CN113115778B - Ethylicin sustained release preparation and preparation method thereof - Google Patents
Ethylicin sustained release preparation and preparation method thereof Download PDFInfo
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- CN113115778B CN113115778B CN202110371366.XA CN202110371366A CN113115778B CN 113115778 B CN113115778 B CN 113115778B CN 202110371366 A CN202110371366 A CN 202110371366A CN 113115778 B CN113115778 B CN 113115778B
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- ethylicin
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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
- A01N41/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a sulfur atom bound to a hetero atom
- A01N41/02—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a sulfur atom bound to a hetero atom containing a sulfur-to-oxygen double bond
- A01N41/04—Sulfonic acids; Derivatives thereof
- A01N41/08—Sulfonic acid halides; alpha-Hydroxy-sulfonic acids; Amino-sulfonic acids; Thiosulfonic acids; Derivatives thereof
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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
- A01N25/08—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 solids as carriers or diluents
- A01N25/10—Macromolecular compounds
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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
- A01N25/18—Vapour or smoke emitting compositions with delayed or sustained release
Abstract
The invention discloses an ethylicin sustained release preparation and a preparation method thereof, wherein the ethylicin sustained release preparation comprises the following components in parts by mass: 1-10 parts of ethylicin missible oil; 20-40 parts of sustained-release oil core auxiliary materials; 2-20 parts of diatomite; 1-5 parts of sodium alginate or sodium polyacrylate; 1-10 parts of soluble calcium salt; 1-5 parts of glycerol; 5-20 parts of water. The ethylicin sustained release preparation prepared by the invention can reduce odor and slow the release speed of the ethylicin, and achieves the purposes of prolonging the retention period of the pesticide effect of the ethylicin and reducing the use times and the application amount of the ethylicin. In addition, the ethylicin sustained release preparation also shows a certain temperature response characteristic, and is more close to the field production requirement.
Description
Technical Field
The invention relates to an ethylicin sustained release preparation and a preparation method thereof, belonging to the technical field of ethylicin application.
Background
Ethylicin is a plant bionic pesticide developed by our country, and has the advantages of quick effect, wide bactericidal spectrum, low residue and the like. The pesticide composition can effectively prevent and treat various crop diseases, such as potato black stem disease, rice bakanae disease, mango tree leaf moss, grape anthracnose, dragon fruit anthracnose, paris polyphylla leaf spot disease, kiwi fruit canker, cassava bacterial wilt, citrus gonggan black rot, paris polyphylla gray mold, strawberry gray mold and the like. In addition, ethylicin also has the effects of regulating plant growth, increasing seed germination rate, promoting crop growth, increasing yield, improving quality and the like. Zhang S and other researches find that ethylicin can inhibit the activity of ribosome and protein synthesis of Phytophthora (Phytophthora infestans), so that the prevention and treatment effect on potato late blight is realized.
At present, ethylicin has two preparation ways of plant extraction and artificial synthesis, is yellowish or brownish yellow oily transparent or semitransparent liquid and has odor. The ethylicin is characterized by volatility and special unpleasant odor, so that the field utilization rate is relatively low, the lasting period is short, and the experience of farmers is not good in the application process, so that the ethylicin medicament product has good effect but is not popular with users.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: provides a ethylicin sustained release preparation and a preparation method thereof, aiming at solving the technical problems of high release speed, short drug effect period and heavy odor of the ethylicin.
The technical scheme of the invention is as follows: a ethylicin sustained release preparation comprises the following components by mass:
1-10 parts of ethylicin missible oil;
20-40 parts of sustained-release oil core auxiliary materials;
2-20 parts of diatomite;
1-5 parts of sodium alginate or sodium polyacrylate;
1-10 parts of soluble calcium salt;
1-5 parts of glycerol;
5-20 parts of water.
Optionally, the slow-release oil core auxiliary material is a mixture of pentaerythritol tetrastearate, pentaerythritol distearate, pentaerythritol tetraoleate and pentaerythritol dioleate.
Optionally, the mass ratio of the pentaerythritol tetrastearate to the pentaerythritol distearate to the pentaerythritol tetraoleate to the pentaerythritol dioleate is 8-2: 8-2: 1-4: 1-4.
