CN112889823B - Liquid preparation for improving stability of diethyl aminoethyl hexanoate preparation and preparation method thereof - Google Patents
Liquid preparation for improving stability of diethyl aminoethyl hexanoate preparation and preparation method thereof Download PDFInfo
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- CN112889823B CN112889823B CN202110083911.5A CN202110083911A CN112889823B CN 112889823 B CN112889823 B CN 112889823B CN 202110083911 A CN202110083911 A CN 202110083911A CN 112889823 B CN112889823 B CN 112889823B
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- diethyl aminoethyl
- aminoethyl hexanoate
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- OORIKNJWZHTXDC-UHFFFAOYSA-N CCCC(CC)C(CC)(C(=O)OCC)N Chemical compound CCCC(CC)C(CC)(C(=O)OCC)N OORIKNJWZHTXDC-UHFFFAOYSA-N 0.000 title claims abstract description 154
- 238000002360 preparation method Methods 0.000 title claims abstract description 80
- 239000007788 liquid Substances 0.000 title claims abstract description 24
- 239000006184 cosolvent Substances 0.000 claims abstract description 43
- 239000002904 solvent Substances 0.000 claims abstract description 41
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims abstract description 31
- LCTONWCANYUPML-UHFFFAOYSA-N Pyruvic acid Chemical compound CC(=O)C(O)=O LCTONWCANYUPML-UHFFFAOYSA-N 0.000 claims abstract description 26
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- 238000000034 method Methods 0.000 claims description 19
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- 239000001069 triethyl citrate Substances 0.000 abstract description 5
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- DMAXMXPDVWTIRV-UHFFFAOYSA-N 2-(2-phenylethyl)phenol Chemical compound OC1=CC=CC=C1CCC1=CC=CC=C1 DMAXMXPDVWTIRV-UHFFFAOYSA-N 0.000 description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
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Classifications
-
- 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
- A01N37/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
- A01N37/12—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing the group, wherein Cn means a carbon skeleton not containing a ring; Thio analogues thereof
-
- 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
-
- 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
- A01N25/22—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 ingredients stabilising the active ingredients
Abstract
The liquid preparation for improving the stability of the diethyl aminoethyl hexanoate preparation comprises, by mass, 0.1-20% of diethyl aminoethyl hexanoate, 0.1-30% of an auxiliary agent, 1-32% of a solvent and the balance of the solvent to 100%; the cosolvent comprises a cosolvent A and a cosolvent B; the cosolvent A is at least one of dimethyl sulfoxide and dimethylacetamide; the cosolvent B is at least one of lactic acid, pyruvic acid and phytic acid; the solvent is at least one of propylene glycol methyl ether acetate, triethyl citrate and glyceryl triacetate. The liquid preparation for improving the stability of the diethyl aminoethyl hexanoate preparation can effectively prevent diethyl aminoethyl hexanoate from decomposing and improve the application effect of the liquid preparation.
Description
Technical Field
The invention relates to the field of pesticide plant growth regulator preparations, in particular to a liquid preparation for improving the stability of an diethyl aminoethyl hexanoate preparation and a preparation method thereof.
Background
Diethyl aminoethyl hexanoate citrate (diethyl aminoethyl hexanoate), also known as diethyl aminoethyl hexanoate (DA-6), is referred to herein as diethyl aminoethyl hexanoate citrate. The diethyl aminoethyl hexanoate is a high-energy plant growth regulator with broad spectrum and breakthrough effects. It can raise the contents of chlorophyll, protein and nucleic acid in plant body and photosynthetic rate, raise the activity of peroxidase and nitrate reductase, promote the metabolism of carbon and nitrogen in plant, raise the absorption of water and fertilizer and the accumulation of dry matter in plant body, regulate water balance in plant body, raise the resistance of crop and fruit tree to diseases, drought and cold, delay senility, promote the early ripening and yield of crop and raise crop quality.
The diethyl aminoethyl hexanoate is white or light yellow powder, has light ester fragrance and greasy feel, is easily dissolved in water, can be dissolved in polar organic solvents such as ethanol, methanol, acetone and the like, and can be prepared into various dosage forms such as water aqua, soluble agent, soluble powder, tablet and the like. But the diethyl aminoethyl hexanoate is extremely easy to hydrolyze and alcoholyze and is extremely easy to decompose in water and alcohol.
