CN112889823A - 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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- CN112889823A CN112889823A CN202110083911.5A CN202110083911A CN112889823A CN 112889823 A CN112889823 A CN 112889823A CN 202110083911 A CN202110083911 A CN 202110083911A CN 112889823 A CN112889823 A CN 112889823A
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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 159
- 238000002360 preparation method Methods 0.000 title claims abstract description 93
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- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims abstract description 33
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Images
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
A liquid preparation for improving the stability of a diethyl aminoethyl hexanoate preparation comprises 0.1 to 20 percent of diethyl aminoethyl hexanoate, 0.1 to 30 percent of auxiliary agent, 1 to 32 percent of dissolution promoter and the balance of solvent to 100 percent by mass percent; 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 triacetin. The liquid preparation for improving the stability of the diethyl aminoethyl hexanoate preparation can effectively prevent the diethyl aminoethyl hexanoate from being decomposed 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 diethyl aminoethyl hexanoate and a preparation method thereof.
Background
Diethylaminoethanol hexanoate citrate (diethyl aminoethyl hexanoate), also known as diethyl aminoethyl hexanoate (DA-6), is referred to herein as diethylaminoethanol hexanoate citrate. Diethyl aminoethyl hexanoate is a high-energy plant growth regulator with broad-spectrum and breakthrough effect. It can raise the content of chlorophyll, protein and nucleic acid in plant body and photosynthetic rate, raise the activity of peroxidase and nitrate reductase, promote the carbon and nitrogen metabolism of plant, enhance the absorption of plant to water and fertilizer and the accumulation of dry matter, regulate the water balance in plant body, raise the disease resistance, drought resistance and cold resistance of crops and fruit trees, delay the senility of plant, promote the early maturing and yield increasing of crops and raise the quality of crops so as to raise yield, quality and value.
The diethyl aminoethyl hexanoate is white or light yellow powder, has light ester fragrance and greasy feeling, is easy to dissolve 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 aqua, soluble liquid, soluble powder, tablets 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 method for overcoming the defects in the prior art.
The invention firstly provides a liquid preparation for improving the stability of diethyl aminoethyl hexanoate, which comprises 0.1 to 20 percent of diethyl aminoethyl hexanoate, 0.1 to 30 percent of auxiliary agent, 1 to 32 percent of dissolution promoter and the balance of solvent to 100 percent by mass percent; 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 triacetin.
The invention also provides the following optimization scheme:
preferably, the content of the diethyl aminoethyl hexanoate is 1% -12%. More preferably, the diethyl aminoethyl hexanoate is 1% to 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 phosphate, phenethyl phenol polyoxyethylene ether phosphate, fatty alcohol polyoxyethylene ether, polyoxyethylene sorbitan fatty acid ester, polyoxyethylene alkyl aryl 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 the dissolution accelerator A and the dissolution accelerator B into the 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, and is preferably dimethyl sulfoxide and pyruvic acid;
s2, adding the diethyl aminoethyl hexanoate raw medicine into a preparation kettle; fully stirring and dissolving;
s3, adding the weighed auxiliary agent 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 discharge pump, and finishing the product preparation.
Preferably, in the step S1, the stirring speed is 400rpm to 500 rpm. The temperature of the solvent in the preparation kettle is controlled at 25-40 ℃.
Preferably, in the step S2-S4, the stirring speed is less than 400 rpm. The temperature of the solvent in the preparation kettle is controlled to be 35-45 ℃.
The invention has the beneficial effects that:
1. the content of diethyl aminoethyl hexanoate in the liquid preparation for improving the stability of the diethyl aminoethyl hexanoate preparation is stable, the diethyl aminoethyl hexanoate is dissolved quickly and is convenient for crops to absorb;
2. the liquid preparation for improving the stability of the diethyl aminoethyl hexanoate preparation can effectively prevent the diethyl aminoethyl hexanoate from being decomposed and improve the application effect of the liquid preparation;
3. the liquid preparation for improving the stability of the diethyl aminoethyl hexanoate preparation conforms to the toxicity evaluation of chemical pesticides and has no influence on environmental safety.