Optionally, the soluble calcium salt is calcium gluconate, calcium acetate or calcium chloride.
Optionally, the sustained release preparation is sustained release granules or sustained release gel.
The invention also provides a method for preparing the ethylicin sustained-release preparation, which comprises the following process steps: firstly, mixing ethylicin missible oil and slow-release oil core auxiliary materials, then uniformly mixing the mixture with diatomite, dispersing the mixture into sodium alginate or sodium polyacrylate aqueous solution, and then dripping the solution into soluble calcium salt aqueous solution for solidification to obtain the ethylicin slow-release particles.
The invention also provides a method for preparing the ethylicin sustained-release preparation, which comprises the following process steps: the ethylicin missible oil is mixed with the sustained-release oil core auxiliary material, then the mixture is uniformly mixed with the diatomite and dispersed in the sodium alginate or sodium polyacrylate aqueous solution, and then the solution is soaked in the soluble calcium salt aqueous solution for solidification, thus obtaining the ethylicin sustained-release gel.
The invention has the beneficial effects that: the ethylicin sustained release preparation prepared by the invention can reduce odor and slow the release speed of the ethylicin, and achieves the purposes of prolonging the retention period of the pesticide effect of the ethylicin and reducing the use times and the application amount of the ethylicin. In addition, the ethylicin sustained release preparation also shows a certain temperature response characteristic, and is more close to the field production requirement.
Applicants have found in their studies that an ethylicin emulsifiable concentrate is miscible with pentaerythritol tetrastearate (PETS), pentaerythritol tetraoleate (PETO) in any ratio, but is not miscible with pentaerythritol distearate (PEDS), pentaerythritol dioleate (PEDO), glycerol and water; PETS, PETO, PEDS and PEDO can be mixed and dissolved in any ratio. Therefore, the temperature-sensitive type medicine carrier can be prepared by exerting the melting point difference between PETS and PETO and the mixing and dissolving characteristic of the PETS and the ethylicin missible oil; meanwhile, the temperature-sensitive type drug release barrier layer which is well fused with the drug carrier is constructed by utilizing the characteristics that PEDS and PEDO have different melting points and are not miscible with ethylicin missible oil but are miscible with the drug carrier PETS and PETO. Finally constructing the ethylicin slow-release body with the temperature response release characteristic: sustained release granules and sustained release gels.
Drawings
FIG. 1 is a product form diagram of ethylicin slow-release granules;
fig. 2 is a release curve chart of the ethylicin sustained-release granules.
Detailed Description
The invention will be further described with reference to specific examples:
measurement method
The relevant assay methods will first be described as follows:
1. method for testing release period of ethylicin sustained-release preparation
Weighing 20 parts of 10 g/part of sustained-release granules or gel, and placing 10 parts of the sustained-release granules or gel at 20 ℃ and 35 ℃ for constant-temperature release. The content of ethylicin sampled and measured at 0d is 100 percent, 1 sample per day is used for measuring the residual amount of the ethylicin in the sustained-release granules or the gel, and the release rate is calculated.
The release rate of ethylicin is calculated by adopting a residual quantity method, namely the content X1 of the ethylicin in the sample of the ethylicin released for a certain time is measured, and the residue rate Y1 is obtained by dividing X1 by the theoretical amount X0 of the ethylicin, and the release rate is obtained by (1-Y1) multiplied by 100 percent.
2. Method for measuring substance concerned
The ethylicin content is determined by high performance liquid chromatography, the chromatographic column is an Aijier Promocil C18 chromatographic column (4.6mm × 250mm, 5 μm), the mobile phase is acetonitrile-water (30: 70), the flow rate is 1.0 mL/min-1, the detection wavelength is 210nm, and the column temperature is 30 ℃.
Example 1
The content of each component in the ethylicin slow release preparation is as follows:
the oil core comprises 1g of ethylicin missible oil, 20g of slow-release oil core auxiliary materials (wherein the mass ratio of pentaerythritol tetrastearate, pentaerythritol distearate, pentaerythritol tetraoleate and pentaerythritol dioleate is 8: 8: 1: 1), 2g of diatomite, 5g of sodium alginate, 1g of calcium gluconate, 1g of glycerol and 5g of water.