Disclosure of Invention
The invention provides a device for solving the defects in the prior art.
The invention provides a liquid preparation for improving the stability of an diethyl aminoethyl hexanoate preparation, which comprises 0.1-20% of diethyl aminoethyl hexanoate, 0.1-30% of an auxiliary agent, 1-32% of a solvent and the balance of the solvent to 100%; the cosolvent comprises a cosolvent A and a cosolvent B; the cosolvent A is at least one of dimethyl sulfoxide and dimethylacetamide; the cosolvent B is at least one of lactic acid, pyruvic acid and phytic acid; the solvent is at least one of propylene glycol methyl ether acetate, triethyl citrate and glyceryl triacetate.
The invention also provides the following optimization scheme:
preferably, the diethyl aminoethyl hexanoate is 1% -12%. More preferably, the diethyl aminoethyl hexanoate is 1% -8%. The pH value of the diethyl aminoethyl hexanoate is controlled to be 3.0-5.0, and the active ingredients of the diethyl aminoethyl hexanoate are controlled to be more than 97%.
Preferably, the auxiliary agent is at least one of phenethyl phenol polyoxyethylene ether, alkylphenol polyoxyethylene ether phosphate, phenethyl phenol polyoxyethylene ether phosphate, fatty alcohol polyoxyethylene ether, polyoxyethylene sorbitan fatty acid ester, polyoxyethylene alkylaryl ether and polyoxyalkylene glycol butyl ether.
The invention also provides a preparation method of the liquid preparation for improving the stability of the diethyl aminoethyl hexanoate preparation, which comprises the following steps:
s1, adding a cosolvent A and a cosolvent B into a preparation kettle, and fully stirring; the cosolvent A is at least one of dimethyl sulfoxide and dimethylacetamide; the cosolvent B is at least one of lactic acid, pyruvic acid and phytic acid, preferably dimethyl sulfoxide and pyruvic acid;
s2, adding the diethyl aminoethyl hexanoate raw material into a preparation kettle; fully stirring and dissolving;
s3, adding the weighing auxiliary into a preparation kettle and uniformly stirring; the auxiliary agent is preferably at least one of polyoxyethylene sorbitan fatty acid ester or polyoxyethylene alkyl aryl ether;
s4, putting the solvent into a preparation kettle and uniformly stirring;
s5, pumping the prepared product into a semi-finished product storage tank by using a discharging pump, and thus, the product preparation is completed.
Preferably, in the step S1, the stirring speed is 400rpm-500rpm. The temperature of the solvent in the preparation kettle is controlled between 25 and 40 ℃.
Preferably, in the steps S2-S4, the stirring speed is less than 400rpm. The temperature of the solvent in the preparation kettle is controlled between 35 and 45 ℃.
The beneficial effects of the invention are as follows:
1. the diethyl aminoethyl hexanoate in the liquid preparation for improving the stability of the diethyl aminoethyl hexanoate preparation is stable in content, quick in dissolution and convenient for crops to absorb;
2. the liquid preparation for improving the stability of the diethyl aminoethyl hexanoate preparation can effectively prevent diethyl aminoethyl hexanoate from decomposing and improve the application effect of the liquid preparation;
3. the liquid preparation for improving the stability of the diethyl aminoethyl hexanoate preparation accords with the toxicity evaluation of chemical pesticides, and has no influence on environmental safety.
Drawings
FIG. 1 is a photograph of an experimental yield increase of diethyl aminoethyl hexanoate versus Fuding big white tea according to a preferred embodiment of the present invention;
FIG. 2 is a photograph of an experimental yield increase of diethyl aminoethyl hexanoate versus Fuding big white tea according to a preferred embodiment of the present invention;
FIG. 3 is a photograph showing the yield increase of the diethyl aminoethyl hexanoate to Fuding big white tea according to a preferred embodiment of the present invention;
FIG. 4 is a photograph of a cherry tomato yield increase experiment with diethyl aminoethyl hexanoate according to a preferred embodiment of the present invention;
FIG. 5 is a photograph of a cherry tomato yield increase experiment with diethyl aminoethyl hexanoate according to a preferred embodiment of the present invention;
FIG. 6 is a photograph of a cherry tomato yield increase experiment with diethyl aminoethyl hexanoate in accordance with a preferred embodiment of the present invention;
FIG. 7 shows the result of the gas chromatography of diethyl aminoethyl hexanoate according to a preferred embodiment of the present invention.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments thereof in order to enable those skilled in the art to better understand the technical aspects of the invention.
