A pesticidal composition, formulation, use and method of use

Abstract

The present application relates to the technical field of pesticides, in particular to a kind of pesticide composition, preparation, use and method, the pesticide composition includes the active ingredient A and active ingredient B with mass ratio of 1: (10-50), the active ingredient A is p-chlorophenoxyacetic acid or its agronomically acceptable salt, the active ingredient B is ethylene.The present application is by p-chlorophenoxyacetic acid (or its salt) and ethylene is compounded according to specific proportion with specific application concentration is applied, reaches the effect of controlling vigorous, inhibiting ear germination and increasing yield, alleviates the negative influence of growth inhibition to root system and young ear development caused by ethylene as the vigorous controller is used and the side effect of early decline and yield reduction caused by as ear germination inhibitor is used;Meanwhile, the pesticide preparation provided by the present application is soluble concentrate, and has high efficacy, strong penetration, convenient use, good safety, and the active ingredient is not easy to decompose, and the physical and chemical properties are stable.

Description

Technical Field

[0001] This invention relates to the field of pesticide technology, specifically to a pesticide composition, formulation, use, and method of application. Background Technology

[0002] According to data from the Food and Agriculture Organization of the United Nations, approximately 25% of nitrogen fertilizer globally is ineffectively consumed, leading not only to resource waste but also exacerbating excessive crop vegetative growth. To control this excessive growth, growers use ethephon and chlormequat chloride during the crop's growth period. The use of ethephon for growth control during crop growth has been widely reported, but excessively high concentrations can lead to severe growth inhibition, resulting in stunted stems, curled leaves, and reduced grain filling; conversely, low concentrations have little effect. Sun Wanchun et al., in their study on the application effects of ethephon and other growth regulators on direct-seeded rice, found that applying ethephon at the late tillering and flowering stages of rice has a certain anti-lodging effect, but improper concentrations can also cause yield reduction. Zhang Rong et al., in their study on the regulation of wheat spike grain formation by ethephon and 1-methylcyclopropene, found that spraying ethephon can accelerate wheat maturity, shorten the development time of caryopsis, and reduce caryopsis size and volume. Furthermore, it also has a significant inhibitory effect on agronomic traits such as spikelet number, grain number per spike, and thousand-grain weight.

[0003] Sprouting at the panicle refers to the phenomenon where crops sprout directly from the panicle due to prolonged periods of high humidity caused by continuous rainfall after maturity but before harvest. It is a global agricultural hazard. In recent years, with global warming and the increasing frequency of extreme weather events, the occurrence of sprouting at the panicle of grain crops coinciding with continuous rainfall during the maturity period has become more frequent. Sprouting at the panicle not only reduces crop yield but also leads to increased activity of hydrolytic enzymes within the grains, resulting in the self-degradation of starch and protein, thus affecting the edible and processing value of the grains. In production practice, sprouting at the panicle is often prevented by regulating crop growth and adjusting the harvest time to avoid rainy weather, or by spraying plant growth regulators. Current literature research indicates that the use of inducing agents, ethephon, paclobutrazol, and malathion can inhibit sprouting at the panicle of rice and wheat to a certain extent.

[0004] The mechanism by which ethephon inhibits pre-germination is mainly through the release of ethylene, which disrupts the hormonal balance between seed dormancy and germination, enhances the inhibitory effect of abscisic acid (ABA), and antagonizes the promoting effect of gibberellin (GA), thereby maintaining seed dormancy and preventing germination. The ethylene response factor ERF12 upregulates ABA levels in rdo3 and negatively regulates GA levels downstream of ETR1, controlling seed dormancy. ERF12 can bind to the promoter of DOG1, recruiting the transcriptional co-repressor TPL to inhibit the expression of the key dormancy gene DOG1, thus regulating seed dormancy. However, the most significant and important effect of ethylene is promoting fruit ripening. Using ethephon alone to inhibit pre-germination accelerates crop development, shortens the development period, and forces grains into a "forced ripening" state before they are fully mature, reducing grain weight. Furthermore, "forced ripening" grains have poor seed coat development and weak dormancy; once rain occurs, dormancy is easily broken, triggering pre-germination. Summary of the Invention

[0005] In view of this, in order to overcome the deficiencies in the prior art, the present invention provides a pesticide composition, formulation, use and method of application, which has the functions of controlling excessive growth, inhibiting ear sprouting and increasing yield and quality.

[0006] To achieve the above objectives, the present invention provides the following technical solutions.

[0007] In a first aspect, the present invention provides a pesticide composition comprising active ingredient A and active ingredient B in a mass ratio of 1:(10-50), wherein active ingredient A is p-chlorophenoxyacetic acid or an agronomically acceptable salt thereof, and active ingredient B is ethephon.

[0008] Furthermore, the agronomically acceptable salts of p-chlorophenoxyacetic acid include sodium p-chlorophenoxyacetic acid and potassium p-chlorophenoxyacetic acid.

