A curcuma rhizome extract emulsion formulation, a preparation method thereof and application thereof in preventing and treating plant powdery mildew

Abstract

The present application relates to a kind of curcuma longa rhizome extract emulsion preparation and its preparation method and application in the prevention and treatment of plant powdery mildew, the component of the curcuma longa rhizome extract emulsion preparation includes 30-70% curcuma longa rhizome extract, 10-35% emulsifier, 15-50% solvent by mass percentage.It is prepared by compounding the component of specific mass ratio of curcuma longa rhizome extract, emulsifier, solvent in a new type of emulsion preparation for preventing and treating plant powdery mildew with curcuma longa rhizome extract as efficacy component, and it has excellent high temperature, low temperature stability, can make curcuma longa rhizome extract more stable and persistent to exert its powdery mildew prevention and treatment efficacy.

Description

TECHNICAL FIELD

[0001] The present application belongs to the technical field of pesticide preparation, and relates to a curcuma rhizome extract emulsifiable concentrate preparation, a preparation method thereof and application thereof in the prevention and treatment of plant powdery mildew. BACKGROUND

[0002] Powdery mildew is a kind of fungal disease, which can occur during the whole growth period of plants and mainly harms leaves, stems and fruits. At the initial stage, it is white spots, and then the color gradually changes to light brown, and black ascus can be formed through selfing or crossing. The mildew spots are initially scattered alone, and then combined into a large mildew spot, and even can cover the whole leaf, seriously affecting photosynthesis, interfering with normal metabolism, causing premature aging, and causing loss of plant yield and quality.

[0003] Legume powdery mildew mainly harms leaves, and at the initial stage of disease, nearly round powdery white mildew is produced on the leaves, or purple-brown spots are produced on the back of the leaves, and a layer of thin white powder is covered, which is the vegetative mycelium of the pathogen, and then the powdery spots are fused into powdery spots, and the reproductive mycelium of the pathogen produces a large number of conidia, and when it is serious, the powdery spots are combined into a piece, and the whole leaf is covered, causing leaf withering or falling off.

[0004] Rose is a plant with ornamental, medicinal and edible functions, and has the effects of relieving spleen, promoting blood circulation and beautifying. With the improvement of people's living standards, the demand for roses in the market is increasing, especially in recent years, there is a situation of shortage. Powdery mildew is one of the common diseases of roses, which harms roses, rosaceous plants and other flowers. After being harmed, a layer of white powdery substance is produced on the leaf surface and tender shoots, and when it is serious, the leaves turn yellow and fall off, which seriously affects the growth and flowering of the plants. This causes huge economic losses to the farmers. However, the existing prevention and treatment methods generally use 1000 times of 70% methylthiophanate or 2000 times of 50% metam granules. However, due to long-term use, the pathogen is easy to develop drug resistance, resulting in reduced drug efficacy, increased pesticide application amount, and greater adverse effects on the environment and food safety.

[0005] Grape has rich nutritional value and medicinal value, the planting area in China is expanding year by year, but a variety of diseases are prone to occur in grape cultivation, grape powdery mildew is the main disease of grape, the fruit, leaf, new branch and other green parts can be harmed, and the loss of fruit is the largest. The fruit is harmed, and a layer of gray white powdery mildew is produced on the surface of the fruit. Leaf damage produces a layer of gray white powdery mildew on the leaf surface, which gradually spreads to the whole leaf, and the diseased leaf shrinks and withers when severe. New shoots are harmed, initially showing gray-white spots, then spreading to the whole vine, the diseased vine turns from gray-white to dark gray, and finally black. It seriously affects the yield and quality of grape. At present, the methods of spraying 3-5 Baume degree of stone sulfur mixture and 0.2-0.5 Baume degree of stone sulfur mixture, or 50% tobramycin 500 times liquid, or 70% methyl tobramycin 1000 times liquid, or 25% triazole ketone wettable powder 1000 times liquid before and after germination are generally used, but the traditional chemical synthesis pesticide spraying has a series of problems such as disease resistance and pesticide residue, so it is necessary to effectively improve the prevention and control of traditional grape powdery mildew.

[0006] In agricultural production, the use of chemical synthetic pesticides has long occupied a large proportion of the total amount of pesticides, but with the continuous popularization and use of chemical synthetic pesticides, its disadvantages have gradually appeared. Chemical synthetic pesticides are difficult to degrade, have high toxicity, and long-term use can easily produce drug resistance, thereby reducing or even losing the prevention and control effect, and the chemical synthetic pesticides entering the environment can easily cause environmental pollution, and some difficult-to-degrade chemical pesticides can even be continuously enriched through the food chain, eventually entering the human body and causing harm to human health. Under the situation of pursuing green and environmental protection, the use of chemical synthetic pesticides is gradually decreasing, and the development of biological pesticides is gradually increasing. Biological pesticides refer to a kind of pesticide preparation whose effective component is a biological active body itself or its metabolic product, or a substance with specific action synthesized by imitation, which can play a role in preventing and controlling pests, diseases, weeds, nematodes, rodents and other harmful organisms. The effective component is mainly derived from animals, plants and microorganisms. Plant source pesticides are a major component of biological pesticides.

[0007] Plant source pesticides are a new type of pesticide developed by using plants themselves or extracting effective active ingredients from them to prevent and control plant pests. Among the numerous plant resources in the world, many plant resources contain effective active substances for preventing and controlling pests, including pyrethrum, neem tree and others. Plant resources for developing plant source pesticides are very rich, and plant source pesticides have broad industrialization prospects.