The invention provides a liquid preparation for improving the stability of an diethyl aminoethyl hexanoate preparation, which comprises 0.1-20% of diethyl aminoethyl hexanoate, 0.1-30% of an auxiliary agent, 1-32% of a solvent and the balance of the solvent to 100%; the cosolvent comprises a cosolvent A and a cosolvent B; the cosolvent A is at least one of dimethyl sulfoxide and dimethylacetamide; the cosolvent B is at least one of lactic acid, pyruvic acid and phytic acid; the solvent is at least one of propylene glycol methyl ether acetate, triethyl citrate and glyceryl triacetate.
The content of the diethyl aminoethyl hexanoate preparation is 1-12%. More preferably, the content of the diethyl aminoethyl hexanoate preparation is 1% -8%. The pH value of the diethyl aminoethyl hexanoate is controlled to be 3.0-5.0, and the active ingredients of the diethyl aminoethyl hexanoate are controlled to be more than 97%.
The diethyl aminoethyl hexanoate is white or light yellow powder, has light ester fragrance and greasy feel, is easily dissolved in water, can be dissolved in polar organic solvents such as ethanol, methanol, acetone and the like, and can be prepared into various dosage forms such as water aqua, soluble agent, soluble powder, tablet and the like. But the diethyl aminoethyl hexanoate is easy to hydrolyze and alcoholyze, and is easy to decompose in water and alcohol, the diethyl aminoethyl hexanoate is a plant growth regulator, and the using method of the diethyl aminoethyl hexanoate is seed soaking or spraying. The most common method is spraying. The dosage and the using method of the diethyl aminoethyl hexanoate have strict requirements, otherwise malformation growth caused by uneven local distribution easily occurs or the usage dosage is insufficient, so that the diethyl aminoethyl hexanoate cannot promote growth, and the diethyl aminoethyl hexanoate needs to be uniformly and effectively distributed on crops. The diethyl aminoethyl hexanoate needs to be prepared into a liquid preparation which is convenient to spray and is homogeneous, and the diethyl aminoethyl hexanoate in the preparation needs to be stable in content, quick in dissolution and convenient for crops to absorb.
The detection problem of the diethyl aminoethyl hexanoate is solved, the detection of the diethyl aminoethyl hexanoate in the diethyl aminoethyl hexanoate citrate is realized by the gas spectrum detection and the liquid spectrum detection at present, and the liquid spectrum detection is low in response value due to the short maximum absorption wavelength, so that the sensitivity of the diethyl aminoethyl hexanoate liquid spectrum detection method is not high, and meanwhile, the diethyl aminoethyl hexanoate and a plurality of acidic substances in the diethyl aminoethyl hexanoate citrate can not be separated in the detection. In order to avoid the influence of the detection method, the diethyl aminoethyl hexanoate preparation needs to be detected by using a gas chromatography method.
Glyceryl triacetate (CAS number 102-76-1) is a colorless odorless liquid. The solubility in water was 64.0g/L, the flash point was 148℃and the saturated vapor pressure was 0.331Pa (temperature: 25 ℃). The property is stable. The glyceryl triacetate has the advantages that the glyceryl triacetate has no forbidden problem, is environment-friendly, has relatively weak polarity, meets the requirement of a soluble agent after being diluted by the soluble agent, has the polarity close to that of the diethyl aminoethyl hexanoate, and is not easy to undergo transesterification in a solvent with the similar polarity.
Triethyl citrate (CAS number 77-93-0) is a colorless odorless liquid. The solubility in water was 57.0g/L, flash point 110℃and saturated vapor pressure 1 mmHg (107 ℃). The property is stable. The method has the advantages that the triethyl citrate has no forbidden use problem, is environment-friendly, has relatively weak polarity, meets the requirement of a soluble agent after being diluted by the soluble agent, has the polarity close to that of the diethyl aminoethyl hexanoate, and is not easy to undergo transesterification in a solvent with the similar polarity.
