An agricultural composition

Abstract

The present invention discloses an agricultural composition, specifically a composition of sanguinarine and plant essential oil A for agricultural use, wherein the plant essential oil A includes d-limonene, eugenol, citronellal, α-pinene, terpinolene, geranyl aldehyde, 4-terpineol, nerolidol, menthone, anethole, thymol, carvacrol, myrcene and β-caryophyllene. The mass ratio of sanguinarine to plant essential oil A is 69:1 to 1:149, and the mass fraction of the sum of the masses of sanguinarine and plant essential oil A in the composition is 0.1%-76%. The composition of the present invention has good activity against harmful mites, pests, nematodes and fungal diseases caused by various crops, and has a significant synergistic effect, reduces the dosage and cost of pesticides, and is beneficial to environmental protection and the comprehensive control of agricultural diseases.

Description

Technical Field

[0001] The present invention relates to a pesticide composition and its application field, in particular to a composition containing sanguinarine and plant essential oil, and a preparation method and application scheme thereof, which are used for preventing and controlling harmful mites, pests, nematodes and pathogenic fungi on crops. Background Art

[0002] With the intensification of agriculture, agricultural production is characterized by concentrated land use, a single crop variety, and a high multiple cropping index. This has led to a high frequency of pest outbreaks in pest control, and frequent pesticide use has led to the development of severe pest resistance. The development and application of new pesticides are of great significance for preventing, controlling, or eradicating pests, diseases, and weeds in agricultural production, regulating crop harvest time, yield, quality, and transportation, storage, and processing performance, and safeguarding my country's food security.

[0003] In the process of exploring pesticide application methods, dosages, types, and integrated pest management strategies, problems caused by excessive chemical pesticide dosages, long-term application of single ingredients, and low pesticide target and utilization rates have gradually become recognized. These problems include the accumulation of resistance in pests, diseases, and weeds, pesticide residues in agricultural and sideline products, ecological damage to agricultural soil, water bodies, and beneficial organisms, and the depletion of non-renewable resources. Consequently, the definition of pesticides has gradually evolved toward "precise control and rational regulation of agricultural ecosystems."

[0004] Compared to chemical pesticides, biopesticides are a type of pesticide derived from biological metabolites or using living organisms for integrated control of biological populations in agricultural ecosystems. Their targeted selectivity, non-target biosafety, eco-friendliness, and sustainability make them a promising choice for agricultural production. The expanded use of biopesticides has positive implications for alleviating environmental pressures, reducing reliance on non-renewable resources, and managing resistance in agricultural pests. Within appropriate use, they can serve as an alternative to chemical pesticides.

[0005] Among biopesticides, sanguinarine and plant essential oils are two types of biopesticides with a wide spectrum of action and research.

[0006] Sanguinarine [Archly der Pharmazie, 1901, 239: 395-408.]; CAS number: 2447-54-3; English name: Sanguinarine; Molecular formula: C 20 H 14NO4; relative molecular weight 332.33. Sanguinarine is a plant-derived alkaloid extracted from the rhizomes of Macleaya and Greater Chelidonium. Studies have shown that sanguinarine has repellent, antifeedant, growth-inhibiting or toxic effects on a variety of agricultural pests, such as tobacco aphids, bean sprout moths and tea caterpillars [Guizhou University, 2008.], tea loopers [Hui Agricultural Sciences. 2007, 35(5):1408,1415.], Asian corn borers [Northwest Botanical Journal, 2007(8):1650-1655.], peach aphid nymphs and red flour beetle adults [Journal of Anhui Agricultural University, 2007(10):114-115.] 09, 36(1):18-21.], diamondback moth and 5th instar larvae of Pieris rapae [Anhui Agricultural Sciences, 2009, 37(25):11904-11905.], 3rd instar larvae of cotton bollworm, armyworm and cabbage worm [Journal of Zhejiang University (Agriculture and Life Sciences), 2008, 34(2):187-192.], hawthorn spider mite [Pesticide Science and Management, 2021, 42(05):60-63.], etc. In addition, it also has bactericidal activity against some sanitary pests, such as fly maggots and dung nematodes [Chinese Journal of Parasitology and Parasitic Diseases, 1999, 1:128]. Public literature shows that sanguinarine also has a broad-spectrum antibacterial effect and can inhibit the growth of many bacteria. It also has different degrees of inhibitory growth or effect on some fungi, such as: wheat fusarium wilt fungus [Hubei Plant Protection, 2006, 2:31-32.], cotton wilt fungus [Chinese Patent Medicine, 2010, 7, 32(7):1108-1111.], apple anthracnose fungus [Journal of Mountain Agriculture and Biology. 2006, 25(1):89-91.], yam anthracnose fungus and corn leaf blight fungus [Hubei Plant Protection, 2006, 2:31-32.], watermelon wilt fungus [Natural Medicine Research and Development, 2009, 21:419.], rice blast fungus and barley stripe fungus [Chinese Patent Medicine, 2010, 7, 32(7):1108-1111.], etc.