[0008] In the process of developing plant source pesticide, the plant effective substance extract obtained by us cannot be directly used, and we need to add some adjuvants to make it a stable, safe and efficient pesticide preparation which can be used. At present, the dosage forms of pesticides mainly include the following types: suspension concentrate (SC), emulsifiable concentrate (EC), microemulsion (ME), emulsion in water (EW), wettable powder (WP), water dispersible granule (WDG, also known as dry suspension concentrate), aqueous solution (AS), granule (GR) and microcapsule suspension concentrate (CS). For plant source pesticide preparation, many studies are devoted to the research of microemulsion, microcapsule suspension concentrate and water dispersible granule, and the development of emulsifiable concentrate is to promote the research and development of new environmentally friendly adjuvants to replace dimethylbenzene and other adjuvants that pollute the environment, so as to upgrade the emulsifiable concentrate dosage form. SUMMARY

[0009] In view of the deficiencies of the prior art, the purpose of the present application is to provide a curcuma rhizome extract emulsifiable concentrate preparation, a preparation method thereof and an application thereof in preventing and treating plant powdery mildew.

[0010] To achieve the purpose of the present application, the following technical solutions are adopted:

[0011] In the first aspect, the present application provides a curcuma rhizome extract emulsifiable concentrate preparation, and the components of the curcuma rhizome extract emulsifiable concentrate preparation include 30-70% curcuma rhizome extract, 10-35% emulsifier and 15-50% solvent in terms of mass percentage.

[0012] The present application prepares a new emulsifiable concentrate preparation for preventing and treating plant powdery mildew by compounding the components of curcuma rhizome extract, emulsifier and solvent in a specific mass ratio, which has simple preparation process, convenient use, excellent high-temperature and low-temperature stability, and can make the curcuma rhizome extract more stably and durably play its role in preventing and treating plant powdery mildew. Compared with chemical synthetic pesticides, the curcuma rhizome extract is derived from natural plants and will not accumulate in the environment to destroy the environment, but will degrade in the environment relatively quickly; it has low toxicity; at the same time, compared with chemical synthetic pesticides with single component, the curcuma rhizome extract prepared by the present application has complex components, and the prevention and treatment of plant powdery mildew is the result of the mutual cooperation of multiple effective components, and other non-effective components also play an auxiliary role, so that the target is not easy to produce drug resistance.

[0013] The mass percentage of the curcuma rhizome extract can be 30%, 35%, 40%, 45%, 50%, 55%, 60%, 65%, 70%, etc.; the mass percentage of the emulsifier can be 10%, 15%, 20%, 25%, 30%, 35%, etc.; and the mass percentage of the solvent can be 15%, 20%, 25%, 30%, 35%, 40%, 45%, 50%, etc. The specific point values in the above numerical ranges can all be selected, and thus will not be described here one by one.

[0014] Preferably, the components of the curcuma rhizome extract emulsion oil preparation include 40-60% curcuma rhizome extract, 20-30% emulsifier, and 15-35% solvent in terms of mass percentage.

[0015] When the three components of curcuma rhizome extract, emulsifier, and solvent are combined in the above more preferred mass ratio, the product has more excellent high-temperature, low-temperature, and room-temperature stability, and can make the curcuma rhizome extract more stably and durably exert its powdery mildew prevention and treatment efficacy.

[0016] Preferably, the solvent includes any one or a combination of at least two of methyl oleate, soybean oil, corn oil, rapeseed oil, or pine oil.

[0017] The present application uses the above green and environmentally friendly solvent which has good biodegradability and small pollution, thereby reducing the pollution to the environment and being more beneficial to the application of the emulsion oil preparation product.

[0018] Preferably, the emulsifier includes a non-ionic emulsifier and an anionic emulsifier.

[0019] Preferably, the non-ionic emulsifier includes any one or a combination of at least two of triphenyl ethylene phenol polyoxyethylene ether, sorbitan trioleate polyoxyethylene ether, triphenyl ethylene phenol-ethoxy-propoxy, or castor oil polyglycol ether ester.

[0020] Preferably, the anionic emulsifier is selected from any one or a combination of at least two of a diphenyl sulfonate, an alpha-olefin sulfonate, a lignin sulfonate, a sulfonate of ethoxylated alkyl phenol, a sulfonate of alkoxylated aryl phenol, a sulfonate of condensed naphthalene, a sulfonate of dodecylbenzene or tridecylbenzene, a sulfonate of naphthalene or alkyl naphthalene, or a sulfosuccinate.

[0021] The present application optimizes the formula of the emulsifier, so that it is better combined with the solvent and the curcuma rhizome extract, thereby making the system more stable and ensuring that the curcuma rhizome extract durably and stably exerts its medicinal efficacy. The following emulsifier formula is a more preferred formula.

[0022] Preferably, the emulsifier comprises, by weight percentage, 30-40% styrene phenol polyoxyethylene ether, 30-40% sorbitan trioleate polyoxyethylene ether and 25-35% calcium dodecylbenzene sulfonate.