[0009] Secondly, the present invention provides a pesticide formulation comprising the aforementioned pesticide composition and a pesticide-acceptable adjuvant, wherein the pesticide formulation is in the form of a soluble concentrate or a soluble powder, and the pesticide composition comprises 5.5% to 51% by mass in the pesticide formulation.

[0010] Furthermore, the additives include surfactants, solvents, fillers, and antifreeze agents.

[0011] Furthermore, the surfactant is selected from at least one of hydroxyl polyethylene oxide block copolymers, alkyl glycosides, styrene-based phenol polyoxyethylene, fatty alcohol polyoxyethylene ethers, fatty amide polyoxyethylene ethers, polyoxyethylene dehydrated sorbitol monooleate, polyethylene glycol-propylene glycol copolymers, cocamidopropyl betaine, tristyrene-based phenol polyoxyethylene ether, and EO-PO block polyoxyethylene ether; the solvent is selected from at least one of dimethylacetamide, dimethyloctadecanamide, dimethylacetamide, dimethyl sulfoxide, ethylene glycol diacetate, diethylene glycol butyl ether acetate, triethyl phosphate, propylene carbonate, and propylene glycol methyl ether; the filler is selected from at least one of silica, anhydrous magnesium sulfate, potassium dihydrogen phosphate, potassium sulfate, anhydrous lactose, boric acid, and exfoliating agent; and the antifreeze is selected from at least one of ethylene glycol, propylene glycol, and glycerol.

[0012] Furthermore, the surfactant has a mass percentage of 1-10% in the pesticide formulation, the solvent has a mass percentage of 5-20% in the pesticide formulation, and the antifreeze has a mass percentage of 5-10% in the pesticide formulation.

[0013] The pesticide composition or formulation provided by this invention contains an active ingredient that is a combination of p-chlorophenoxyacetic acid (or its salt) and ethephon. P-chlorophenoxyacetic acid (or its salt), as a phenoxycarboxylic acid, has physiological effects similar to endogenous hormones and a long duration of biological activity. However, its structure differs significantly from that of IAAs, making it difficult for polar transport systems to recognize. It can be absorbed through the roots, stems, leaves, flowers, and fruits of plants, primarily through non-polar transport via the phloem along the "source-sink" flow of photosynthetic products. This stimulates cell division and tissue differentiation, ovary enlargement, and promotes fruit setting and fruit enlargement. This invention, by rationally controlling the ratio of p-chlorophenoxyacetic acid (or its salt) to ethephon, allows for combined application during the crop's jointing stage. Ethephon effectively controls excessive growth, reducing crop height and center of gravity, and enhancing lodging resistance. P-chlorophenoxyacetic acid (or its salt) mitigates the negative effects of excessive growth inhibition by ethephon on root and young spike development. Furthermore, combined application during the grain-filling stage synergistically enhances the inhibition of spikelet bud break. The reason for ear sprouting is based on the relationship between abscisic acid (ABA) and gibberellin (GA). Gibberellin is the main germination promoting hormone, while abscisic acid is the main germination inhibiting hormone. It can maintain seed dormancy. p-Chlorophenoxyacetic acid (or its salt) can indirectly promote the biosynthesis of ABA and enhance the tissue's sensitivity to ABA, increasing the ABA / GA ratio. It synergistically enhances the effect of inhibiting ear sprouting with ethephon, thereby reducing the amount of ethephon used and reducing the premature senescence effect of exogenous ethephon during seed maturity. Furthermore, p-chlorophenoxyacetic acid (or its salts) is absorbed through the roots, stems, leaves, flowers, and fruits of plants, exhibiting long-lasting biological activity. It primarily undergoes non-polar transport via the phloem along the source-sink flow of photosynthetic products, mobilizing nutrients for fruit transport and accumulating in sink organs such as young fruits. This regulates plant growth and development. Therefore, the combined use of p-chlorophenoxyacetic acid (or its salts) and ethephon can regulate the grain-filling process, resulting in fuller, more mature grains, improving quality and increasing yield, while mitigating the premature yield decline caused by using ethephon alone during the grain-filling period. Simultaneously, the combined use of p-chlorophenoxyacetic acid (or its salts) and ethephon reduces the time required to alleviate the inhibitory effect of ethylene on seeds, without affecting the germination of seeds used for seed production the following year.

[0014] Thirdly, the present invention provides the application of the pesticide composition or pesticide formulation in increasing crop yield and improving quality, wherein the crops include wheat, rice and corn.

[0015] Furthermore, the method for applying the pesticide composition or pesticide formulation to increase wheat yield and improve quality is to spray the whole plant with a diluted solution of the pesticide composition or pesticide formulation during the jointing stage and the grain-filling stage of wheat, respectively. The application concentration of active ingredient A is 8-10 ppm, and the application concentration of active ingredient B is 100-400 ppm. The diluted solution is sprayed at a rate of 40 L of water per acre to dilute active ingredients A and B in the pesticide composition or pesticide formulation to the application concentration.