[0007] Essential oils are a class of secondary metabolites extracted from plants. They are composed of a variety of small molecules, including alcohols, aldehydes, phenols, and terpenes, and possess a characteristic aromatic odor. They are reported to exhibit a wide range of antibacterial, insecticide, and antiviral activities. These oils can exhibit antifungal and antibacterial activity by disrupting bacterial cell walls or membranes, inhibiting DNA synthesis, inhibiting energy metabolism, and inhibiting microbial nutrient absorption and utilization [Food Control, 2014. Journal of Microbiology, 2019]. They can also exhibit insecticide and repellent activity by destroying the wax layer of the body wall and blocking neural signals [PLoS neglected tropical diseases, 2016]. They can also achieve antiviral effects by disrupting viral envelopes, affecting viral replication, and inducing autophagy [Molecules, 2020. Nutrients, 2019]. Essential oils of different structural types exhibit significant differences in their targets and bioactivities against crop pests and diseases.

[0008] The plant essential oils of the present invention include d-limonene, eugenol, citronellal, α-pinene, terpinolene, geranyl aldehyde, 4-terpineol, nerolidol, menthone, anethole, thymol, carvacrol, myrcene and β-caryophyllene. In agriculture, d-limonene, eugenol, citronellal and carvacrol are more commonly used.

[0009] d-limonene[China Plant Protection Guide, 2019, 39(8):24-28.]; CAS number: 5989-27-5; English name: D-limonene; Molecular formula: C 10 H 16; Relative molecular weight 136.24. d-limonene is extracted from the peel or pulp of citrus or lemon fruits [Phytomedicine, 2013]. d-limonene belongs to the monocyclic monoterpenoid plant essential oil and is the right-handed isomer of limonene. Studies have shown that d-limonene has certain contact and repellent activity against red flour beetles, green bean weevils, and whiteflies [South China Agricultural University, 2020-07-20.]. Studies have shown that d-limonene has the effect of inhibiting the laying of eggs by female adult mites of citrus [Biological Disaster Science, 2019, 42(04):268-271.] and has a certain ovicidal effect [Biological Disaster Science, 2019, 42(04):268-271.]. Studies have shown that d-limonene also has a certain preventive effect on tomato whiteflies [Vegetables, 2019(02):48-51.]. Studies have shown that d-limonene has an antibacterial effect on some bacilli and cocci [Nutrition & Agriculture, 2015], and is also active against a small number of fungi, such as: Penicillium digitatum [Xiangtan University, 2015.], Bacillus subtilis, Pseudomonas aeruginosa, Aspergillus niger, Fusarium moniliforme, etc. [Zhejiang Agricultural Sciences, 2013(1):73-74.].

[0010] Eugenol [Chemistry and Chemical Engineering Dictionary, 2003]; CAS No.: 97-53-0; English name: eugenol; Molecular formula: C 10 H 12 O2; relative molecular weight 164.1. Eugenol is extracted from plant metabolites such as clove oil and cinnamon leaf oil. Studies have shown that eugenol has a certain preventive effect on mung bean leaf spot [Agricultural Science and Technology Newsletter, 2021(4):102-105.], pepper blight [Yangtze River Vegetables, 2011(24):55-56.], potato black mole fungus and potato early blight fungus [Heilongjiang Agricultural Sciences, 2021(11):35-38.]. Studies have shown that eugenol has a certain preventive effect on tomato yellow leaf curl virus [Jiangxi Journal of Agricultural Sciences, 2013, 25(9):78-80.]. It has been commercialized in chemical control, such as: 0.3% eugenol soluble solution is used to control tomato late blight, tomato gray mold, grape downy mildew, potato late blight and ornamental peony gray mold. 20% eugenol water emulsion is used to control tomato virus diseases.