[0023] The mass percentage of the tristyrene phenol polyoxyethylene ether can be selected from 30%, 32%, 33%, 35%, 36%, 38%, 40%, etc.; the mass percentage of the sorbitan trioleate polyoxyethylene ether can be selected from 30%, 32%, 33%, 35%, 36%, 38%, 40%, etc.; the mass percentage of the calcium dodecylbenzenesulfonate can be selected from 25%, 27%, 28%, 30%, 32%, 35%, 40%, etc. Specific values ​​within the above ranges can be selected, and will not be elaborated further here.

[0024] This invention optimizes the selection of solvent and emulsifier types, resulting in an emulsifiable concentrate formulation that is low in toxicity, safe, environmentally friendly, stable, has good emulsifying properties, and excellent long-lasting effects.

[0025] In this invention, the turmeric rhizome extract is prepared by a method comprising the following steps:

[0026] (1) The turmeric rhizome raw material was dried, pulverized, and then extracted with an ethanol aqueous solution to obtain the extract;

[0027] (2) After concentrating the extract, extract it with an organic solvent to obtain an aqueous product and an oil product;

[0028] (3) The oil phase product was subjected to molecular distillation to remove the turmeric oil resin, and the turmeric rhizome extract was obtained.

[0029] The turmeric rhizome extract prepared using the above-mentioned specific preparation process is more operable and more suitable for industrial-scale production as a raw material for emulsifiable concentrate formulations.

[0030] Furthermore, the turmeric rhizome extract prepared using the aforementioned specific preparation process is stable and has a long shelf life. At the same time, this turmeric rhizome extract is very environmentally friendly, with low toxicity to terrestrial species such as birds, bees, and silkworms in the application environment, and has superior efficacy in preventing and treating powdery mildew in plants, especially in legumes, roses, and grapes.

[0031] Preferably, the concentration of the ethanol aqueous solution is 65-85%, such as 65%, 68%, 70%, 72%, 75%, 78%, 80%, 82%, 85%, etc. Other specific values ​​within this range can be selected, and will not be elaborated here.

[0032] The concentration of the ethanol-water solution is more preferably 65-85% because the turmeric rhizome extract prepared using ethanol-water solutions within this concentration range has a more significant effect in preventing and treating powdery mildew in plants, especially in preventing and treating powdery mildew in legumes, roses, and grapes.

[0033] Preferably, the ratio of the turmeric rhizome raw material to the ethanol aqueous solution is (30-70) g / L, such as 30 g / L, 35 g / L, 40 g / L, 45 g / L, 50 g / L, 55 g / L, 60 g / L, 65 g / L, 70 g / L, etc. Other specific values ​​within this range can be selected, and will not be elaborated here.

[0034] Preferably, the extraction temperature is 15-30℃, such as 15℃, 20℃, 25℃, 30℃, etc., and the extraction time is 30-50h, such as 30h, 35h, 40h, 45h, 48h, 50h, etc. Other specific values ​​within the above range can be selected, and will not be elaborated here.

[0035] Preferably, the pressure conditions for molecular distillation are 0.1-5 Pa, such as 0.1 Pa, 0.5 Pa, 1 Pa, 1.5 Pa, 2 Pa, 2.5 Pa, 3 Pa, 3.5 Pa, 4 Pa, 5 Pa, etc., and the temperature for molecular distillation is 110-130℃, such as 110℃, 115℃, 120℃, 125℃, 130℃, etc. Other specific values ​​within the above range can be selected, and will not be elaborated here.

[0036] Preferably, the components of the turmeric rhizome extract emulsifiable concentrate further include any one or a combination of at least two of the following: synergists, defoamers, or adhesives.

[0037] The synergist may be, for example, 5-[2-(octylsulfinyl)propyl]-1,3-benzodioxane, azone, JPC-2, etc.; the adhesive may be, for example, mineral oil, gelatin, polyvinyl alcohol, etc.

[0038] In a second aspect, the present invention provides a method for preparing a turmeric rhizome extract emulsifiable concentrate formulation according to the first aspect, the preparation method comprising:

[0039] The emulsifier and solvent are mixed in the prescribed amounts for initial emulsification, and then mixed with turmeric rhizome extract for further emulsification to obtain the final product.

[0040] Preferably, the emulsification is carried out under stirring conditions, and the stirring speed is 3000-8000 rpm, such as 3000 rpm, 4000 rpm, 5000 rpm, 6000 rpm, 7000 rpm, 8000 rpm, etc. Other specific values ​​within this range can be selected, and will not be described in detail here.

[0041] Preferably, the time for the first emulsification and the second emulsification is independently 3-10 minutes, such as 3 minutes, 4 minutes, 5 minutes, 6 minutes, 7 minutes, 8 minutes, 9 minutes, 10 minutes, etc. Other specific values ​​within this range can be selected, and will not be elaborated here.

[0042] Thirdly, the present invention provides the application of the turmeric rhizome extract emulsifiable concentrate preparation according to the first aspect in the prevention and control of powdery mildew in plants, wherein the plants include legumes, roses, and viticultures.

[0043] Fourthly, the present invention provides a method for controlling powdery mildew in plants, the method comprising: applying an effective dose of the turmeric rhizome extract emulsifiable concentrate preparation described in the first aspect to legumes, roses, or viticulture plants.