Drawings
FIG. 1 is a photograph of a yield increase experiment of diethyl aminoethyl hexanoate on Fuding white tea according to a preferred embodiment of the present invention;
FIG. 2 is a photograph of a yield increase experiment of diethyl aminoethyl hexanoate on Fuding white tea according to a preferred embodiment of the present invention;
FIG. 3 is a photograph of a yield increase experiment of diethyl aminoethyl hexanoate on Fuding white tea according to a preferred embodiment of the present invention;
FIG. 4 is a photograph of an experiment of increasing yield of cherry tomatoes by diethyl aminoethyl hexanoate in accordance with a preferred embodiment of the present invention;
FIG. 5 is a photograph of an experiment of increasing yield of cherry tomatoes with diethyl aminoethyl hexanoate in accordance with a preferred embodiment of the present invention;
FIG. 6 is a photograph of an experiment of increasing yield of cherry tomatoes with diethyl aminoethyl hexanoate in accordance with a preferred embodiment of the present invention;
FIG. 7 shows the result of the detection of diethyl aminoethyl hexanoate by gas chromatography according to a preferred embodiment of the present invention.
Detailed Description
In order that those skilled in the art will better understand the technical solutions of the present invention, the present invention will be further described in detail with reference to the following embodiments.
The invention firstly provides a liquid preparation for improving the stability of diethyl aminoethyl hexanoate, which comprises 0.1 to 20 percent of diethyl aminoethyl hexanoate, 0.1 to 30 percent of auxiliary agent, 1 to 32 percent of dissolution promoter and the balance of solvent to 100 percent by mass percent; 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 triacetin.
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 feeling, is easy to dissolve 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 aqua, soluble liquid, soluble powder, tablets and the like. But the diethyl aminoethyl hexanoate is very easy to hydrolyze and alcoholyze and is very easy to decompose in water and alcohol, the diethyl aminoethyl hexanoate is a plant growth regulator, and the application method of the diethyl aminoethyl hexanoate is seed soaking or spraying. The most common method is spraying. The dosage and the use method of the diethyl aminoethyl hexanoate have strict requirements, otherwise, the diethyl aminoethyl hexanoate is easy to grow abnormally due to local uneven distribution or the insufficient dosage can not play a role in promoting the growth, and the diethyl aminoethyl hexanoate needs to be uniformly and effectively distributed on crops. The requirement is that the diethyl aminoethyl hexanoate needs to be prepared into a liquid preparation which is convenient to spray and has homogeneous phase, and the content of the diethyl aminoethyl hexanoate in the preparation needs to be stable, the diethyl aminoethyl hexanoate can be dissolved quickly and is convenient for crops to absorb.
The detection problem of diethyl aminoethyl hexanoate in diethyl aminoethyl hexanoate citrate is that the detection of diethyl aminoethyl hexanoate in diethyl aminoethyl hexanoate citrate cannot be separated from a plurality of acidic substances in diethyl aminoethyl hexanoate citrate at the same time. In order to avoid the influence of a detection method, the diethyl aminoethyl hexanoate preparation needs to be detected by using a gas chromatography.
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 method has the advantages that the glyceryl triacetate has no forbidden use problem, is environment-friendly, has relatively weak polarity, meets the requirements of a soluble agent after being diluted by the soluble agent, and has similar polarity compared with diethyl aminoethyl hexanoate, and the diethyl aminoethyl hexanoate is not easy to generate ester exchange reaction in solvents with similar polarity.
Triethyl citrate, (CAS number 77-93-0) is a colorless, odorless liquid. The solubility in water was 57.0g/L, the flash point: 110 ℃ and the saturated vapor pressure 1mm Hg (107 ℃ C.). The property is stable. The triethyl citrate 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, and has close polarity compared with diethyl aminoethyl hexanoate, and the diethyl aminoethyl hexanoate is not easy to generate ester exchange reaction in solvents with 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, the flash point was 42 ℃ and the saturated vapor pressure was 2.7mm Hg (temperature: 20 ℃). The property is stable. The method has the advantages that the polarity is relatively weak, the requirements of the soluble agent are met after the soluble agent is diluted, and compared with diethyl aminoethyl hexanoate, the polarity of the diethyl aminoethyl hexanoate is close, and diethyl aminoethyl hexanoate is not easy to generate ester exchange reaction in solvents with similar polarities.