Propylene glycol methyl ether acetate (CAS number 108-65-6) is a colorless odorless liquid. The solubility in water was 160.0g/L, flash point: 42 ℃, saturated vapor pressure 2.7 mmHg (temperature: 20 ℃ C.). The property is stable. The method has the advantages that the polarity of the diethyl aminoethyl hexanoate is relatively weak, the requirement of the soluble agent is met after the diethyl aminoethyl hexanoate is diluted by the soluble agent, and compared with the diethyl aminoethyl hexanoate, the diethyl aminoethyl hexanoate has the polarity close to that of the diethyl aminoethyl hexanoate, and the diethyl aminoethyl hexanoate is not easy to undergo transesterification in a solvent with the similar polarity.
The cosolvent comprises a cosolvent A and a cosolvent B; the cosolvent A is at least one of dimethyl sulfoxide and dimethylacetamide; the cosolvent B is at least one of lactic acid, pyruvic acid and phytic acid.
Dimethyl sulfoxide and dimethylacetamide are solvents with good dissolving property for diethyl aminoethyl hexanoate, the solubility of diethyl aminoethyl hexanoate is high, meanwhile, the two solvents belong to dipolar aprotic solvents, the molecular cohesion is high, the solvent is stable, and the reaction with diethyl aminoethyl hexanoate is difficult to occur.
The lactic acid, the pyruvic acid and the phytic acid of the cosolvent B are mainly used for accelerating the dissolution of the cosolvent to the raw medicine, when the raw medicine is dissolved by dimethyl sulfoxide and dimethylacetamide, the raw medicine is easy to wrap and agglomerate together, a sealing layer is formed outside the raw medicine to prevent the dissolution of the raw medicine, and after the liquid acid is added into the solvent, the raw medicine is easy to scatter, the dissolution speed is fast, and the whole processing time is shortened.
The auxiliary agent is at least one of phenethyl phenol polyoxyethylene ether, alkylphenol polyoxyethylene ether phosphate, phenethyl phenol polyoxyethylene ether phosphate, fatty alcohol polyoxyethylene ether, polyoxyethylene sorbitan fatty acid ester, polyoxyethylene alkylaryl ether and polyoxyalkylene glycol butyl ether. The auxiliary agents in the invention are esters, ethers and the like, so that the auxiliary agents are not easy to carry out alcoholysis reaction with the diethyl aminoethyl hexanoate, and the diethyl aminoethyl hexanoate and the auxiliary agents are well mixed and are stable. The preparation is a solution, and is clear and transparent after dilution, so that the application range of the preparation technology is wider, the clear and transparent of other raw medicines after dilution is ensured, and the added auxiliary agent has the effects of emulsification and solubilization.
Besides, the addition of the auxiliary agent can also have the functions of increasing the permeability and adhesiveness after the product is diluted and reducing the surface tension, so that the permeability and adhesiveness of the medicament are improved when the product is sprayed and used.
The auxiliary agent, the cosolvent and the solvent are beneficial to the stability of the diethyl aminoethyl hexanoate, the toxicity of the preparation is low after the three are compounded, the preparation is environment-friendly, the cosolvent ensures the quick dissolution of the diethyl aminoethyl hexanoate, the auxiliary agent ensures better permeability and adhesiveness of the product when the diethyl aminoethyl hexanoate is used, better use effect is ensured, and the solvent keeps stable in the preparation due to the weak polarity property of the solvent.
The preparation method of the liquid preparation for improving the stability of the diethyl aminoethyl hexanoate preparation comprises the following steps:
s1, adding a cosolvent A and a cosolvent B into a preparation kettle, and fully stirring; the preferred solvents dimethyl sulfoxide and pyruvic acid are placed in a compounding kettle.
S2, adding the diethyl aminoethyl hexanoate raw material into a preparation kettle, and fully stirring and dissolving;
s3, adding the weighing auxiliary into a preparation kettle and uniformly stirring;
s4, putting the solvent into a preparation kettle, complementing to 100%, and uniformly stirring;
s5, pumping the prepared product into a semi-finished product storage tank by using a discharging pump, and thus, the product preparation is completed.
Preferably, in the step S1, the stirring speed is 400rpm-500rpm. The temperature of the solvent in the preparation kettle is controlled between 25 and 40 ℃.