[0044] Compared with the prior art, the present invention has the following beneficial effects:

[0045] This invention prepares a novel emulsifiable concentrate formulation for controlling powdery mildew in plants by compounding components including turmeric rhizome extract, emulsifier, and solvent in specific mass ratios. The preparation process is simple and convenient, and it exhibits excellent high-temperature, low-temperature, and room-temperature stability, enabling the turmeric rhizome extract to exert its powdery mildew control efficacy more stably and persistently. Compared to chemically synthesized pesticides, turmeric rhizome extract is derived from natural plants, does not accumulate and damage the environment, and degrades relatively quickly; it is also low in toxicity. Furthermore, compared to single-component chemically synthesized pesticides, the turmeric rhizome extract prepared by this invention has a complex composition. Its powdery mildew control effect is the result of the synergistic effect of multiple active ingredients, with other non-active components also playing a supporting role. Therefore, the target plant is less likely to develop resistance. Detailed Implementation

[0046] To further illustrate the technical means and effects of the present invention, the following describes the technical solution of the present invention in conjunction with preferred embodiments of the present invention. However, the present invention is not limited to the scope of the embodiments.

[0047] The composite emulsifier TERSPERSE 3016 (abbreviated as T-3016) involved in the following examples was purchased from Indorama Laboratory (formerly the Agrochemical Laboratory of Huntsman Chemical R&D Center (Shanghai) Co., Ltd.); the tristyrene phenol polyoxyethylene ether in Example 7 was purchased from Yixing Jiateng Chemical Co., Ltd. as product No. 602#; the sorbitan trioleate polyoxyethylene ether in Example 7 was purchased from Jiangsu Haian Petrochemical Plant as product No. T-85.

[0048] Preparation Example 1

[0049] This preparation example provides a turmeric rhizome extract, the preparation method of which is as follows:

[0050] (1) The dried turmeric rhizome raw material was crushed and extracted with 75% ethanol aqueous solution (material-liquid ratio of 50g / L), the extraction temperature was 20℃ and the extraction time was 48h to obtain the extract;

[0051] (2) The extract was concentrated and then extracted with n-hexane to obtain an aqueous product and an oil product;

[0052] (3) The oil phase product was subjected to molecular distillation at a pressure of 3 Pa and a temperature of 120 °C to remove the turmeric oil resin and obtain the turmeric rhizome extract.

[0053] Preparation Example 2

[0054] This preparation example provides a turmeric rhizome extract, the only difference from preparation example 1 is that an equal amount of 75% ethanol aqueous solution is replaced with 55% ethanol aqueous solution, while all other conditions remain unchanged.

[0055] Preparation Example 3

[0056] This preparation example provides a turmeric rhizome extract, the only difference between which is the preparation method and that of Preparation Example 1, except that an equal amount of 75% ethanol aqueous solution is replaced with 95% ethanol aqueous solution, while all other conditions remain unchanged.

[0057] Example 1

[0058] This embodiment provides an emulsifiable concentrate of turmeric rhizome extract, the formulation of which is as follows: 50% turmeric rhizome extract obtained in Preparation Example 1, 30% methyl oleate, and 20% composite emulsifier T-3016 (composed of 30% styrene phenol polyoxyethylene ether, 38% sorbitan trioleate polyoxyethylene ether, and 32% calcium dodecylbenzene sulfonate).

[0059] The preparation method is as follows: mix the formulated amount of compound emulsifier T-3016 and methyl oleate and emulsify for the first time at 5000 rpm for 5 min, then mix with turmeric rhizome extract and continue to emulsify again at 5000 rpm for 5 min to obtain the final product.

[0060] Example 2

[0061] This embodiment provides a turmeric rhizome extract emulsifiable concentrate formulation, the composition of which is as follows: 50% turmeric rhizome extract obtained in Preparation Example 1, 25% soybean oil, and 25% composite emulsifier T-3016 (composed of 30% styrene phenol polyoxyethylene ether, 38% sorbitan trioleate polyoxyethylene ether, and 32% calcium dodecylbenzene sulfonate).

[0062] The preparation method is as follows: the compound emulsifier and soybean oil of the prescribed amount are mixed and emulsified for the first time at 7000 rpm for 3 min, and then mixed with turmeric rhizome extract and emulsified again at 3000 rpm for 10 min to obtain the final product.

[0063] Example 3

[0064] This embodiment provides a turmeric rhizome extract emulsifiable concentrate formulation, the composition of which is as follows: 50% turmeric rhizome extract obtained in Preparation Example 1, 20% corn oil, and 30% composite emulsifier T-3016 (composed of 30% styrene phenol polyoxyethylene ether, 38% sorbitan trioleate polyoxyethylene ether, and 32% calcium dodecylbenzene sulfonate).

[0065] The preparation method is as follows: the compound emulsifier and corn oil of the prescribed amount are mixed and emulsified for the first time at 3000 rpm for 10 min, and then mixed with turmeric rhizome extract and emulsified again at 6000 rpm for 8 min to obtain the final product.

[0066] Examples 4-5

[0067] This embodiment provides two emulsifiable concentrate formulations of turmeric rhizome extract. The only difference between these formulations and those of Example 1 is that the turmeric rhizome extract prepared in Example 1 is replaced in equal amounts with the turmeric rhizome extract prepared in Examples 2-3. All other components and their contents remain unchanged.

[0068] Example 6

[0069] This embodiment provides an emulsifiable concentrate of turmeric rhizome extract. The only difference between this formulation and that of Example 1 is that the composite emulsifier T-3016 is replaced in equal amounts with other composite emulsifiers (composed of 50% Tween 80 and 50% calcium dodecylbenzenesulfonate). All other components and their contents remain unchanged.