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 good solvents for dissolving diethyl aminoethyl hexanoate, have high solubility to diethyl aminoethyl hexanoate, belong to dipolar aprotic solvents, have high molecular cohesion and are stable, and are not easy to react with diethyl aminoethyl hexanoate.
The lactic acid, pyruvic acid and phytic acid of the dissolution accelerator B are mainly used for accelerating the dissolution of the dissolution accelerator B on a technical material, the technical material is easy to wrap and agglomerate together when dimethyl sulfoxide and dimethylacetamide dissolve the technical material, a sealing layer is formed outside the technical material to hinder the dissolution of the technical material, and after liquid acid is added into the solvent, the technical material is easy to disperse, the dissolution speed is high, and the whole processing time is shortened.
The auxiliary agent is at least one of phenethyl phenol polyoxyethylene ether, alkylphenol polyoxyethylene phosphate, phenethyl phenol polyoxyethylene ether phosphate, fatty alcohol polyoxyethylene ether, polyoxyethylene sorbitan fatty acid ester, polyoxyethylene alkyl aryl ether and polyoxyalkylene glycol butyl ether. The auxiliaries in the invention are ester, ether and the like, the auxiliaries are not easy to generate alcoholysis reaction with diethyl aminoethyl hexanoate, and diethyl aminoethyl hexanoate and the auxiliaries are well mixed and relatively stable. The preparation is soluble liquid, is clear and transparent liquid after being diluted, ensures that other raw medicines are clear after being diluted in order to widen the application range of the preparation technology, and has the effects of emulsification and solubilization by adding the auxiliary agents.
In addition, the addition of the auxiliary agent can also increase the permeability and the adhesiveness of the product after dilution and reduce the surface tension, so that the permeability and the adhesiveness of the medicament are improved when the product is sprayed for use.
The auxiliary agent, the dissolution promoter and the solvent are all beneficial to the stability of the diethyl aminoethyl hexanoate, after the three are compounded, the toxicity of the preparation is low, the preparation is environment-friendly, the dissolution promoter ensures the quick dissolution of the diethyl aminoethyl hexanoate, the auxiliary agent ensures that the product has better permeability and adhesiveness when in use, and better use effect is ensured, and the diethyl aminoethyl hexanoate is kept stable in the preparation due to the weak polarity 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 the dissolution accelerator A and the dissolution accelerator B into the preparation kettle, and fully stirring; the preferred solvents, dimethyl sulfoxide and pyruvic acid, are charged into a formulation kettle.
S2, adding the diethyl aminoethyl hexanoate raw drug into a preparation kettle, and fully stirring for dissolving;
s3, adding the weighed auxiliary agent into a preparation kettle and uniformly stirring;
s4, adding the solvent into the preparation kettle, complementing the solvent to 100% and uniformly stirring;
s5, pumping the prepared product into a semi-finished product storage tank by using a discharge pump, and finishing the product preparation.
Preferably, in the step S1, the stirring speed is 400rpm to 500 rpm. The temperature of the solvent in the preparation kettle is controlled at 25-40 ℃.
Preferably, in the step S2-S4, the stirring speed is less than 400 rpm. The temperature of the solvent in the preparation kettle is controlled to be 35-45 ℃.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
Example one
TABLE 18% diethyl aminoethyl hexanoate solubles
| Name of raw materials | Proportioning | Toxicity information on 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 | |
| |
4％ | 710 | Chemical engineering of star fly |
| Propylene glycol methyl ether acetate | Complement | 180 | Conventional solvents |
The processing technology comprises the following steps: weighing a promoter A dimethyl sulfoxide and a promoter B pyruvic acid, putting the promoter A dimethyl sulfoxide and the promoter B pyruvic acid into a preparation kettle, weighing a diethyl aminoethyl hexanoate original drug, putting the diethyl aminoethyl hexanoate original drug into the preparation kettle, adding an auxiliary agent polyoxyethylene alkyl aryl ether, uniformly stirring, complementing 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. And pumping the finished product into a semi-finished product storage after the preparation is finished.