Preferably, in the steps S2-S4, the stirring speed is less than 400rpm. The temperature of the solvent in the preparation kettle is controlled between 35 and 45 ℃.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
Example 1
Table 1 8% diethyl aminoethyl hexanoate soluble solution
| Raw material name | Proportioning of | Toxicity information, for fish LC50,96h (mg/kg) | Manufacturer information |
| Diethyl aminoethyl hexanoate | 8％ | - | Sichuan Runer Technology Co.,Ltd. |
| Dimethyl sulfoxide | 30％ | ＞35000 | |
| Pyruvic acid | 0.5％ | ＞20 | |
| Polyoxyethylene alkylaryl ethers | 4％ | 710 | Star flying chemical industry |
| Propylene glycol methyl ether acetate | Complement to | 180 | Conventional solvents |
The processing technology comprises the following steps: weighing a cosolvent A dimethyl sulfoxide and a cosolvent B pyruvic acid, putting the weighed diethyl aminoethyl hexanoate raw material into a preparation kettle, putting the weighed diethyl aminoethyl hexanoate raw material into the preparation kettle, adding an auxiliary agent polyoxyethylene alkyl aryl ether, uniformly stirring, supplementing a solvent propylene glycol methyl ether acetate, and controlling the temperature of the solvent in the preparation kettle to be 30-35 ℃ in the whole dissolving process. After the preparation is completed, the finished product is pumped into a semi-finished product storage warehouse.
Toxicity of the formulation: by toxicity analysis of raw materials of the product, the toxicity of the product to the zebra fish is low (see table 2), and the toxicity is low according to the section 12 of the environmental safety evaluation test rule of chemical pesticides of GB/T31270.12-2014: fish acute toxicity test the fish toxicity test is carried out. The preparation according to the above formula is diluted to have the diethyl aminoethyl hexanoate content of 10mg/kg. The toxicity analysis of the remaining raw materials was as follows:
table 2 8% analysis results of toxicity of the diethyl aminoethyl hexanoate as a raw material
| Raw material name | Formulation ratio | The preparation is diluted 8000 times | Toxicity information of raw materials, for fish LC50,96h (mg/kg) | Comparison result |
| Diethyl aminoethyl hexanoate | 8％ | 10ppm | - | |
| Dimethyl sulfoxide | 30％ | 37.5ppm | 35000 | Less than LC50 |
| Pyruvic acid | 0.5％ | 10ppm | ＞20 | Less than LC50 |
| Polyoxyethylene alkylaryl ethers | 4％ | 5ppm | 710 | Less than LC50 |
| Propylene glycol methyl ether acetate | Complement to | 71.25ppm | 180 | Less than LC50 |
After the product is diluted by 800 times, experiments are carried out according to a toxicity experiment method, the final 96-hour fish survival rate is 100%, and the toxicity of the preparation of the final product is low.
Product stability: and carrying out heat storage and normal temperature storage experiments on the diethyl aminoethyl hexanoate according to the storage requirement of the soluble solution, and judging the decomposition condition of the diethyl aminoethyl hexanoate by referring to a detection method gas spectrum detection method of the diethyl aminoethyl hexanoate original drug, detecting the content of the diethyl aminoethyl hexanoate. The specific decomposition conditions are shown in Table 3 and FIG. 7.
Table 3 8% evaluation of storage stability of the diethyl aminoethyl hexanoate soluble product
Table 4 8% analysis results of storage stability of the diethyl aminoethyl hexanoate aqueous solution
Example one conclusion:
as shown in fig. 7, the first gas spectrogram of fig. 7 is a 2-year storage spectrogram of 8% diethyl aminoethyl hexanoate soluble solution at normal temperature, the second gas spectrogram is a 14-day storage spectrogram of 8% diethyl aminoethyl hexanoate soluble solution at normal temperature, the third gas spectrogram is a 1-year storage spectrogram of 8% diethyl aminoethyl hexanoate aqueous solution at normal temperature, the fourth gas spectrogram is a 14-day storage spectrogram of 8% diethyl aminoethyl hexanoate aqueous solution heat storage (54 ℃) and the fifth gas spectrogram is a diethyl aminoethyl hexanoate standard spectrogram.
Through toxicity experiments and storage experiments on 8% diethyl aminoethyl hexanoate soluble solution, the 8% diethyl aminoethyl hexanoate soluble solution has low toxicity, meets registration requirements, and uses solvents in environmental protection. The product has good stability, and the decomposition rate of the diethyl aminoethyl hexanoate in the heat storage and normal temperature storage processes is low, thereby meeting the registration requirements.