[0070] Example 7

[0071] This example provides an emulsifiable concentrate preparation of turmeric rhizome extract. The difference in its formulation composition from that of Example 1 is only that the compound emulsifier T-3016 is replaced with an equal amount of other compound emulsifiers (composed of 48% tri-styrylphenol polyoxyethylene ether and 52% sorbitan trioleate polyoxyethylene ether), and the other components and their contents remain unchanged.

[0072] Example 8

[0073] This example provides an emulsifiable concentrate preparation of turmeric rhizome extract. The difference in its formulation composition from that of Example 1 is only that the compound emulsifier T-3016 is replaced with a single emulsifier (calcium dodecylbenzenesulfonate), and the other components and their contents remain unchanged.

[0074] Test Example 1

[0075] The emulsifiable concentrate preparations of turmeric rhizome extract prepared in Examples 1 - 3 were characterized for the following properties:

[0076] (1) Detection of the mass fraction (%) of ar-turmerone: The sample was dissolved in anhydrous methanol. Using methanol and water as the mobile phase, a C18 (4.6 mm × 250 mm, 5 μm) chromatographic column was used for high-performance liquid chromatography separation of the sample. The content of ar-turmerone in the sample was quantitatively determined by the external standard method at a UV wavelength of 242 nm.

[0077] (2) Evaluation of emulsion stability: Emulsion stability is a specific index of emulsifiable concentrate products and is directly related to the usage of the products. The test sample was diluted 200 times with standard hard water and tested according to GB / T 1603 - 2001. If there is no floating oil on the upper part and no sunken oil and precipitation on the lower part in the graduated cylinder, the emulsion stability is judged to be qualified.

[0078] (3) Evaluation of persistent foaming (1 min): The addition of emulsifiers causes a certain amount of bubbles to form when the product is dispersed in water. The amount of bubbles directly affects the usage effect of the product, so the amount of foam must be controlled. It was carried out according to GB / T 2,8137 - 2011. The foam volume ≤ 60 mL after 1 min is qualified.

[0079] (4) Evaluation of low-temperature stability: The product sometimes needs to be stored and transported under relatively cold conditions, which requires the product to still maintain a good appearance at a lower temperature without precipitation. It was carried out according to Method 2.1 in GB / T 19,137 - 2003. After storing at 2°C for 7 days, the volume of the precipitated matter ≤ 0.3 mL is qualified. <\

[0080] (5) Evaluation of thermal storage stability: Thermal storage stability is an indicator for verifying the storage period of pesticides. The thermal storage stability test is conducted by heating the product to rapidly age it, indicating whether the product has good stability when stored at room temperature. The test is carried out according to method 2.1 in GB / T19136-2003, storing the product at 55℃ for 14 days. Based on the review requirements of the pesticide testing institute and the actual measured data from the product's storage test, it is stipulated that the mass fraction and concentration of aromatic curcuminone in the turmeric extract emulsion after thermal storage should not be lower than 95% of those measured before thermal storage, and the emulsion stability should still meet the standard requirements.

[0081] The results are shown in Table 1.

[0082] Table 1

[0083]

[0084]

[0085] As shown in Table 1, the emulsifiable concentrate of turmeric rhizome extract involved in this invention has excellent emulsion stability, thermal storage stability, and low temperature stability, which enables turmeric rhizome extract to exert its powdery mildew control effect more stably and for a longer period of time.

[0086] Test Example 2

[0087] Toxicological characterization was performed on the emulsifiable concentrate formulations of turmeric rhizome extract prepared in Examples 1-3:

[0088] (1) The acute oral median lethal dose of female and male SD rats was determined by the method described in Part 4 of GB / T 15670.4-2017 "Toxicological Test Methods for Pesticide Registration";

[0089] (2) The acute dermal median lethal dose of female and male SD rats was determined by referring to the method described in Part 5 of GB / T 15670.5-2017 "Toxicological Test Methods for Pesticide Registration";

[0090] (3) The median lethal concentration (LD50) of acute inhalation in female and male SD rats was determined by referring to the method described in Part 6 of GB / T 15670.6-2017 "Toxicological Test Methods for Pesticide Registration";

[0091] (4) New Zealand white rabbit eye irritation test, the test was conducted according to the method described in Part 8 of GB / T 15670.8-2017 "Toxicological Test Methods for Pesticide Registration";

[0092] (5) Hartley guinea pig sensitization test, the test shall be conducted in accordance with the method described in Part 9 of GB / T 15670.9-2017 "Toxicological Test Methods for Pesticide Registration".

[0093] The measurement results are shown in Table 2:

[0094] Table 2

[0095] Property Example 1 Example 2 Example 3 Acute oral LD50 in female rats > 5500 mg / kg > 5500 mg / kg > 5500 mg / kg Acute oral LD50 in male rats > 7000 mg / kg > 7000 mg / kg > 7000 mg / kg Acute dermal LD50 in female rats > 2000 mg / kg > 2000 mg / kg > 2000 mg / kg Acute dermal LD50 in male rats > 2000 mg / kg > 2000 mg / kg > 2000 mg / kg Acute inhalation LD50 in female rats > 5000 mg / m 3 ]] > 5000 mg / m 3 ]] > 5000 mg / m 3 <!-- 7 -->]]> Acute inhalation LD50 in male rats > 5000 mg / m 3 ]] > 5000 mg / m 3 ]] > 5000 mg / m 3 ]] New Zealand white rabbits eye irritation Recovery within 30 h Recovery within 34 h Recovery within 36 h Hartley guinea pig sensitization rate 0％ 0％ 0％

[0096] As shown in Table 2, the turmeric rhizome extract emulsifiable concentrate preparation involved in this invention has high safety, low toxicity, low irritation, and weak allergenicity.