The preparation method comprises the following steps: the ethylicin missible oil is mixed with the sustained-release oil core auxiliary material, then the mixture is uniformly mixed with the diatomite and dispersed in 1.5 percent sodium alginate aqueous solution, and then the solution is dripped into 2 percent calcium gluconate aqueous solution for solidification, thus obtaining the ethylicin sustained-release granules.
The test shows that the sustained release preparation of ethylicin has a release rate of 99.2% at 35 ℃ for 10 days, which is 81.2% higher than 18.0% at 20 ℃. Meanwhile, the sensory experience shows that the odor of the ethylicin sustained-release preparation is obviously reduced.
Example 2
The content of each component in the ethylicin slow release preparation is as follows:
10g of ethylicin missible oil, 40g of slow-release oil core auxiliary materials (wherein the mass ratio of pentaerythritol tetrastearate, pentaerythritol distearate, pentaerythritol tetraoleate and pentaerythritol dioleate is 2: 2: 4: 4), 20g of diatomite, 2g of sodium polyacrylate, 10g of calcium acetate, 5g of glycerol and 20g of water.
The preparation method comprises the following steps: firstly, mixing ethylicin missible oil and sustained-release oil core auxiliary materials, then uniformly mixing the mixture with diatomite, dispersing the mixture into 1.5% sodium polyacrylate aqueous solution, and then dripping the solution into 2% calcium acetate aqueous solution for solidification to obtain the ethylicin sustained-release particles.
The test shows that the sustained release preparation of ethylicin has a release rate of 99.7% at 35 ℃ for 10 days, which is 81.5% higher than 18.2% at 20 ℃. Meanwhile, the sensory experience shows that the odor of the ethylicin sustained-release preparation is obviously reduced.
Example 3
The content of each component in the ethylicin slow release preparation is as follows:
5g of ethylicin missible oil, 30g of slow-release oil core auxiliary materials (wherein the mass ratio of pentaerythritol tetrastearate, pentaerythritol distearate, pentaerythritol tetraoleate and pentaerythritol dioleate is 6: 4: 2: 2), 10g of diatomite, 3g of sodium alginate, 6g of calcium chloride, 2g of glycerol and 14g of water.
The preparation method comprises the following steps: firstly, mixing ethylicin missible oil and sustained-release oil core auxiliary materials, then uniformly mixing the mixture with diatomite, dispersing the mixture into 1.5% sodium alginate aqueous solution, and then dripping the solution into 2% calcium chloride aqueous solution for solidification to obtain the ethylicin sustained-release particles.
The test shows that the sustained release preparation of ethylicin has a release rate of 99.3% at 35 ℃ for 10 days, which is 81.4% higher than the release rate of 17.9% at 20 ℃. Meanwhile, the sensory experience shows that the odor of the ethylicin sustained-release preparation is obviously reduced.
Example 4
The content of each component in the ethylicin slow release preparation is as follows:
6g of ethylicin missible oil, 25g of slow-release oil core auxiliary materials (wherein the mass ratio of pentaerythritol tetrastearate, pentaerythritol distearate, pentaerythritol tetraoleate and pentaerythritol dioleate is 4: 4: 2: 2), 8g of diatomite, 2g of sodium alginate, 8g of calcium chloride, 3g of glycerol and 13g of water.
The preparation method comprises the following steps: firstly, mixing ethylicin missible oil and sustained-release oil core auxiliary materials, then uniformly mixing the mixture with diatomite, dispersing the mixture into 1.5% sodium alginate aqueous solution, and then dripping the solution into 2% calcium chloride aqueous solution for solidification to obtain the ethylicin sustained-release particles.
The test shows that the sustained release preparation of ethylicin has a release rate of 99.4% at 35 ℃ for 10 days, which is 80.9% higher than 18.5% at 20 ℃. Meanwhile, the sensory experience shows that the odor of the ethylicin sustained-release preparation is obviously reduced.
Example 5
The content of each component in the ethylicin slow release preparation is as follows:
the oil core comprises 4g of ethylicin missible oil, 26g of slow-release oil core auxiliary materials (wherein the mass ratio of pentaerythritol tetrastearate, pentaerythritol distearate, pentaerythritol tetraoleate and pentaerythritol dioleate is 2: 2: 3: 3), 6g of diatomite, 4g of sodium alginate, 7g of calcium chloride, 3g of glycerol and 12g of water.