Example two
12% diethyl aminoethyl hexanoate soluble solution
TABLE 4 12% diethyl aminoethyl hexanoate soluble solution
| Raw material name | Proportioning of | Toxicity information, for fish LC50,96h (mg/kg) | Manufacturer information |
| Diethyl aminoethyl hexanoate | 12％ | - | Sichuan Runer Technology Co.,Ltd. |
| Lactic acid | 0.5％ | 130 | |
| Dimethyl sulfoxide | 30％ | ＞35000 | Conventional solvents |
| Polyoxyethylene sorbitan fatty acid ester | 20％ | 1000 | CORDA |
| Glyceryl triacetate | Complement to | 100 | Conventional solvents |
The processing technology comprises the following steps: weighing a cosolvent A dimethyl sulfoxide and a cosolvent B lactic acid, putting the obtained diethyl aminoethyl hexanoate raw material into a preparation kettle, putting the obtained diethyl aminoethyl hexanoate raw material into the preparation kettle, adding an auxiliary agent polyoxyethylene sorbitan fatty acid ester, uniformly stirring, supplementing the solvent glyceryl triacetate, and controlling the temperature of the solvent in the preparation kettle to be 30-35 ℃ in the whole dissolving process. After the preparation is completed, the semi-finished product is pumped into a semi-finished product storage warehouse.
Toxicity of the formulation: by toxicity analysis of the raw materials of the product, the toxicity of the product is low (see Table 5), and the toxicity is low according to the section 12 of the environmental safety evaluation test rule of chemical pesticides of GB/T31270.12-2014: fish acute toxicity test the fish toxicity test is carried out. The preparation according to the formula is diluted to have the original drug content of 15mg/kg. The toxicity analysis of the remaining raw materials was as follows:
TABLE 5 toxicity analysis results of 12% diethyl aminoethyl hexanoate soluble solution raw materials
The product is diluted 8000 times and then is tested according to a toxicity test method, the final 96-hour fish survival rate is 100%, and the toxicity of the final product preparation is low.
Product stability: the 12% diethyl aminoethyl hexanoate soluble solution is subjected to heat storage and normal temperature storage experiments according to the storage requirement of the soluble solution, and the content of diethyl aminoethyl hexanoate is detected by referring to the detection method gas spectrum detection method of the diethyl aminoethyl hexanoate original drug, so as to judge the decomposition condition of diethyl aminoethyl hexanoate. Specific decomposition conditions (see Table 6).
TABLE 6 analysis of storage stability of 12% diethyl aminoethyl hexanoate soluble product
Conclusion of example two: by carrying out fish toxicity experiments and product storage experiments on the 12% diethyl aminoethyl hexanoate soluble solution, the product toxicity is low and the decomposition rate of diethyl aminoethyl hexanoate is low.
Example III
10% diethyl aminoethyl hexanoate soluble solution
TABLE 7 10% diethyl aminoethyl hexanoate solubles
The processing technology comprises the following steps: weighing a cosolvent A dimethylacetamide and a cosolvent B phytic acid, putting the obtained mixture into a preparation kettle, weighing an diethyl aminoethyl hexanoate raw material, putting the obtained mixture into the preparation kettle, adding an auxiliary agent polyoxyethylene sorbitan fatty acid ester, uniformly stirring, supplementing a solvent propylene glycol methyl ether acetate, controlling the temperature of the solvent in the preparation kettle to be 30-35 ℃ in the whole dissolving process, and pumping the semi-finished product into a semi-finished product storage tank after the preparation is completed.
Toxicity of the formulation: through toxicity analysis of raw materials of the product, the toxicity of the product is low (see Table 8), and the toxicity is low according to the section 12 of the environmental safety evaluation test criterion of chemical pesticides of GB/T31270.12-2014: fish acute toxicity test the fish toxicity test is carried out. The preparation according to the above formula is diluted to have the diethyl aminoethyl hexanoate content of 10mg/kg. The toxicity analysis of the remaining raw materials was as follows:
TABLE 8 toxicity analysis results of 10% diethyl aminoethyl hexanoate soluble solution raw materials
After the product is diluted 10000 times, experiments are carried out according to a toxicity experiment method, the final 96-hour fish survival rate is 100%, and the toxicity of the preparation of the final product is low.