[0097] Test Example 3

[0098] Environmental impact tests were conducted on the emulsifiable concentrate formulations of turmeric rhizome extract prepared in Examples 1-3:

[0099] The environmental impact tests were all conducted by Shenyang Chemical Research Institute Co., Ltd., and the results are as follows:

[0100] (1) Acute oral toxicity of quail, the method is as described in Part 9 of GB / T 31270.9-2014 "Guidelines for Environmental Safety Evaluation Tests of Chemical Pesticides" (24h / 48h / 72h / 7d, female);

[0101] (2) Acute oral toxicity of honeybees was determined by referring to the contents of Part 10 of GB / T 31270.10-2014 "Guidelines for Environmental Safety Evaluation of Chemical Pesticides" (24h / 48h, female).

[0102] (3) Acute contact toxicity of bees, the method is as described in Part 10 of GB / T 31270.10-2014 "Guidelines for Environmental Safety Evaluation Tests of Chemical Pesticides" (24h / 48h, males);

[0103] (4) Acute toxicity of silkworm was determined by referring to the test method described in Part 11 of GB / T 31270.11-2014 "Guidelines for Environmental Safety Evaluation of Chemical Pesticides" (96h).

[0104] The measurement results are shown in Table 3:

[0105] Table 3

[0106]

[0107] As shown in Table 3, the turmeric root extract involved in this invention is very environmentally friendly and has low toxicity to organisms such as birds, bees, and silkworms in the environment.

[0108] Test Example 4

[0109] The emulsifiable concentrate of turmeric rhizome extract prepared in Examples 1-8 was used to conduct a control test on powdery mildew in peas:

[0110] (1) Cultivation of pea sprouts: Soak pea seeds (variety "Sweet Crisp Pea") in water in a petri dish at room temperature for 24 hours. Then drain the water, place a moistened cotton ball at the bottom of the petri dish, and evenly disperse the pea seeds in the petri dish. Water daily to keep the cotton ball moist. After about a week, when the pea sprouts grow to about 2-3 cm tall, they can be transplanted into small pots. Water them every two days. When the first true leaf of the pea sprout grows and the second true leaf unfolds, healthy sprouts with similar growth can be selected for experiments.

[0111] (2) Preparation of spore suspension of Erysphe pist DC., the pathogen of pea powdery mildew: Pea seedlings were inoculated with the conidial suspension of the pathogen by spraying. Therefore, it is necessary to prepare a spore suspension of appropriate concentration. The method is as follows:

[0112] (2.1) Fill a small spray bottle with pure water, select fresher white powdery spots on the leaves of diseased plants, and spray water to rinse the spores into a clean beaker.

[0113] (2.2) Mix the obtained spore suspension thoroughly, drop a drop onto a glass slide, and observe the spore morphology under a microscope to see if it is plump and the number of spores in one field of view at 15*10x magnification to see if it meets the requirements. Requirements for spore suspension: The spore morphology should be plump to ensure viability; the number of spores in one field of view at 15*10x magnification should be around 20-30, not too few or too many; to ensure spore activity, the time from preparation to use of the spore suspension should not exceed 2 hours.

[0114] (3) Inoculation with pea powdery mildew pathogen:

[0115] (3.1) Spray the prepared spore suspension evenly onto the pea leaves;

[0116] (3.2) Transfer the inoculated pea seedlings into a box, spray the remaining spore suspension into the box to create a high humidity environment inside the box, then cover the box and incubate at a temperature of about 25°C for 24 hours.

[0117] (3.3) After 24 hours, the pea sprouts can be removed from the lid. Once the moisture on the leaves has dried, the pesticide can be applied.

[0118] (4) Application method:

[0119] (4.1) Dilute 0.1 ml of each emulsifiable concentrate preparation 200 times with deionized water, put it into a small spray bottle and label it for later use;

[0120] (4.2) Preparation of adjuvant control group: According to the formulation, the content of turmeric extract was replaced with water to prepare an adjuvant solution with the same concentration as the adjuvant contained in the formulation. Take 0.1 ml, dilute it with water 200 times, put it into a small spray bottle, and mark it for later use.

[0121] (4.3) Preparation of reagents for positive control group: Dilute 430 g / L tebuconazole suspension with water 2000 times and put it into a small spray bottle, mark it and set it aside for later use;

[0122] (4.4) Preparation of blank control group: Fill a small spray bottle with deionized water and mark it for later use;

[0123] (4.5) Spraying: Divide the pea seedlings that have been incubated for 24 hours after inoculation into 4 replicates for each agent treatment, and spray the corresponding agent evenly on the leaf surface until the leaf surface is covered with the agent.

[0124] (4.6) Cultivation: After spraying, place the pea seedlings in an environment with a temperature of about 25℃ and a humidity of about 70% and water them every two days;

[0125] (4.7) Observation: Observe the phytotoxicity 24 hours and 5 days after spraying. Discard the formulations with severe phytotoxicity based on the phytotoxicity. Start to count the disease incidence of the remaining formulations after six days, calculate the control effect, and observe and record the changes in control effect for several consecutive days.