Preparation toxicity: through the toxicity analysis of raw materials of the product, the toxicity of the product to the zebra fish is low (see table 2), and according to the GB/T31270.12-2014 environmental safety evaluation test criterion, part 12: acute toxicity test of fish the toxicity test of fish was carried out. The preparation according to the formula is diluted to have the content of diethyl aminoethyl hexanoate of 10 mg/kg. The toxicity of the remaining raw materials was analyzed as follows:
TABLE 28% raw material toxicity analysis results of diethyl aminoethyl hexanoate solubles
| Name of raw materials | Formula proportion | The preparation is diluted 8000 times in concentration | Toxicity information on raw materials, for fish LC50,96h (mg/kg) | Comparison results |
| Diethyl aminoethyl hexanoate | 8％ | 10ppm | - | |
| Dimethyl sulfoxide | 30％ | 37.5ppm | 35000 | Smaller than LC50 |
| Pyruvic acid | 0.5％ | 10ppm | ＞20 | Smaller than LC50 |
| |
4％ | 5ppm | 710 | Smaller than LC50 |
| Propylene glycol methyl ether acetate | Complement | 71.25ppm | 180 | Smaller than LC50 |
After the product is diluted by 800 times, experiments are carried out according to a toxicity experiment method, the survival rate of the fish in 96 hours is 100 percent, and the preparation toxicity of the final product is low.
Product stability: and (3) carrying out hot storage and normal-temperature storage experiments on the diethyl aminoethyl hexanoate according to the storage requirement of the soluble agent, detecting the content of the diethyl aminoethyl hexanoate by referring to a detection method of a diethyl aminoethyl hexanoate technical product, and judging the decomposition condition of the diethyl aminoethyl hexanoate. The specific decomposition is shown in Table 3 and FIG. 7.
TABLE 38% diethyl aminoethyl hexanoate soluble product storage stability analysis results
TABLE 48% diethyl aminoethyl hexanoate aqueous product storage stability analysis results
In a conclusion of the examples:
as shown in the attached figure 7, a first spectrogram of the attached figure 7 is a normal-temperature 2-year storage spectrogram of 8% diethyl aminoethyl hexanoate soluble liquid, a second spectrogram is a normal-temperature 14-day storage spectrogram of 8% diethyl aminoethyl hexanoate soluble liquid, a third spectrogram is a normal-temperature 1-year storage spectrogram of 8% diethyl aminoethyl hexanoate aqueous liquid, a fourth spectrogram is a heat storage spectrogram of 8% diethyl aminoethyl hexanoate aqueous liquid (54 ℃) for 14 days, and a fifth spectrogram is a chromatogram of diethyl aminoethyl hexanoate standard substance.
Through toxicity experiments and storage experiments on the 8% diethyl aminoethyl hexanoate soluble agent, the 8% diethyl aminoethyl hexanoate soluble agent has low toxicity, meets the registration requirements, and uses an environment-friendly solvent. The product has good stability, the decomposition rate of the diethyl aminoethyl hexanoate in the processes of hot storage and normal-temperature storage is low, and the registered requirement is met.
Example two
12% diethyl aminoethyl hexanoate solution
TABLE 412% diethyl aminoethyl hexanoate solution
| Name of raw materials | Proportioning | Toxicity information on 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 |
| Glycerol triacetate | Complement | 100 | Conventional solvents |
The processing technology comprises the following steps: weighing a promoter A dimethyl sulfoxide and a promoter B lactic acid, putting the dimethyl sulfoxide and the promoter B lactic acid into a preparation kettle, weighing a diethyl aminoethyl hexanoate raw drug, putting the diethyl aminoethyl hexanoate raw drug into the preparation kettle, adding an auxiliary agent polyoxyethylene sorbitan fatty acid ester, uniformly stirring, complementing a solvent glyceryl triacetate, and 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 after the preparation is finished.