Product stability: and (3) carrying out heat storage and normal temperature storage experiments on the 10% diethyl aminoethyl hexanoate soluble solution according to the storage requirement of the soluble solution, and determining the decomposition condition of diethyl aminoethyl hexanoate by referring to a detection method gas spectrum detection method of diethyl aminoethyl hexanoate original drug. Specific decomposition conditions (see Table 9).
TABLE 9 analysis of 10% diethyl aminoethyl hexanoate soluble product storage stability
Conclusion of example three: by carrying out fish toxicity experiments and product storage experiments on 10% diethyl aminoethyl hexanoate soluble solution, the product toxicity is low and the decomposition rate of diethyl aminoethyl hexanoate is low. The stability of the diethyl aminoethyl hexanoate is still better. Solves the problem of poor stability of the diethyl aminoethyl hexanoate preparation.
Example IV
According to the using method of the regulator in pesticide field efficacy test criterion GB/T17980, an efficacy test is carried out on the 8% diethyl aminoethyl hexanoate soluble solution in the first embodiment. Meanwhile, a comparison group of 8% diethyl aminoethyl hexanoate aqueous solution is arranged, the 8% diethyl aminoethyl hexanoate aqueous solution is the same as an auxiliary agent and a cosolvent used in the 8% diethyl aminoethyl hexanoate soluble solution, and clear water is used for replacing the solvent to complement the solvent. The specific implementation mode is as follows:
and (3) medicament treatment: the 8% diethyl aminoethyl hexanoate solution (solvent complement) of the medicament is named A1, the 8% diethyl aminoethyl hexanoate solution (purified water complement) of the medicament is named A2, and the two preparations are stored for half a year at normal temperature for use.
The experimental object: in the spring tea stage of Fuding big white tea, a tea garden with a flat land is selected, and tea rows with the same variety, tree age and tree form (photo) are selected.
Experimental action: regulating growth and increasing yield
Experiment setting: the test is carried out by setting 2 medication treatments and 1 clear water control, repeating each treatment for 4 times, marking the same area size of the cells as 6 square meters, and randomly selecting 1 area with the area of 50cm multiplied by 40cm as a photographic observation point in each cell.
The using method comprises the following steps: the 8% diethyl aminoethyl hexanoate can be diluted by 5000 times, and the liquid medicine is prepared in strict compliance with the concentration designed by the test and is uniformly sprayed.
Investigation indexes:
A. safety (whether tea buds are inhibited from growing normally or not and whether leaf yellowing and scorching occur or not is observed by naked eyes).
B. Bud count (3 points were randomly selected for investigation per treatment, the investigation area per point was 0.2 square meter, total 0.6 square meter tea leaf bud count)
C. Single bud weight (single bud weight = cell yield/cell bud number)
D. District yield (weighing 1 bud 1 leaf weight per treatment 0.6 square meter using an electronic scale)
Table 10 design list of efficacy test of 8% diethyl aminoethyl hexanoate
Table 11 results of yield increase of 8% diethyl aminoethyl hexanoate on Fuding Dabai tea
Conclusion of example four:
drug effect: according to the concentration of the product preparation, a dilution experiment is carried out on the product, wherein in the experiment, 8% of diethyl aminoethyl hexanoate aqueous solution and diethyl aminoethyl hexanoate soluble solution in the first embodiment are shown in fig. 1, 1 in the A1 group is the initial growth condition of Fuding white tea, 2 is the growth condition of Fuding white tea after spraying A1 for 8 days, and 3 is the growth condition after 16 days. 4 is the growth after 24 days. As shown in fig. 2, group A1 is the initial growth condition of the fuding white tea, 2 is the growth condition of the fuding white tea after spraying group A2 for 8 days, and 3 is the growth condition after spraying group 16 days. 4 is the growth after 24 days. As shown in fig. 3, CK group 1 is the initial growth condition of fuding white tea, 2 is the growth condition of fuding white tea after spraying CK for 8 days, and 3 is the growth condition after spraying CK for 16 days. 4 is the growth after 24 days.
Compared with the same concentration, the diethyl aminoethyl hexanoate soluble solution in the first embodiment has promotion effect on germination density and single bud of Fuding big white tea under the same concentration, thereby promoting the improvement of the whole yield of the tea.