[0126] (5) Evaluation of efficacy:

[0127] Each sample group consisted of 10 plants, and all leaves of each plant were examined. The grading criteria are as follows:

[0128] Grade 0: No lesions;

[0129] Grade 1: The lesion area accounts for less than 5% of the total leaf area;

[0130] Grade 3: The lesion area accounts for less than 6-15% of the total leaf area;

[0131] Level 5: The area of ​​lesions accounts for less than 16-25% of the total leaf area;

[0132] Level 7: The area of ​​lesions accounts for less than 26-50% of the total leaf area;

[0133] Level 9: The lesion area accounts for more than 51% of the total leaf area.

[0134]

[0135]

[0136] The data on prevention and control effectiveness are shown in Table 4:

[0137] Table 4

[0138] Group Control effect (%) Example 1 85.71 Example 2 82.38 Example 3 83.26 Example 4 74.82 Example 5 72.25 Example 6 80.96 Example 7 78.22 Example 8 75.43 Adjuvant control group 0 Positive control group 85.47 Blank control group 0

[0139] As shown in Table 4, the turmeric root extract emulsifiable concentrate formulation involved in this invention has excellent control effect on pea powdery mildew. The preparation process conditions of the turmeric root extract and the formulation of the emulsifiable concentrate also affect this control effect.

[0140] Test Example 5

[0141] Field efficacy trials were conducted on the turmeric rhizome extract emulsifiable concentrates prepared in Examples 1 and 4-6 against grape powdery mildew.

[0142] (1) Test targets and crop varieties

[0143] Grape variety: Red Globe; Target: Grape powdery mildew;

[0144] (2) The test reagents were diluted 500 times with water in Examples 1 and 4-6 respectively for later use;

[0145] Positive control agent: 325 g / L azoxystrobin SC, Zhejiang Tianfeng Biotechnology Co., Ltd., Registration Certificate No.: PD20172823, Batch No.: 20210318; diluted 1000 times for later use; a water control was also set up.

[0146] (3) Test site: Zengjiaying, Binchuan County, Dali, Yunnan Province

[0147] Cell arrangement: The experiment was set up with 6 treatments, each treatment had 4 replicates, and each replicate area was 15 square meters;

[0148] (4) Application method: Zhengzhou Xinxiu Agricultural Machinery Co., Ltd. used a 20-type backpack electric sprayer to apply the pesticide. The pesticide was prepared according to the experimental design and sprayed evenly on the plants of each treatment until small water droplets were formed.

[0149] Apply the medicine at the early stage of the disease (that is, when there are scattered lesions on the lower leaves of the plant), apply the medicine twice, with an 8-day interval, and record the application time.

[0150] (5) Survey methods:

[0151] Five points were surveyed for each treatment, with two plants at each point, and all leaves of each plant were surveyed.

[0152] Disease severity grading criteria:

[0153] Grade 0: No lesions;

[0154] Grade 1: The lesion area accounts for less than 5% of the total leaf area;

[0155] Grade 3: Lesions cover 6%-10% of the total leaf area;

[0156] Level 5: Lesions cover 11%-20% of the total leaf area;

[0157] Level 7: Lesions cover 21%-40% of the total leaf area;

[0158] Level 9: The lesion area accounts for more than 40% of the total leaf area.

[0159] (6) Method for calculating drug efficacy:

[0160] Disease index = (∑(number of diseased leaves at each level × relative level value) / total number of leaves surveyed × 9) × 100

[0161] Efficacy (%) = (1 - (Disease index in treatment area / Disease index in control area)) × 100

[0162] The results are shown in Table 5:

[0163] Table 5

[0164]

[0165] As shown in Table 5, the turmeric root extract emulsifiable concentrate of the present invention has excellent effect in controlling grape powdery mildew. The preparation process conditions of the turmeric root extract and the emulsifiable concentrate formulation also affect this control effect.

[0166] Test Example 6

[0167] Field efficacy trials were conducted on the turmeric rhizome extract emulsifiable concentrates prepared in Examples 1 and 4-6 to treat rose powdery mildew.

[0168] (1) Test targets and crop varieties

[0169] Rose variety: Awakening; Target: Rose powdery mildew;

[0170] (2) Test reagents, in Examples 1 and 4-6, were diluted 500 times with water for later use;

[0171] Positive control reagent, 25% ethirimol sulfonate ME, Xi'an Modern Science and Technology Industry Co., Ltd., Registration Certificate No.: PD20190149, Batch No.: 20201023018; diluted 1000 times for later use; a water control group was also set up.

[0172] (3) Test location: Goujie Town, Yiliang County, Kunming, Yunnan Province

[0173] Cell arrangement: The experiment was set up with 6 treatments, each treatment had 4 replicates, and each replicate area was 15 square meters;

[0174] (4) Application method: Zhengzhou Xinxiu Agricultural Machinery Co., Ltd. used a 20-type backpack electric sprayer to apply the pesticide. The pesticide was prepared according to the experimental design and sprayed evenly on the plants of each treatment until small water droplets were formed.

[0175] Apply the medicine at the early stage of the disease (that is, when there are scattered lesions on the lower leaves of the plant), apply the medicine once, and record the time of application.

[0176] (5) Survey methods:

[0177] Five points were surveyed for each treatment, with two plants at each point, and all leaves of each plant were surveyed.