[0016] Furthermore, the method for applying the pesticide composition or pesticide formulation to increase rice yield and improve quality is to spray the entire plant with a diluted solution of the pesticide composition or pesticide formulation during the jointing stage and the grain-filling stage of rice, respectively. The application concentration of active ingredient A is 8-10 ppm, and the application concentration of active ingredient B is 100-400 ppm. The diluted solution is sprayed at a rate of 40 L of water per acre to dilute active ingredients A and B in the pesticide composition or pesticide formulation to the application concentration.

[0017] Furthermore, the method for applying the pesticide composition or pesticide formulation to increase corn yield and improve quality is as follows: when the corn has 6-10 unfolded leaves and during the grain-filling stage, spray the entire plant with a diluted solution of the pesticide composition or pesticide formulation. The application concentration of active ingredient A is 4-10 ppm, and the application concentration of active ingredient B is 100-400 ppm. The diluted solution is applied by diluting active ingredients A and active ingredients B in the pesticide composition or pesticide formulation to the application concentration using 30 L of water per acre.

[0018] In summary, compared with the prior art, the present invention has the following beneficial effects: The pesticide composition and pesticide formulation provided by this invention, by compounding p-chlorophenoxyacetic acid (or its salt) with ethephon in a specific ratio and applying it at a specific concentration, achieves the effects of controlling excessive growth, inhibiting ear sprouting, and increasing yield and quality. It alleviates the negative impact of growth inhibition on root and young ear development caused by the use of ethephon as a growth regulator, as well as the side effects of premature yield reduction caused by its use as an ear sprouting inhibitor. At the same time, the pesticide formulation provided by this invention is a soluble agent with high efficacy, strong permeability, convenient use, good safety, and the active ingredients are not easily decomposed and have stable physicochemical properties. Detailed Implementation

[0019] The present invention will be further described below with reference to specific embodiments. It should be understood that the following embodiments are merely illustrative of the present invention and should not be considered as the entirety of the invention or as a limitation or restriction of the technical solution of the present invention. Unless otherwise specified, the raw materials used in the following embodiments can be obtained through conventional commercial channels.

[0020] Example 1: Effects of sodium p-chlorophenoxyacetate and ethephon on wheat growth I. Experimental Objective: To investigate the effects of different ratios and dosages of sodium p-chlorophenoxyacetate and ethephon on wheat.

[0021] II. Test location: Wangchang Village, Yanjin County, Xinxiang City, Henan Province.

[0022] III. Test subject: Wheat, variety Bainong 1316.

[0023] IV. Test reagents: 98% sodium p-chlorophenoxyacetate technical grade was supplied by Sichuan Runer Technology Co., Ltd. 40% ethephon soluble concentrate, provided by Sichuan Runer Technology Co., Ltd.

[0024] V. Experimental Basis: NY / T2061.5-2016 "Guidelines for Indoor Bioassay Testing of Pesticides - Plant Growth Regulators - Part 5: Determination of Combined Effects of Mixtures"; 《NY / T 1739-2009 Test Method for Wheat Resistance to Sprouting》.

[0025] VI. Test Methods: Multiple treatment groups were designed using a randomized block design. According to the pesticide application design in Table 1, each treatment group was sprayed with the pesticide corresponding to Table 1 at the jointing and grain-filling stages of wheat, and the amount of water used to dilute the pesticide was 40L / mu.

[0026] Table 1. Treatment design for treatment groups

[0027] VII. Evaluation Indicators: 1. Safety: Whether the application of the pesticide will cause phytotoxicity (such as dry tips of wheat awns, withered leaves, and grain loss).

[0028] The method for classifying phytotoxicity is as follows: - No pesticide damage; +: Very slight impact, no effect on crop growth; ++: Moderate impact, no effect on crop yield, recoverable; +++: Severely affects normal growth and has a certain impact on yield; ++++: Very serious, causing losses and severe production reduction.

[0029] 2. Indicator Measurement: Thirty plants were randomly selected from each treatment group, and plant height, number of grains per ear, number of effective ears per square meter, and thousand-grain weight were investigated at maturity.

[0030] Plant height: Measure the vertical distance from the ground surface (or tillering node) to the top of the wheat ear (excluding the awns). Take 30 plants for measurement and take the average value. Number of grains per ear: count the grains threshed from a single ear of wheat, and take the average of the counts from 20 ears of wheat; Effective number of ears per square meter: The effective number of ears per square meter was measured using the sampling point method. The area of ​​the sampling point and the count were determined using the "1-meter double row" method, and the average value was taken after five repetitions. 1000-grain weight: Randomly select 100 whole grains and weigh them, repeat eight times and take the average value. Multiply the average value by ten to get the 1000-grain weight.

[0031] 3. Indicator Calculation ; ; .