Preparation toxicity: through the toxicity analysis of raw materials of the product, the toxicity of the product is low (see table 5), and according to the GB/T31270.12-2014 test rule of environmental safety evaluation of chemical pesticides, part 12: acute toxicity test of fish the toxicity test of fish was carried out. The preparation according to the formula is diluted to have the original medicine content of 15 mg/kg. The toxicity of the remaining raw materials was analyzed as follows:
TABLE 512% raw material toxicity analysis result of diethyl aminoethyl hexanoate soluble agent
The product is diluted 8000 times and tested according to toxicity test method, the survival rate of fish in 96h is 100%, and the toxicity of the final product is low.
Product stability: the 12% diethyl aminoethyl hexanoate soluble solution is subjected to hot storage and normal-temperature storage experiments according to the storage requirement of the soluble solution, the content of diethyl aminoethyl hexanoate is detected by referring to a detection method of diethyl aminoethyl hexanoate raw drug, and the decomposition condition of diethyl aminoethyl hexanoate is judged. The decomposition conditions were specified (see table 6).
TABLE 612% Aminodiethyl Ethanolate soluble solution product storage stability analysis results
Conclusion in example two: by carrying out fish toxicity experiments and product storage experiments on the 12% diethyl aminoethyl hexanoate soluble solution, the product has low toxicity and low decomposition rate of diethyl aminoethyl hexanoate.
EXAMPLE III
10% diethyl aminoethyl hexanoate solution
TABLE 710% diethyl aminoethyl hexanoate solubles
The processing technology comprises the following steps: weighing a promoter A dimethylacetamide and a promoter B phytic acid, putting the raw diethyl aminoethyl hexanoate into a preparation kettle, adding an auxiliary agent polyoxyethylene sorbitan fatty acid ester, uniformly stirring, complementing a solvent propylene glycol monomethyl ether acetate, controlling the temperature of the solvent in the preparation kettle to be 30-35 ℃ in the whole dissolving process, and pumping a semi-finished product into a semi-finished product storage tank after the preparation is finished.
Preparation toxicity: through the toxicity analysis of raw materials of the product, the toxicity of the product is low (see table 8), and according to the GB/T31270.12-2014 test rule of environmental safety evaluation of chemical pesticides, part 12: acute toxicity test of fish the toxicity test of fish was carried out. The preparation according to the formula is diluted to have the content of diethyl aminoethyl hexanoate of 10 mg/kg. The toxicity of the remaining raw materials was analyzed as follows:
TABLE 810% raw material toxicity analysis of diethyl aminoethyl hexanoate solution
After the product is diluted by 10000 times, experiments are carried out according to a toxicity experiment method, the survival rate of the fish for 96 hours is 100 percent, and the preparation toxicity of the final product is low.
Product stability: and (3) carrying out hot storage and normal-temperature storage experiments on the 10% diethyl aminoethyl hexanoate soluble solution according to the storage requirement of the soluble solution, detecting the content of diethyl aminoethyl hexanoate by referring to a detection method of diethyl aminoethyl hexanoate raw drug by a gas spectrum detection method, and judging the decomposition condition of the diethyl aminoethyl hexanoate. The decomposition was detailed (see table 9).
TABLE 910% assay of the storage stability of the diethyl aminoethyl hexanoate soluble product
Example iii theory: by carrying out fish toxicity experiments and product storage experiments on the 10% diethyl aminoethyl hexanoate soluble solution, the product has low toxicity and low decomposition rate of diethyl aminoethyl hexanoate. The stability of diethyl aminoethyl hexanoate was still good. Solves the problem of poor stability of the diethyl aminoethyl hexanoate preparation.
Example four
The pesticide effect experiment of the 8% diethyl aminoethyl hexanoate soluble agent in the first example is carried out according to the using method of the regulator in the pesticide field pesticide effect test rule GB/T17980. Meanwhile, a comparison group of 8% diethyl aminoethyl hexanoate aqueous solution is set, the auxiliary agent and the cosolvent used in the 8% diethyl aminoethyl hexanoate aqueous solution and the 8% diethyl aminoethyl hexanoate soluble solution are the same, and the solvent is replaced by clear water for complement. The specific implementation mode is as follows:
medicament treatment: the preparation 8% diethyl aminoethyl hexanoate soluble solution (solvent complement) is named as A1, the preparation 8% diethyl aminoethyl hexanoate aqueous solution (purified water complement) is named as A2, and the two preparations are stored at normal temperature for half a year for use.