The preparation method comprises the following steps: the ethylicin missible oil is mixed with the sustained-release oil core auxiliary material, then the mixture is uniformly mixed with the diatomite and dispersed in 1.5 percent sodium alginate aqueous solution, and then the solution is soaked in 2 percent calcium chloride aqueous solution for solidification, thus obtaining the ethylicin sustained-release gel.
The test shows that the sustained release preparation of ethylicin has 90% of release rate at 35 ℃ for 10 days and 74% of release rate at 20 ℃ higher than 16%. Meanwhile, the sensory experience shows that the odor of the ethylicin sustained-release preparation is obviously reduced.
FIG. 1 is a product form diagram of ethylicin slow-release granules, and the granules are round in form, uniform in size and good in product appearance. FIG. 2 is a graph showing the release profile of sustained release granules of ethylicin measured in example 1.
From examples 1 to 5, the sustained release preparation of ethylicin prepared by the invention can reduce odor and slow the release rate of ethylicin, and achieves the purposes of prolonging the retention period of the pesticide effect of ethylicin and reducing the use times and application amount of the ethylicin. In addition, the ethylicin sustained release preparation also shows a certain temperature response characteristic, and is more close to the field production requirement. For example, various crop diseases such as potato black-stem disease and rice bakanae disease do not occur at about 20 ℃, but these diseases begin to appear on crops at 30 ℃.
The following experiments illustrate the screening of the sustained release oil core excipients of the present invention:
1. test reagents and instruments
Test reagents: ethylicin, provided by Hanbang plant protectant Limited liability company of Tianjin, with a content of 80%; pentaerythritol tetrastearate (PETS), Pentaerythritol distearate (PEDS), Pentaerythritol tetraoleate (PETO), and Pentaerythritol dioleate (PEDO) are all products of Jiaxing Zhongcheng environmental protection science and technology, and the palm oil is Philippine natural palm oil, mineral oil, Tween 80, span 80, sodium alginate, calcium acetate, calcium gluconate, diatomaceous earth, and the like, which are all domestic industrial-grade reagents.
The LT202 electronic balance scale is a product of the ever-ripe market quantity Limited liability company, the constant-temperature magnetic stirrer 85-2 type is a product of Shanghai Zhi Cheng electric appliances Limited company, the constant-temperature water bath HH-1 and the mechanical stirrer OES-20 are products of Shanghai Kazuo scientific instruments Limited company, and the micro liquid-moving gun 100-.
2. Drug core oil phase formula screening and optimization
2.1 screening of compatibility between candidate drug core material and ethylicin
Respectively mixing 1mL of ethylicin solution with equal volume of PETS (molten), PEDS (molten), PETO, PEDO, palm oil (molten), mineral oil, Tween 80 and span 80, rapidly oscillating at normal temperature, mixing uniformly, standing for 10min, and determining whether the mixture can be mixed or not by observing whether the layers are layered or not.
Tests prove that the ethylicin missible oil can be completely mixed with PETS, PETO and span 80 and can not be mixed with PEDS, PEDO, mineral oil and Tween 80. Considering that the solidification temperature of PETS and PETO is higher, and the solidification temperature of PEDS and PEDO is lower, the possibility that the mixed product has proper processing temperature and the slow release of the ethylicin is higher, a mixture of pentaerythritol tetrastearate, pentaerythritol distearate, pentaerythritol tetraoleate and pentaerythritol dioleate is adopted as the slow release oil core auxiliary material.
2.2 measurement of melting and solidification temperatures of Mixed cores
In order to measure the solidification condition of PETS and PETO mixed with PEDS and PEDO, the applicant selects the PETS and PEDO mixture to perform the test.
Preparing a mixture according to the mass ratio of PETS to PEDO of 9:1, 6:1, 4:1, 1:4, 1:6 and 1: 9. Heating and melting in 80 deg.C water bath, mixing, and cooling at 5 deg.C to observe the solidification state of the mixture (the retention time of each temperature gradient is 30 min). After the temperature reduction procedure is finished, the temperature is gradually increased according to 5 ℃ steps to observe whether the mixture is melted or not. The melting temperature and the solidification temperature of each sample of the mixing ratio were thus determined.