[0032] 4. Evaluation of germination resistance in panicles At physiological maturity, 20 whole wheat ears were randomly selected from each treatment group. The total number of grains in the 20 ears was counted. The 20 ears were soaked in tap water for 4 hours, then disinfected with 0.1% sodium hypochlorite solution for 5 minutes. They were then placed in an artificial climate chamber simulating the field germination temperature and humidity conditions (22℃, 100%RH) for germination culture. After germination was terminated, the grains were manually removed, and the number of germinated grains in the 20 ears was counted to calculate the germination rate per ear.

[0033] .

[0034] Daily number of germinated grains: When wheat reaches the germination standard, it is judged as wheat germination; each treatment has a total of 5 ears of wheat, and the number of germinated grains per ear per day is investigated for each treatment.

[0035] The germination resistance level is graded according to Table 2 based on the relative germination index.

[0036] .

[0037] Table 2. Evaluation Criteria for Wheat Ear Germination Resistance

[0038] 5. Data Analysis The Gowing method was used to test the yield-increasing and bud-suppressing effects of the mixture of two plant growth regulators. The theoretical formula for calculating the mixed effect is: E0 = X + Y - XY / 100, where X represents the yield-increasing or bud-suppressing rate of regulator "sodium p-chlorophenoxyacetate (A)" at a dosage of P; Y represents the yield-increasing or bud-suppressing rate of regulator "ethephon (B)" at a dosage of Q; and E0 represents the theoretical yield-increasing or bud-suppressing rate of regulator (A+B) at a dosage of (P+Q).

[0039] According to the Gowing method, when E-EO>10%, it indicates that the mixed plant growth regulator has a synergistic effect; when E-E0<-10%, it indicates that the mixed plant growth regulator has an antagonistic effect; when the E-E0 value is between ±10%, it indicates that the mixed plant growth regulator has an additive effect, where E represents the measured yield increase rate or bud suppression rate of each treatment.

[0040] VIII. Test Results Safety results are shown in Table 3, yield increase results are shown in Table 4, and wheat spike sprouting inhibition results are shown in Table 5.

[0041] Table 3. Safety evaluation of different treatment agents

[0042] As can be seen from Table 3, the medication was safe in all treatment groups, and no phytotoxicity occurred.

[0043] Table 4. Effects of different treatments on wheat yield

[0044] As shown in Table 4, the combined application concentrations of sodium chlorophenoxyacetate and ethephon at 2ppm+100ppm (mass ratio 1:50), 4ppm+200ppm (mass ratio 1:50), 8ppm+100 / 200ppm (mass ratio 1:12.5, 1:25), and 10ppm+100 / 200 / 400 / 600ppm (mass ratio 1:10, 1:20, 1:40, 1:60) had a synergistic effect on wheat yield.

[0045] Table 5. Effects of different treatments on wheat's resistance to pre-harvest sprouting.

[0046] As shown in Table 5, the combined application concentrations of sodium chlorophenoxyacetate and ethephon at 2 ppm + 100 ppm (mass ratio 1:50) and 4 ppm + 200 ppm (mass ratio 1:50) exhibited a synergistic effect in inhibiting wheat ear germination, with the ear germination resistance level being moderately resistant. Furthermore, the combined application concentrations of sodium chlorophenoxyacetate and ethephon at 8 ppm + 200 / 400 ppm (mass ratios 1:25 and 1:50) and 10 ppm + 100 / 200 / 400 / 600 ppm (mass ratios 1:10, 1:20, 1:40, and 1:60) also exhibited a synergistic effect in inhibiting wheat ear germination, with the ear germination resistance level being resistant.

[0047] Considering the impact on yield, anti-sprouting effect, and economic factors, the optimal application concentrations for the combination of sodium chlorophenoxyacetate and ethephon are 8ppm + 200 / 400ppm (mass ratio of 1:25, 1:50) and 10ppm + 100 / 200 / 400ppm (mass ratio of 1:10, 1:20, 1:40).

[0048] IX. Pesticide Residue Detection According to GB 2763.1-2022, the national food safety standard for maximum residue limits of 112 pesticides, including sodium 2,4-D butyrate, in food, the residue limit for sodium p-chlorophenoxyacetate is 0.05 mg / kg. According to GB 2763—2021, the national food safety standard for maximum residue limits of pesticides in food, the residue limit for ethephon in wheat is 1 mg / kg. Therefore, the maximum residue limit for sodium p-chlorophenoxyacetate in wheat is set at 0.05 mg / kg, and the maximum residue limit for ethephon is set at 1 mg / kg.

[0049] Residue testing was performed on the seeds harvested from the treatment groups (No. 18-19 and No. 21-23) using the above-mentioned preferred concentrations of compound preparation.

[0050] The testing methods were based on SNT 3725-2013, the testing methods for grains, beans, and tea. The tests showed that no residues of sodium p-chlorophenoxyacetate and ethephon were detected in the seeds harvested from the above-mentioned treatment groups, indicating that they are safe to use.