Subject: in the spring tea period of the Fuding white tea, a tea garden with flat land is selected, and tea rows with the same variety and basically consistent tree age and tree shape (pictures) are selected.
The experimental effect is as follows: regulating growth and increasing yield
Experimental setup: the test is carried out by setting 2 medicine treatments and 1 clear water for comparison, repeating each treatment for 4 times, marking the same area of each cell as 6 square meters, and randomly selecting 1 area of 50cm multiplied by 40cm as a photographic observation point for each cell.
The using method comprises the following steps: 8% diethyl aminoethyl hexanoate soluble solution is diluted by 5000 times, and liquid medicine is prepared according to the concentration strictly conforming to the experimental design and is sprayed evenly.
Survey indexes are as follows:
A. safety (whether the normal growth of tea buds is inhibited or not, whether the yellowing and scorching of leaves occur or not is observed by naked eyes).
B. The number of sprouts (every treatment randomly selects 3 points to investigate, each point investigates the area of 0.2 square meter, surveys the sprout number of 0.6 square meter tea compartment surface altogether)
C. Single bud weight (cell yield/number of sprouts)
D. Cell output (using electronic scale to weigh each 0.6 square meter, 1 bud and 1 leaf weight)
TABLE 108% Aminodiethyl ester design of drug efficacy test
Yield increasing result of Table 118% diethyl aminoethyl hexanoate on Fuding white tea
Example four conclusions:
the drug effect is as follows: according to the concentration of the prepared product, the product is diluted, and in the experiment, 8% of diethyl aminoethyl hexanoate aqueous solution and diethyl aminoethyl hexanoate soluble solution in the first example, as shown in figure 1, 1 of group A1 is the growth condition of original Foding white tea, 2 is the growth condition of Foding white tea after 8 days after spraying A1, and 3 is the growth condition after 16 days. And 4 is the growth status after 24 days. As shown in fig. 2, 1 in group a1 is the initial growth condition of fuding white tea, 2 is the growth condition of fuding white tea 8 days after spraying a2, and 3 is the growth condition of tea 16 days after spraying. And 4 is the growth status 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 8 days after CK spraying, and 3 is the growth condition of the tea 16 days after CK spraying. And 4 is the growth status after 24 days.
Compared with the same concentration, the diethyl aminoethyl hexanoate soluble solution in the first embodiment has the function of promoting the sprouting density and single sprout of the Fuding white tea at the same concentration, thereby promoting the improvement of the whole yield of the tea.
Reason analysis: the 8% diethyl aminoethyl hexanoate soluble solution A1 can still ensure that the decomposition rate of diethyl aminoethyl hexanoate is low after the diethyl aminoethyl hexanoate is stored at normal temperature for half a year because the diethyl aminoethyl hexanoate in the product is stable, thereby achieving the expected effect of the diethyl aminoethyl hexanoate. The 8% diethyl aminoethyl hexanoate aqua A2 is unstable in water, so that diethyl aminoethyl hexanoate is decomposed after being stored at normal temperature for half a year, and the expected effect cannot be achieved.
EXAMPLE five
According to the using method of the regulator in the pesticide field efficacy test criterion GB/T17980, 2% diethyl aminoethyl hexanoate water agent is directly purchased from the market and 2% diethyl aminoethyl hexanoate soluble solution is prepared according to the method of the invention, and the efficacy is compared.
Subject: cherry tomatoes (millennium) are cultivated by mulching film mulching and ridging, the plant row spacing is 45cm by 50cm, the ridge width is 90cm, and the ridge spacing is 50 cm. The management level of the planters is good, the tomato stems are thick and strong, the leaves are dark green, thick and solid, and the tomato leaves are glossy and have no plant diseases and insect pests.
The function is as follows: regulating growth and increasing yield
Experimental setup: in the test, 2 drug treatments and 1 clear water control are arranged, 1 ridge of each treatment is selected as an experimental object, and 1 tomato is randomly selected as a photographic observation point in each treatment.