[0011] Citronellal and citronellol have right-hand and left-hand isomers. Citronellal [Applied Chemistry, 1992(02)]; CAS No.: 106-23-0; English name: Citronellal; Molecular formula: C 10 H 18O; relative molecular weight 154.249. Citronellol [Chemical Industry Press, 2008]; CAS number: 106-22-9; English name: Citronellol; Molecular formula: C 10 H 20 O; relative molecular weight 156.26. Studies have shown that citronellal and citronellol have a significant fumigating effect on corn weevils, Indian meal borers, green bean weevils, red flour beetles, and mealworms. They also have an inhibitory effect on corn weevils larvae and eggs [Journal of Zhengzhou Grain College, 1994, 15(1):39-47.]. Studies have shown that citronellal has an inhibitory effect on the growth of Pseudomonas aeruginosa [Ecological Science, 2021, 40(4):27-35.] and tea anthracnose pathogens [Tea Science, 2019, 39(4):425-430.].

[0012] Due to its wide range of biological activities and environmental friendliness, sanguinarine has been widely studied in agriculture, and many documents have disclosed its application in the agricultural field.

[0013] Patent CN109645002A discloses a pesticide composition of D-limonene compounded with a number of active ingredients, including D-limonene compounded with neonicotinoids and diamide insecticides, but does not describe the control scheme and effect of D-limonene compounded with plant-derived compounds; Patent CN113134031A discloses a composition of Macleaya cordata extract with cinnamaldehyde, thymol, eugenol, carvacrol, peppermint oil, and eucalyptus oil, wherein the Macleaya cordata extract contains 0.8-1.3% sanguinarine as a It is a feed additive for preventing and treating coccidia; Patent CN109833296A discloses a combination of thymol, eugenol, methyl eugenol, carvacrol, cinnamaldehyde, chelerythrine and sanguinarine as a feed additive for preventing and treating chiggers in chickens; Patent CN113491740B discloses a combination of a plant essential oil composition and a plant extract, wherein the plant essential oil includes citrus oil, cinnamaldehyde, etc., and the plant extract includes a Macleaya cordata extract, etc., as a feed additive for preventing and treating Candida albicans from pigeons. The sanguinarine and plant extract compositions disclosed in the above documents are all used as feed additives in the breeding industry to prevent and treat coccidia, mites or pathogenic bacteria in livestock and poultry farming, and do not involve pest control in the field of crops, which is significantly different from the scope of the invention described in the present invention.

[0014] Patent CN105532682B discloses a pesticide composition of veratridine with sanguinarine, triptolide, and wolfberry toxin, which is used to control crop pests such as wolfberry psyllids, jujube red spiders, jujube gall midges, cabbage worms, cucumber whiteflies, wolfberry aphids, and tomato whiteflies; Patent CN101518249B discloses a pesticide composition of sanguinarine from Macleaya cordata extract, nicotine from tobacco extract, tea saponins from tea oil cake extract, and natural borneol from borneol camphor extract, which is used to control crop pests such as aphids, rice planthoppers, or cabbage greens. Patent CN105494380A discloses a pesticide composition of sanguinarine with amino oligosaccharides, osthole, spinosad, artemisinin, azadirachtin, triptolide, wolfberry toxin, scopolamine, and matrine, which is used to control a variety of crop pests and diseases, such as watermelon wilt, wolfberry aphids, wolfberry thrips, wolfberry psyllids, wolfberry red spiders, jujube tree gall midges, cucumber downy mildew, etc. Patent CN110012909A discloses a pesticide composition of sanguinarine with pyrethrins, celangulin, sodium pinealate, eucalyptol, and tea saponin. , used to control a variety of crop pests and diseases, such as: aphids, pear psyllids, two-spotted spider mites, cabbage worms, scale insects, thrips, leafhoppers, beet armyworms, etc.; Patent CN106577788A discloses a pesticide composition of sanguinarine with nicotine, chelerythrine, leucanthemum, ramie oil, salicylic acid, etc., for controlling aphids, rice planthoppers, etc.; Patent CN108812715A discloses a pesticide composition of various plant extracts such as Macleaya cordata and plant essential oils, wherein the plant extract is an ethanol extract after drying and crushing, including tassels Dan, chamomile, American pokeweed, airplane grass, white wormwood, lemon peel, white clover, tung oil fruit, pearly root, Angelica dahurica, etc., plant essential oils include tung oil leaf oil, clove basil essential oil, forsythia oil, schisandra essential oil, wild mint essential oil, eucalyptus oil, etc., which is a special botanical insecticide for winter peach; Patent CN105981750A discloses a combination of macleaya powder with camphor leaf oil, eucalyptus oil, rose oil, tangerine peel powder, fennel powder, ethanol extract of cupulaa odorata, and fresh ethanol extract of citronella, as a fertilizer additive for repelling plant pests.