[0051] Example 2: Effects of sodium p-chlorophenoxyacetate and ethephon on rice growth I. Experimental Objective: To investigate the effects of different ratios and dosages of sodium p-chlorophenoxyacetate and ethephon on rice.

[0052] II. Test location: Fenjie Town, Taixing City, Jiangsu Province.

[0053] III. Experimental subject: Rice, variety Nanjing 5055, with a full growth period of 158 days, an early-maturing late-japonica type.

[0054] IV. Test reagents: 98% sodium p-chlorophenoxyacetate technical grade was supplied by Sichuan Runer Technology Co., Ltd. 40% ethephon soluble concentrate, provided by Sichuan Runer Technology Co., Ltd.

[0055] V. Experimental Basis: NY / T2061.5-2016 "Guidelines for Indoor Bioassay Testing of Pesticides: Plant Growth Regulators Part 5: Determination of Combined Effects of Mixtures"; There is currently no method for testing rice's resistance to panicle germination. Since the mechanism of rice panicle germination is similar to that of wheat, the method is based on "NY / T1739-2009 Test Method for Wheat Resistance to Panicle Germination".

[0056] VI. Test Methods: Multiple treatment groups were designed using a randomized block design. Following the pesticide application design in Table 1 of Example 1, each treatment group was sprayed with the pesticide corresponding to Table 1 of Example 1 at the jointing and grain-filling stages of rice. The amount of water used to dilute the pesticide was 40 L / mu.

[0057] VII. Evaluation Indicators: 1. Safety: Observe the rice plants for any side effects (such as yellowing leaves, wrinkling, etc.) 3 days after application; observe the overall growth of the rice for any side effects (such as yellowing leaves, wrinkling, etc.) 7 days after application; continue to observe the growth of the rice.

[0058] The method for grading pesticide damage is the same as that for wheat in Example 1.

[0059] 2. Indicator Measurement: Thirty plants were randomly selected from each treatment group, and plant height, number of grains per ear, number of effective ears per square meter, and thousand-grain weight were investigated at maturity.

[0060] Plant height: Measure the vertical distance from the ground surface (or tillering node) to the top of the rice panicle (excluding the awn). Take 30 plants for measurement and take the average value. Number of grains per panicle: count the grains threshed from a single panicle, and take the average of the counts from 20 panicles; Effective ears per square meter: The effective ears per square meter were measured using a sampling point method. The area of ​​the sampling point and the count were determined using the "1-meter double row" method, and the average value was taken after five repetitions. 1000-grain weight: Randomly select 100 whole grains and weigh them, repeat eight times and take the average value. Multiply the average value by ten to get the 1000-grain weight.

[0061] 3. Indicator Calculation ; ; .

[0062] 4. Evaluation of sprouting resistance in wheat ears: The evaluation of sprouting resistance in wheat ears in Example 1 was conducted in accordance with the evaluation of sprouting resistance in wheat ears in Example 1.

[0063] 5. Data analysis: Same as in Example 1.

[0064] VIII. Test Results Safety results are shown in Table 6, yield increase results are shown in Table 7, and results on inhibiting rice panicle germination are shown in Table 8.

[0065] Table 6. Safety evaluation of different treatment agents

[0066] As can be seen from Table 6, the medication was safe in all treatment groups, and no phytotoxicity occurred.

[0067] Table 7. Effects of different treatments on rice yield

[0068] As shown in Table 7, the combined application concentrations of sodium chlorophenoxyacetate and ethephon at 2ppm+100ppm (mass ratio 1:50), 4ppm+200ppm (mass ratio 1:50), 8ppm+100 / 200 / 400ppm (mass ratios 1:12.5, 1:25, 1:50), and 10ppm+100 / 200 / 400 / 600ppm (mass ratios 1:10, 1:20, 1:40, 1:60) enhanced rice yield.

[0069] Table 8. Effects of different treatments on rice's resistance to panicle sprouting.

[0070] As shown in Table 8, the combined application concentrations of sodium chlorophenoxyacetate and ethephon at 2 ppm + 100 ppm (mass ratio 1:50) and 4 ppm + 200 ppm (mass ratio 1:50) showed a synergistic effect in inhibiting rice panicle germination, but the panicle germination resistance level was susceptible. The combined application concentrations of sodium chlorophenoxyacetate and ethephon at 8 ppm + 100 / 200 / 400 / 600 ppm (mass ratios 1:12.5, 1:25, 1:50, 1:75) and 10 ppm + 100 / 200 / 400 / 600 ppm (mass ratios 1:10, 1:20, 1:40, 1:60) showed a synergistic effect in inhibiting rice panicle germination, and the panicle germination resistance level was resistant.

[0071] Considering the impact on yield, anti-sprouting effect, and economic factors, the optimal application concentrations for the compound application of sodium chlorophenoxyacetate and ethephon are 8ppm + 100 / 200 / 400ppm (mass ratios of 1:12.5, 1:25, and 1:50) and 10ppm + 100 / 200 / 400ppm (mass ratios of 1:10, 1:20, and 1:40).

