reference to specific examples.
Example 7: adding 60g of propylene glycol (heated to 40-45 ℃) into a mixing device, gradually adding the 6-BA technical material, stirring and dissolving for 30min, stopping adding the 6-BA technical material when solute particles or liquid drops just appear in the mixing device, and recording the adding amount of the 6-BA.
Example 8: adding 60g of propylene glycol (heated to 40-45 ℃) into a mixing device, adding 2g of citric acid, gradually adding the 6-BA technical material, stirring and dissolving for 30min, stopping adding the 6-BA technical material when solute particles or liquid drops just appear in the mixing device, and recording the adding amount of 6-BA.
Example 9: adding 60g of propylene glycol (heated to 40-45 ℃), 2g of citric acid and 2g of aluminum formate into a mixing device, gradually adding the 6-BA technical product, stirring and dissolving for 30min, stopping adding the 6-BA technical product when solute particles or liquid drops just appear in the mixing device, and recording the adding amount of 6-BA.
Example 10: adding 60g of propylene glycol (heated to 40-45 ℃) into a mixing device, adding 4g of tartaric acid into 6-BA raw pesticide by volume, stirring and dissolving for 30min, stopping adding the 6-BA raw pesticide when solute particles or liquid drops just appear in the mixing device, and recording the adding amount of 6-BA.
Example 11: adding 60g of propylene glycol (heated to 40-45 ℃), 4g of tartaric acid and 3g of magnesium formate into a mixing device, gradually adding the 6-BA technical product, stirring and dissolving for 30min, stopping adding the 6-BA technical product when solute particles or liquid drops just appear in the mixing device, and recording the adding amount of 6-BA.
Example 12: adding 60g of propylene glycol (heated to 40-45 ℃), 10g of tartaric acid and 5g of aluminum sulfate into a mixing device, gradually adding the 6-BA technical product, stirring and dissolving for 30min, stopping adding the 6-BA technical product when solute particles or liquid drops just appear in the mixing device, and recording the adding amount of 6-BA.
Example 13: adding 60g of propylene glycol (heated to 40-45 ℃) into a mixing device, adding 10g of tartaric acid, gradually adding 6-BA technical material, stirring and dissolving for 30min, stopping adding the 6-BA technical material when solute particles or liquid drops just appear in the mixing device, and recording the adding amount of 6-BA.
Example 14: adding 60g of propylene glycol (heated to 40-45 ℃), 25g of citric acid and 15g of magnesium sulfate into a mixing device, gradually adding the 6-BA technical material, stirring and dissolving for 30min, stopping adding the 6-BA technical material when solute particles or liquid drops just appear in the mixing device, and recording the adding amount of 6-BA.
Example 15: adding 60g of propylene glycol (heated to 40-45 ℃) into a mixing device, adding 25g of citric acid, gradually adding the 6-BA technical material, stirring and dissolving for 30min, stopping adding the 6-BA technical material when solute particles or liquid drops just appear in the mixing device, and recording the adding amount of 6-BA.
Example 16: adding 60g of propylene glycol (heated to 40-45 ℃), 60g of lactic acid and 8g of aluminum sulfate into a mixing device, gradually adding the 6-BA technical raw material, stirring and dissolving for 30min, stopping adding the 6-BA technical raw material when solute particles or liquid drops just appear in the mixing device, and recording the adding amount of 6-BA.
Example 17: adding 60g of propylene glycol (heated to 40-45 ℃) into a mixing device, adding 60g of lactic acid, gradually adding 6-BA technical material, stirring and dissolving for 30min, stopping adding the 6-BA technical material when solute particles or liquid drops just appear in the mixing device, and recording the adding amount of 6-BA.
Example 18: adding 60g of propylene glycol (heated to 40-45 ℃), 2g of lactic acid and 1g of calcium chloride into a mixing device, gradually adding the 6-BA technical product, stirring and dissolving for 30min, stopping adding the 6-BA technical product when solute particles or liquid drops just appear in the mixing device, and recording the adding amount of 6-BA.
Example 19: adding 60g of propylene glycol (heated to 40-45 ℃), 4g of lactic acid and 2g of trimethyl phosphate into a mixing device, gradually adding the 6-BA technical raw material, stirring and dissolving for 30min, stopping adding the 6-BA technical raw material when solute particles or liquid drops just appear in the mixing device, and recording the adding amount of 6-BA.
The results of the measurements are shown in the following table:
solvent solubility of 6-BA at 40 deg.C
It should be noted that the above-mentioned embodiments should not be construed as limiting the present invention, and the scope of the present invention should be subject to the scope defined by the appended claims. It will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the spirit and scope of the invention, and these modifications and adaptations should be considered within the scope of the invention.
Claims (9)
1. A soluble solution for improving the stability of a 6-benzylaminopurine preparation, which is characterized in that: the soluble agent comprises the following components in parts by weight:
0.1-30 parts of 6-benzylaminopurine, 0.1-30 parts of cosolvent, 1-60 parts of stabilizer and 1-60 parts of solvent;
the cosolvent is a strong acid weak base salt or a strong acid lipid compound; the solvent is a high flash point polar solvent; the stabilizer is an acid compound.
2. The solubles of claim 1 wherein said 6-benzylaminopurine formulation has improved stability as a result of: the soluble agent also comprises 1-20 parts by weight of a synergist.
3. The solubles of claim 1 wherein said 6-benzylaminopurine formulation has improved stability as a result of: the solvent is a polar solvent having a flash point above 60 ℃, and the class of polar solvents includes, but is not limited to, alcohols, dialkyl ketones, alkylene carbonates, alkyl esters, aryl esters, and sulfone type solvents.
4. The solubles of claim 1 wherein said 6-benzylaminopurine formulation has improved stability as a result of: the stabilizer is selected from lactic acid, citric acid, malic acid, tartaric acid and phytic acid.
5. The solubles of claim 2 wherein said 6-benzylaminopurine formulation has improved stability as a result of: the synergist is selected from tween, glucoside, alkyl polyglycoside, alkyl polyether and sugar.
6. The solubles of claim 1 wherein said 6-benzylaminopurine formulation has improved stability as a result of: the cosolvent is selected from formate, sulfate, chloride and phosphate ester compounds.
7. The solubles of claim 6 for improving the stability of a 6-benzylaminopurine formulation, wherein: the formate is aluminum formate or magnesium formate, and the sulfate is aluminum sulfate or ferric sulfate.
8. A method for preparing a soluble solution for improving the stability of a 6-benzylaminopurine preparation is characterized in that: the method comprises the following steps:
weighing the following raw materials in parts by weight: 0.1-30 parts of 6-benzylaminopurine, 0.1-30 parts of cosolvent, 1-60 parts of stabilizer, 1-60 parts of solvent and 1-20 parts of synergist, wherein the solvent, the cosolvent and the stabilizer are uniformly mixed, and 6-benzylaminopurine is added to completely dissolve the mixture to obtain the 6-benzylaminopurine soluble solution; the cosolvent is a strong acid weak base salt or a strong acid lipid compound; the solvent is a polar high flash point solvent; the stabilizer is an acid compound.
9. The method of claim 8, wherein the step of preparing a solubles comprises the steps of: the 6-benzylaminopurine soluble solution also comprises 1-20 parts by weight of a synergist, wherein the 6-benzylaminopurine soluble solution is obtained by uniformly mixing a solvent, a cosolvent and a stabilizer, adding 6-benzylaminopurine to dissolve completely, and adding the synergist; the synergist is selected from tween, glucoside, alkyl polyglycoside, alkyl polyether and sugar.
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