[0178] Disease severity grading criteria:

[0179] Grade 0: No lesions;

[0180] Grade 1: The lesion area accounts for less than 5% of the total leaf area;

[0181] Grade 3: Lesions cover 6%-10% of the total leaf area;

[0182] Level 5: Lesions cover 11%-20% of the total leaf area;

[0183] Level 7: Lesions cover 21%-40% of the total leaf area;

[0184] Level 9: The lesion area accounts for more than 40% of the total leaf area.

[0185] (6) Method for calculating drug efficacy:

[0186] Disease index = (∑(number of diseased leaves at each level × relative level value) / total number of leaves surveyed × 9) × 100

[0187] Efficacy (%) = (1 - (Disease index in treatment area / Disease index in control area)) × 100

[0188] The results are shown in Table 6:

[0189] Table 6

[0190] Group Control effect after 7 days after 1 application Control group / Positive control group 65.53％ Example 1 75.46％ Example 4 61.25％ Example 5 60.88％ Example 6 72.21％

[0191] The data in Table 6 show that the turmeric root extract emulsifiable concentrate of the present invention has excellent effect in controlling powdery mildew of roses. The preparation process conditions of the turmeric root extract and the formulation of the emulsifiable concentrate also affect this control effect.

[0192] The applicant declares that this invention illustrates a turmeric rhizome extract emulsifiable concentrate preparation, its preparation method, and its application in controlling powdery mildew in plants through the above embodiments. However, this invention is not limited to the above embodiments, meaning that this invention does not necessarily rely on the above embodiments for implementation. Those skilled in the art should understand that any improvements to this invention, equivalent substitutions of the raw materials in the product, addition of auxiliary components, and selection of specific methods all fall within the protection and disclosure scope of this invention.

[0193] The preferred embodiments of the present invention have been described in detail above. However, the present invention is not limited to the specific details in the above embodiments. Within the scope of the technical concept of the present invention, various simple modifications can be made to the technical solution of the present invention, and these simple modifications all fall within the protection scope of the present invention.

[0194] It should also be noted that the various specific technical features described in the above specific embodiments can be combined in any suitable manner without contradiction. In order to avoid unnecessary repetition, the present invention will not describe the various possible combinations separately.

Claims

1. A curcuma rhizome extract emulsion formulation, characterized by, The components of the ginger rhizome extract emulsifiable concentrate formulation include 30-70% ginger rhizome extract, 10-35% emulsifier, and 15-50% solvent by mass percentage; The ginger rhizome extract is prepared by a preparation method comprising the following steps: (1) drying and pulverizing ginger rhizome raw materials, and then extracting with an ethanol aqueous solution having a concentration of 65-85%, the solid-liquid ratio of the ginger rhizome raw materials to the ethanol aqueous solution being (30-70) g / L, to obtain an extraction liquid; (2) concentrating the extraction liquid, and then extracting with an organic solvent to obtain a water phase product and an oil phase product; (3) subjecting the oil phase product to molecular distillation to remove ginger oleoresin, to obtain the ginger rhizome extract; The emulsifier includes 30-40% tristyrylphenol polyoxyethylene ether, 30-40% sorbitan trioleate polyoxyethylene ether, and 25-35% calcium dodecylbenzenesulfonate by mass percentage.

2. The Curcuma longa rhizome extract emulsifiable formulation according to claim 1, characterized in that, The components of the ginger rhizome extract emulsifiable concentrate formulation include 40-60% ginger rhizome extract, 20-30% emulsifier, and 15-35% solvent by mass percentage.

3. The Curcuma rhizome extract emulsifiable formulation according to claim 1, characterized by, The solvent includes any one or a combination of at least two of methyl oleate, soybean oil, corn oil, rapeseed oil, or pine oil.

4. The Curcuma rhizome extract emulsifiable formulation according to claim 1, characterized by, The extraction temperature is 15-30℃, and the extraction time is 30-50 h.

5. The curcuma rhizome extract emulsifiable formulation according to claim 1, characterized by, The pressure condition of the molecular distillation is 0.1-5 Pa, and the temperature of the molecular distillation is 110-130℃.

6. The Curcuma rhizome extract emulsion formulation as claimed in claim 1 wherein, The components of the ginger rhizome extract emulsifiable concentrate formulation further include any one or a combination of at least two of a synergist, an antifoaming agent, or a sticking agent.

7. The method of preparing Curcuma longa rhizome extract emulsifiable formulation according to any one of claims 1 to 6, characterized in that, The preparation method comprises: mixing the emulsifier and the solvent in a formula amount to perform first emulsification, and then mixing the ginger rhizome extract to perform second emulsification, to obtain the ginger rhizome extract emulsifiable concentrate formulation.

8. The method of preparing Curcuma longa rhizome extract emulsifiable formulation as claimed in claim 7, wherein, The emulsification is performed under stirring, and the stirring speed is 3000-8000 rpm.

9. The method of preparing curcuma rhizome extract emulsifiable formulation according to claim 7, characterized in that, The first emulsification and the second emulsification are independently for 3-10 min.

10. Use of the Curcuma longa rhizome extract emulsion formulation according to any one of claims 1 to 6 for the control of plant powdery mildew, characterized in that, The plant includes a leguminous plant, a rosaceous plant, or a vitaceous plant.

11. A method for controlling powdery mildew of plants, characterized by, The control method comprises: applying an effective dose of the ginger rhizome extract emulsifiable concentrate formulation of any one of claims 1-6 to the leguminous plant, the rosaceous plant, or the vitaceous plant.

Images