[0072] IX. Pesticide Residue Detection According to GB 2763.1-2022, the national food safety standard for maximum residue limits of 112 pesticides, including sodium 2,4-D butyrate, in food, the residue limit for sodium p-chlorophenoxyacetate is 0.05 mg / kg. According to GB 2763—2021, the national food safety standard for maximum residue limits of pesticides in food, the residue limit for ethephon in rice is 1 mg / kg. Therefore, the maximum residue limit for sodium p-chlorophenoxyacetate in rice is set at 0.05 mg / kg, and the maximum residue limit for ethephon is set at 1 mg / kg.

[0073] Residue testing was performed on the seeds harvested from the treatment groups (Nos. 17-19 and 21-23) using the above-mentioned preferred concentrations of compound preparation.

[0074] The testing methods were based on SNT 3725-2013, the testing methods for grains, beans, and tea. The tests showed that no residues of sodium p-chlorophenoxyacetate and ethephon were detected in the seeds harvested from the above-mentioned treatment groups, indicating that they are safe to use.

[0075] Example 3: Effects of sodium p-chlorophenoxyacetate and ethephon on maize growth I. Experimental Objective: To investigate the effects of different ratios and dosages of sodium p-chlorophenoxyacetate and ethephon on corn.

[0076] II. Test location: Shuangfu Town, Taihe County, Fuyang City, Anhui Province.

[0077] III. Experimental subject: Maize, variety Dingyou 151P, which belongs to the Huang-Huai-Hai summer maize variety.

[0078] IV. Test reagents: 98% sodium p-chlorophenoxyacetate technical grade was supplied by Sichuan Runer Technology Co., Ltd. 40% ethephon soluble concentrate, provided by Sichuan Runer Technology Co., Ltd.

[0079] V. Experimental Basis: NY / T2061.5-2016 "Guidelines for Indoor Bioassay Testing of Pesticides - Plant Growth Regulators - Part 5: Determination of Combined Effects of Mixtures"; There is currently no method for testing corn ear germination resistance. Since the germination mechanism of corn ears is similar to that of wheat, the method is based on the "NY / T1739-2009 Test Method for Wheat Ear Germination Resistance".

[0080] VI. Test Methods: Multiple treatment groups were designed using a randomized block design. Following the pesticide application design in Table 1 of Example 1, each treatment group was sprayed with the pesticide corresponding to Table 1 of Example 1 when the corn had 6-10 unfolded leaves and during the grain-filling stage. The amount of water used to dilute the pesticide was 30L / acre.

[0081] VII. Evaluation Indicators: 1. Safety: After application, continuously observe whether it affects the normal growth of corn, and observe the effect on tasseling and the effect on ear maturity after grain filling.

[0082] The method for classifying pesticide damage is the same as that for wheat pesticide damage in Example 1.

[0083] 2. Indicator Measurement: Ten plants were randomly selected from each treatment group, and at maturity, plant height, ear length, tip barrenness length, total number of grains per ear, and weight of 100 grains were investigated.

[0084] Plant height: The distance measured vertically upwards from the point where the main stem of the plant contacts the ground to the highest natural point of the male tassel (crown of the ear). The average value is taken from 10 plants. Ear length: The length from the leaf scar at the lower end of the ear to the tip of the ear, measured from 10 plants and the average value is taken; Bald tip length: The straight-line distance from the last row of normal kernels at the top of the corn ear to the top of the ear, measured on 10 plants and the average value is taken; Total number of grains per ear: Determine the number of grain rows and the average number of grains per row, and obtain the estimate using the "number of rows × number of grains per row" method, taking the average value of 10 plants; Weight per 100 kernels: Randomly select 100 whole kernels and weigh them, repeat ten times and take the average value.

[0085] 3. Indicator Calculation ; ; ; ; ; .

[0086] 4. Evaluation of sprouting resistance in wheat ears: The evaluation of sprouting resistance in wheat ears in Example 1 was conducted in accordance with the evaluation of sprouting resistance in wheat ears in Example 1.

[0087] 5. Data analysis: Same as in Example 1.

[0088] VIII. Test Results Safety results are shown in Table 9, yield increase results are shown in Table 10, and results on inhibiting corn ear germination are shown in Table 11.

[0089] Table 9. Safety evaluation of different treatment agents

[0090] As can be seen from Table 9, the medication was safe in all treatment groups, and no phytotoxicity occurred.

[0091] Table 10. Effects of different treatments on maize yield

[0092] As shown in Table 10, the combined application concentrations of sodium chlorophenoxyacetate and ethephon at 2 ppm + 100 ppm (mass ratio 1:50), 4 ppm + 100 / 200 ppm (mass ratio 1:25, 1:50), 8 ppm + 100 / 200 / 400 ppm (mass ratio 1:12.5, 1:25, 1:50), and 10 ppm + 100 / 200 / 400 ppm (mass ratio 1:10, 1:20, 1:40) had a synergistic effect on corn yield.