And (3) reason analysis: the 8% diethyl aminoethyl hexanoate solution A1 can still ensure lower diethyl aminoethyl hexanoate decomposition rate after being stored for half a year at normal temperature because the diethyl aminoethyl hexanoate in the product is stable, so that the expected effect of the diethyl aminoethyl hexanoate can be achieved. 8% of the diethyl aminoethyl hexanoate aqueous agent A2 is unstable in water, so that the diethyl aminoethyl hexanoate is decomposed after being stored for half a year at normal temperature, and the expected effect cannot be achieved.
Example five
According to the using method of the regulator in pesticide field efficacy test criterion GB/T17980, 2% diethyl aminoethyl hexanoate aqueous solution is directly purchased in the market, and 2% diethyl aminoethyl hexanoate soluble solution is prepared according to the method in the invention, so that efficacy comparison is carried out.
The experimental object: cherry tomatoes (millennium) are cultivated by adopting plastic film mulching ridging, the plant row spacing is 45cm, 50cm, the ridge width is 90cm, and the ridge spacing is 50cm. The management level of the growers is good, the tomato stems are thick, the leaves are thick green and thick, the tomato leaves are glossy, and the tomato leaves are free of plant diseases and insect pests.
The function is as follows: regulating growth and increasing yield
Experiment setting: in the experiment, 2 medication treatments and 1 clear water control are set, 1 ridge is selected as an experimental object in each treatment, and 1 tomato is randomly selected as a photographing observation point in each treatment.
The using method comprises the following steps: the 2% diethyl aminoethyl hexanoate soluble agent and the 2% diethyl aminoethyl hexanoate water agent are diluted 1000 times, and the preparation is applied once in tomato seedling stage and bud stage, and is sprayed uniformly.
Test agent: 2% diethyl aminoethyl hexanoate soluble solution, labeled treatment one in the experiment
Contrast agent: 2% diethyl aminoethyl hexanoate aqua (commercially available) labeled treatment two in the experiment
Control agent: clear water, set as a blank control group, labeled CK in the experiment
Table 12 results of experiments on the efficacy of 2% diethyl aminoethyl hexanoate on millennium tomato
| Treatment of | Fruit setting quantity | Growth rate (%) | Total flowering number | Growth rate (%) | Cell yield, kg | Yield increase (%) |
| Process one | 8.3 | 18.57 | 9.2 | 15 | 759.35 | 16.11 |
| Treatment two | 7.6 | 8.57 | 8.7 | 8.75 | 687.68 | 5.15 |
| Control | 7 | — | 8 | — | 653.97 | — |
Conclusions of example five:
as shown in fig. 4-6, fig. 4 is a graph of the results of picking cherry tomato treatment one, fig. 5 is a graph of the results of picking cherry tomato treatment two, and fig. 6 is a graph of the results of picking cherry tomato control group.
From the experimental results, the 2% diethyl aminoethyl hexanoate soluble agent and the 2% diethyl aminoethyl hexanoate aqueous agent have larger difference in tomato yield increase effect under the same concentration, and the diethyl aminoethyl hexanoate soluble agent has more excellent effects on flower preservation, fruit preservation and yield increase of tomatoes.
The foregoing is merely a preferred embodiment of the present invention, and it should be noted that the above-mentioned preferred embodiment should not be construed as limiting the invention, and the scope of the invention should be 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 such modifications and adaptations are intended to be comprehended within the scope of the invention.
Claims (1)
1. A liquid formulation for improving stability of an diethyl aminoethyl hexanoate formulation, comprising: according to the mass percentage, the composition comprises 8% of diethyl aminoethyl hexanoate, 4% of auxiliary agent, 30.5% of cosolvent and 100% of solvent; the cosolvent comprises a cosolvent A and a cosolvent B; the cosolvent A is dimethyl sulfoxide; the cosolvent B is pyruvic acid; the solvent is propylene glycol methyl ether acetate; the dimethyl sulfoxide content is 30%; the pyruvic acid content is 0.5%; the auxiliary agent is polyoxyethylene alkyl aryl ether, the content of the diethyl aminoethyl hexanoate in the diethyl aminoethyl hexanoate liquid preparation is detected by a gas chromatography method, and the detected change rate of the diethyl aminoethyl hexanoate is less than 1.375%.
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