The using method comprises the following steps: diluting 2% diethyl aminoethyl hexanoate soluble solution and 2% diethyl aminoethyl hexanoate aqueous solution by 1000 times, applying the solution once in the seedling stage and the bud stage of the tomato, and spraying uniformly.
Test agents: 2% diethyl aminoethyl hexanoate solution, labeled treatment one in the experiment
Comparison of the medicaments: 2% diethyl aminoethyl hexanoate aqueous solution (commercially available) labeled treatment two in the experiment
Control agents: clear water, set as blank control group, marked as CK in experiment
TABLE 122% Aminodiethyl ester to millennium tomato pharmacodynamic experiment results
| Treatment of | Fruit setting amount | Growth rate (%) | Total number of flowers | Growth rate (%) | Cell output, 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 | — |
Example five conclusions:
as shown in fig. 4-6, fig. 4 is a photograph of the results at the time of picking for cherry tomato treatment one, fig. 5 is a photograph of the results at the time of picking for cherry tomato treatment two, and fig. 6 is a photograph of the results at the time of picking for the cherry tomato control group.
From the experimental results, the difference of the 2% diethyl aminoethyl hexanoate soluble solution and the 2% diethyl aminoethyl hexanoate aqueous solution on the tomato yield increase effect is larger under the same concentration, and the diethyl aminoethyl hexanoate soluble solution has more excellent effects on the flower retention, fruit retention and yield increase of the tomatoes.
The above is only a preferred embodiment of the present invention, and it should be noted that the above preferred embodiment should not be considered as limiting the present invention, and the protection scope of the present invention should be subject to the scope defined by the 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 (7)
1. A liquid preparation for improving the stability of diethyl aminoethyl hexanoate, which is characterized in that: according to the mass percentage, the composite preservative comprises 0.1 to 20 percent of diethyl aminoethyl hexanoate, 0.1 to 30 percent of auxiliary agent, 1 to 32 percent of dissolution promoter and the balance of solvent to 100 percent; 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 triacetin.
2. The liquid preparation for improving the stability of the diethyl aminoethyl hexanoate, according to claim 1, wherein the liquid preparation comprises: the content of diethyl aminoethyl hexanoate is 1-12%.
3. The liquid preparation for improving the stability of the diethyl aminoethyl hexanoate, according to claim 1, wherein the liquid preparation comprises: the content of diethyl aminoethyl hexanoate is 1-8%.
4. The liquid preparation for improving the stability of the diethyl aminoethyl hexanoate, according to claim 1, wherein the liquid preparation comprises: the auxiliary agent is at least one of phenethyl phenol polyoxyethylene ether, alkylphenol polyoxyethylene phosphate, phenethyl phenol polyoxyethylene ether phosphate, fatty alcohol polyoxyethylene ether, polyoxyethylene sorbitan fatty acid ester, polyoxyethylene alkyl aryl ether and polyoxyalkylene glycol butyl ether.
5. A method for preparing a liquid preparation for improving the stability of a diethyl aminoethyl hexanoate preparation according to claim 1, wherein the method comprises the following steps: the method comprises the following steps:
s1, adding the dissolution accelerator A and the dissolution accelerator B into the preparation kettle, and fully stirring the mixture for 25 minutes;
s2, adding the diethyl aminoethyl hexanoate-containing technical product into a preparation kettle; fully stirring and dissolving, and controlling the process to be 20-60 minutes;
s3, adding weighed auxiliary agents into the preparation kettle, and uniformly stirring for 25 minutes;
s4, putting the solvent into a preparation kettle, and stirring uniformly for 30-60 minutes;
s5, pumping the prepared product into a semi-finished product storage tank by a discharge pump, and finishing the product preparation.
6. The method for preparing a liquid preparation for improving the stability of a diethyl aminoethyl hexanoate (DATE) as claimed in claim 5, wherein the method comprises the following steps: in the step S1, the stirring speed is 400-500 rpm.
7. The method for preparing a liquid preparation for improving the stability of a diethyl aminoethyl hexanoate (DATE) as claimed in claim 5, wherein the method comprises the following steps: and in the steps S2-S4, the stirring speed is less than 400 rpm.
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