[0093] Table 11. Effects of different treatments on maize's resistance to ear sprouting.

[0094] As shown in Table 11, the combined application concentrations of sodium chlorophenoxyacetate and ethephon are 2 ppm + 100 ppm (mass ratio 1:50) and 8 ppm + 600 ppm. At a concentration of ppm (mass ratio of 1:75), it had a synergistic effect on inhibiting corn ear germination, but the ear germination resistance level was susceptible; when the combined application concentration of sodium chlorophenoxyacetate and ethephon was 4ppm+100ppm (mass ratio of 1:25), it had a synergistic effect on inhibiting corn ear germination, but the ear germination resistance level was moderately resistant; when the combined application concentration of sodium chlorophenoxyacetate and ethephon was 4ppm+200ppm (mass ratio of 1:50), 8ppm+100 / 200 / 400ppm (mass ratios of 1:12.5, 1:25, 1:50), and 10ppm+100 / 200 / 400 / 600ppm (mass ratios of 1:10, 1:20, 1:40, 1:60), it had a synergistic effect on inhibiting corn ear germination, and the ear germination resistance level was resistant.

[0095] Considering the impact on yield, anti-spillage and germination effects, and economic factors, the optimal application concentrations for the compound application of sodium chlorophenoxyacetate and ethephon are 4ppm + 200ppm (mass ratio 1:50), 8ppm + 100 / 200 / 400ppm (mass ratios 1:12.5, 1:25, 1:50), and 10ppm + 100 / 200 / 400ppm (mass ratios 1:10, 1:20, 1:40).

[0096] IX. Pesticide Residue Detection According to GB 2763.1-2022, the national food safety standard for maximum residue limits of 112 pesticides, including sodium 2,4-D butyrate, in food, the residue limit for sodium p-chlorophenoxyacetate is 0.05 mg / kg. According to GB 2763—2021, the national food safety standard for maximum residue limits of pesticides in food, the residue limit for ethephon in corn is 0.5 mg / kg. Therefore, the maximum residue limit for sodium p-chlorophenoxyacetate in corn is set at 0.05 mg / kg, and the maximum residue limit for ethephon is set at 0.5 mg / kg.

[0097] Residue testing was performed on the seeds harvested from the treatment groups (No. 14, No. 17-19, No. 21-23) using the above-mentioned preferred concentrations of compound preparation.

[0098] The testing methods were based on SNT 3725-2013, the testing methods for grains, beans, and tea. The tests showed that no residues of sodium p-chlorophenoxyacetate and ethephon were detected in the seeds harvested from the above-mentioned treatment groups, indicating that they are safe to use.

[0099] Example 4: Preparation and storage stability testing of sodium p-chlorophenoxyacetate-ethephon soluble concentrate. According to the dosage shown in Table 12, measure each reagent and adjuvant. First, put the measured solvent into the reaction vessel, turn on the stirrer, and then add the measured sodium p-chlorophenoxyacetate technical, surfactant, and antifreeze into the reaction vessel in sequence. Then, add purified water into the reaction vessel and stir evenly. Finally, add ethephon technical and dissolve it completely. After standing, filter to obtain sodium p-chlorophenoxyacetate•ethephon soluble concentrate with different active ingredient contents.

[0100] The pesticide formulations prepared above were stored at 0±2℃ for 7 days, 54±2℃ for 14 days, and 30±2℃ for 2 years, respectively. Their morphological changes were observed, and the decomposition of the active ingredients was detected by HPLC and ion chromatography (refer to GB / T 23554). The results are shown in Table 13.

[0101] Table 12. Raw material list for preparing sodium p-chlorophenoxyacetate•ethephon soluble concentrate (mass percentage, %)

[0102] Table 13. Storage stability of sodium p-chlorophenoxyacetate-ethephon soluble concentrate

[0103] As can be seen from Table 13 above, the storage stability of formulations 1 to 6 all meet the relevant requirements of GB / T19137-2003 Determination of Low Temperature Stability of Pesticides, GB / T19136-2003 Determination of Thermal Storage Stability of Pesticides, and NY / T1427-2016 General Standard for Stability Testing of Pesticides at Room Temperature.

[0104] Example 5: Preparation and storage stability testing of sodium p-chlorophenoxyacetate-ethephon soluble powder According to the dosage shown in Table 14, measure each reagent and excipient. First, put the measured silica and anhydrous magnesium sulfate into the mixing vessel, turn on the stirrer, then put the measured ethephon technical into the mixing vessel and mix evenly. Then, add the sodium p-chlorophenoxyacetate technical, other fillers, and surfactants and mix evenly. After crushing the above materials, finely mix for 10-15 minutes to obtain sodium p-chlorophenoxyacetate•ethephon soluble powder with different active ingredient contents.