The melting/solidification of the different PETS and PEDO mixtures at the respective temperatures is shown in table 1. It can be seen from table 1 that with increasing PETS ratio, the mixture solidification temperature increases progressively; instead, the mixture solidification temperature decreases with increasing proportion of PEDO.
TABLE 1 solidification of PETS and PEDO mixtures in various proportions under a temperature reduction program
"-" indicates a clear liquid state, "+" indicates a flocculent precipitate, "+ + +" indicates a soft gel state, and "+ + + +" indicates a hard solid state
It can be seen from table 2 that the dissolution temperature of the mixture also increases gradually with increasing PETS ratio, with the same tendency to change its setting temperature.
TABLE 2 melting State of PETS and PEDO mixtures in the proportions under the temperature reduction program
"-" shows complete dissolution, "+" shows flocculent precipitate, "+ + +" shows soft gel state, and "+ + + +" shows hard solid state
From the above, the ethylicin emulsifiable concentrate is miscible with pentaerythritol tetrastearate (PETS), pentaerythritol tetraoleate (PETO) in any ratio, but is not miscible with pentaerythritol distearate (PEDS), pentaerythritol dioleate (PEDO), glycerol and water; PETS, PETO, PEDS and PEDO can be mixed and dissolved in any ratio. Therefore, the temperature-sensitive type medicine carrier can be prepared by exerting the melting point difference between PETS and PETO and the mixing and dissolving characteristic of the PETS and the ethylicin missible oil; meanwhile, the temperature-sensitive type drug release barrier layer which is well fused with the drug carrier is constructed by utilizing the characteristics that PEDS and PEDO have different melting points and are not miscible with ethylicin missible oil but are miscible with the drug carrier PETS and PETO. Finally constructing the ethylicin slow-release body with the temperature response release characteristic: sustained release granules and sustained release gels.
The foregoing is a more detailed description of the invention in connection with specific preferred embodiments and it is not intended that the invention be limited to these specific details. For those skilled in the art to which the invention pertains, several simple deductions or substitutions can be made without departing from the spirit of the invention, and all shall be considered as belonging to the protection scope of the invention.
Claims (5)
1. The ethylicin sustained-release preparation is characterized by comprising the following components in parts by mass:
1-10 parts of ethylicin missible oil;
20-40 parts of sustained-release oil core auxiliary materials;
2-20 parts of diatomite;
1-5 parts of sodium alginate or sodium polyacrylate;
1-10 parts of soluble calcium salt;
1-5 parts of glycerol;
5-20 parts of water;
the slow-release oil core auxiliary material is a mixture of pentaerythritol tetrastearate, pentaerythritol distearate, pentaerythritol tetraoleate and pentaerythritol dioleate, and the mass ratio of the pentaerythritol tetrastearate to the pentaerythritol distearate to the pentaerythritol tetraoleate to the pentaerythritol dioleate is 8-2: 8-2: 1-4: 1-4.
2. The sustained-release ethylicin formulation according to claim 1, wherein said soluble calcium salt is calcium gluconate, calcium acetate or calcium chloride.
3. The sustained-release ethylicin preparation according to claim 1, wherein said sustained-release preparation is a sustained-release granule or a sustained-release gel.
4. A process for preparing a sustained release formulation of ethylicin according to any one of claims 1 to 3, comprising the process steps of: firstly, mixing ethylicin missible oil and slow-release oil core auxiliary materials, then uniformly mixing the mixture with diatomite, dispersing the mixture into sodium alginate or sodium polyacrylate aqueous solution, and then dripping the solution into soluble calcium salt aqueous solution for solidification to obtain the ethylicin slow-release particles.
5. A process for preparing a sustained release formulation of ethylicin according to any one of claims 1 to 3, comprising the process steps of: the ethylicin missible oil is mixed with the sustained-release oil core auxiliary material, then the mixture is uniformly mixed with the diatomite and dispersed in the sodium alginate or sodium polyacrylate aqueous solution, and then the solution is soaked in the soluble calcium salt aqueous solution for solidification, thus obtaining the ethylicin sustained-release gel.
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