[0015] The above patent documents disclose multiple compositions of sanguinarine and plant extracts for use in the prevention and control of crop diseases and insect pests in agriculture. These disclosed compositions have good environmental compatibility and are not prone to resistance. When combined, they can enhance activity against a variety of crop diseases and insect pests, thereby reducing the dosage of the drug. The active ingredients in these compositions are different from the plant extracts contained in Compound A disclosed in the present invention. Therefore, the present invention and the disclosed patents have significant differences in multiple aspects such as the composition, ratio, total content, method of use, and scope of use of the composition.

[0016] In the composition of the present invention, sanguinarine is an alkaloid compound, and the plant essential oil is a plant extract containing carbon and hydrogen or carbon, hydrogen and oxygen elements. The different chemical structures and mechanisms of action enable their combined use to achieve synergistic efficacy and expand the control spectrum. The plant essential oil's ability to easily penetrate the surface of crops promotes rapid absorption of sanguinarine by the crops, effectively reducing the insect population or bacterial population in the early stages of pests and diseases, achieving better control effects with a lower dose of pesticide preparation, and facilitating resistance management of crop pests and diseases.

[0017] The technical solution disclosed in the present invention provides a new solution to the current serious resistance situation in agricultural pest control. The combined application of two types of plant-based pesticides has positive significance for green prevention and control in agricultural planting and the "reduction and increase in efficiency" of pesticides. Summary of the Invention

[0018] The invention discloses an agricultural composition, in particular a composition of sanguinarine and plant essential oil A for agricultural use, and a preparation method and application scheme thereof.

[0019] Among them, sanguinarine includes one or more of sanguinarine, sanguinarine inorganic salts and sanguinarine organic salts. Sanguinarine inorganic salts include sanguinarine sulfate, sanguinarine hydrochloride, sanguinarine nitrate and sanguinarine phosphate, etc. Sanguinarine organic salts include sanguinarine citrate, sanguinarine acetate, sanguinarine propionate, sanguinarine citrate and sanguinarine malate, etc.

[0020] Among them, plant essential oil A is a biologically active substance extracted from plant sources, specifically including d-limonene, eugenol, citronellal, α-pinene, terpinolene, geranial, 4-terpineol, nerolidol, menthone, anethole, thymol, carvacrol, myrcene and β-caryophyllene. These active substances come from the corresponding plants, and the extraction methods have been reported.

[0021] The active ingredients of the composition include sanguinarine and compound A, wherein compound A is a plant essential oil. The weight ratio of sanguinarine to compound A is 69:1-1:149, and the total weight percentage of sanguinarine and compound A in the composition is 2%-76%.

[0022] Furthermore, the active ingredients of the composition include sanguinarine and plant essential oil A, the weight ratio of sanguinarine to plant essential oil A is 39:1-1:129, and the total weight percentage of sanguinarine and plant essential oil A in the sterilization composition is 2%-50%. Plant essential oil A includes d-limonene, eugenol, citronellal, and carvacrol.

[0023] The composition can be formulated into various pesticide formulations, including wettable powders, soluble powders, water-dispersible granules, soluble granules, tablets, emulsifiable concentrates, emulsions in water, microemulsions, suspoemulsions, suspension concentrates, dispersible oil suspensions, microcapsule suspensions, soluble concentrates, and suspension seed coatings. For definitions of various formulations, types of adjuvants, their usage and dosage, and preparation and related application techniques, please refer to "Modern Pesticide Formulation Processing Technology" (2013, Chemical Industry Press).