[0105] The pesticide formulations prepared above were stored at 54±2℃ for 14 days and at 30±2℃ for 2 years, respectively. Their morphological changes were observed, and the decomposition of the active ingredients was detected by HPLC and ion chromatography (refer to GB / T 23554). The results are shown in Table 15.

[0106] Table 14. Raw material list (mass percentage) for preparing sodium p-chlorophenoxyacetate•ethephon soluble powder

[0107] Table 15. Storage stability of sodium p-chlorophenoxyacetate•ethephon soluble powder

[0108] As can be seen from Table 15 above, the storage stability of formulations 7 to 12 all meet the relevant requirements of GB / T 19136-2003 Determination of thermal storage stability of pesticides and NY / T 1427-2016 General Rules for the Stability Test of Pesticides at Room Temperature.

[0109] The above description is merely an embodiment of the present invention and does not limit the patent scope of the present invention. Any equivalent structural or procedural transformations made using the present invention specification, or direct or indirect applications in other related technical fields, are similarly included within the patent protection scope of the present invention.

Claims

1. A method for applying a pesticide composition or pesticide formulation to control excessive crop growth, inhibit panicle sprouting, and increase yield and quality, characterized in that: The pesticide composition comprises active ingredient A and active ingredient B in a mass ratio of 1:(10-50), wherein active ingredient A is p-chlorophenoxyacetic acid or an agronomically acceptable salt thereof, and active ingredient B is ethephon; The pesticide formulation includes the pesticide composition and pesticide-acceptable adjuvants. The crops include wheat, rice, and corn; The method for applying the pesticide composition or pesticide formulation to control excessive growth, inhibit ear sprouting, and increase yield and quality in wheat is to spray the entire plant with a diluted solution of the pesticide composition or pesticide formulation during the jointing and grain-filling stages of wheat, respectively. The application concentration of active ingredient A is 8-10 ppm, and the application concentration of active ingredient B is 100-400 ppm. The diluted solution is applied by diluting active ingredients A and active ingredients B in the pesticide composition or pesticide formulation to the application concentration using 40 L of water per acre. The method for applying the pesticide composition or pesticide formulation to control excessive growth, inhibit panicle sprouting, and increase yield and quality in rice is to spray the entire plant with a diluted solution of the pesticide composition or pesticide formulation during the jointing stage and the grain-filling stage of rice, respectively. The application concentration of active ingredient A is 8-10 ppm, and the application concentration of active ingredient B is 100-400 ppm. The diluted solution is applied by diluting the active ingredients A and B in the pesticide composition or pesticide formulation to the application concentration using 40L of water per acre. The method for applying the pesticide composition or pesticide formulation to control excessive growth, inhibit ear sprouting, and increase yield and quality in corn is as follows: when the corn has 6-10 unfolded leaves and during the grain-filling stage, spray the entire plant with a diluted solution of the pesticide composition or pesticide formulation. The application concentration of active ingredient A is 4-10 ppm, and the application concentration of active ingredient B is 100-400 ppm. The diluted solution is applied by diluting active ingredients A and active ingredient B in the pesticide composition or pesticide formulation to the application concentration using 30 L of water per acre.

2. The method according to claim 1, characterized in that: The agronomically acceptable salts of p-chlorophenoxyacetic acid include sodium p-chlorophenoxyacetic acid and potassium p-chlorophenoxyacetic acid.

3. The method according to claim 1, characterized in that: The pesticide formulation is in the form of a soluble concentrate or a soluble powder, and the pesticide composition accounts for 5.5% to 51% of the pesticide formulation by mass.

4. The method according to claim 1, characterized in that: The additives include surfactants, solvents, fillers, and antifreeze agents.

5. The method according to claim 4, characterized in that: The surfactant is selected from at least one of hydroxyl polyethylene oxide block copolymer, alkyl glycoside, styrylphenol polyoxyethylene, fatty alcohol polyoxyethylene ether, fatty amide polyoxyethylene ether, polyoxyethylene dehydrated sorbitol monooleate, polyethylene glycol propylene glycol copolymer, cocamidopropyl betaine, tristyrylphenol polyoxyethylene ether, and EO-PO block polyoxyethylene ether. The solvent is selected from at least one of dimethylacetamide, dimethyloctadecanamide, dimethylacetamide, dimethyl sulfoxide, ethylene glycol diacetate, diethylene glycol butyl ether acetate, triethyl phosphate, propylene carbonate, and propylene glycol methyl ether. The filler is selected from at least one of the following: silica, anhydrous magnesium sulfate, potassium dihydrogen phosphate, potassium sulfate, anhydrous lactose, boric acid, and exfoliating powder. The antifreeze is selected from at least one of ethylene glycol, propylene glycol, and glycerol.

6. The method according to claim 5, characterized in that: The surfactant has a mass percentage of 1-10% in the pesticide formulation, the solvent has a mass percentage of 5-20% in the pesticide formulation, and the antifreeze has a mass percentage of 5-10% in the pesticide formulation.

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