[0024] Among them, the preparation and processing of the dosage form of the composition contains commonly used auxiliary materials required for the preparation of pesticide formulations. The auxiliary materials are a mixture of one or more of solvents, emulsifiers, wetting agents, dispersants, thickeners, pH regulators, stabilizers, defoaming agents, antifreeze agents and fillers. The application of these auxiliary materials is to achieve the stability of the physical properties of the dosage form and achieve the field application effect. The types, functions, and application techniques of the auxiliary materials are referred to in "Pesticide Adjuvants" (2018, Chemical Industry Press).

[0025] The composition is used to prevent and control agricultural pests and diseases, including phytophagous mites, phytophagous nematodes, lepidopteran pests, dipteran pests, coleopteran pests, hemiptera pests, thysanitary pests and fungal diseases. The herbivorous mites include the panonychus mite, cotton spider mite, cinnabarinus spider mite, two-spotted spider mite, hawthorn spider mite, etc.; the herbivorous nematodes include tobacco root knot nematodes, soybean cyst nematodes, southern root knot nematodes, potato stem nematodes, etc.; the lepidopteran pests include the diamondback moth, beet armyworm, Spodoptera litura, fall armyworm, two-spotted armyworm, etc.; the dipteran pests include the pea leafminer, bean stalk blackminer, citrus leafminer, rice leafminer, citrus fruit fly, melon fruit fly, citrus fruit fly, etc.; the coleopteran pests include rhinoceros beetles and their larvae, grubs, click beetles, stag beetles, melon beetles, sweet potato leaf beetles, small blue beetles, etc.; the hemiptera pests include brown planthoppers, gray planthoppers, white-backed planthoppers , rice planthoppers, whiteflies, Bemisia tabaci, peach aphids, wheat aphids, wheat bifurcated aphids, cotton aphids, apple aphids, scale insects, etc.; the Thysanoptera pests include rice thrips, western flower thrips, melon thrips, onion thrips, etc.; the sanitary pests include gadflies, gall midges, Anopheles gambiae, Culex pipiens, Aedes, etc.; the fungal diseases include cucumber powdery mildew, zucchini powdery mildew, cucumber downy mildew, melon downy mildew, grape downy mildew, cucumber gray mold, lettuce gray mold, etc., and the pathogens include the Powdery Mildewales order of the Ascomycota, the genera Sporozoites, Peronospora, Pseudocypsum, and Monosporus in the Ascomycota, such as: melon powdery mildew, Cuban pseudoperonospora, northeastern mold, grape monosporus, and botrytis cinerea.

[0026] The composition provided by the present invention can be used to control crop diseases and insect pests, wherein the crops are selected from food crops, cash crops, fruit trees, vegetables, and medicinal crops. Food crops include corn, rice, wheat, sorghum, etc.; cash crops include peanuts, cotton, rapeseed, sesame, tea, alfalfa, etc.; fruit trees include citrus, apples, pears, kiwis, hawthorns, etc.; vegetables include Solanaceae crops such as eggplant and tomato, Cucurbitaceae crops such as cucumber, early melon, and zucchini, and Cruciferae crops such as cabbage and pakchoy; and medicinal crops include ginseng, wolfberry, and astragalus.

[0027] The composition provided by the present invention can be applied to plants, plant parts, plant propagation materials and subsequent plant organs, soil or cultivation media, materials, or spaces, acting on larvae, adults, and other insect structures, as well as spores, hyphae, asci, and other bacterial structures of plant pathogens. Application to these locations can achieve control of corresponding crop diseases and insect pests.

[0028] The composition provided by the present invention is usually applied to plants, plant propagation materials and subsequently grown plant organs, cultivation media, materials or spaces in an agronomically effective and substantially non-phytotoxic application amount by methods such as seed dressing, root irrigation, flushing, soil mixing, fertilizer mixing, soaking, dripping, pouring, spraying, spraying, dusting, spreading and fumigation to achieve the prevention and control of diseases and insect pests.

[0029] Compared with the prior art, the composition of the present invention has the following characteristics:

[0030] 1. Diverse control targets: The composition has control effects on mites, pests, nematodes and pathogenic fungi, with diverse target types and a wide range of control.

[0031] 2. Significant synergistic effect: The combination of sanguinarine and plant essential oils has a significant synergistic effect. Compared with a single dose, the prevention and control effect on insects and pathogens is improved.

[0032] 3. Delaying drug resistance: Sanguinarine and plant essential oils belong to different categories in the classification of mechanism of action, and their targets are quite different, so they are less likely to cause resistance accumulation in target pests or fungi.

[0033] 4. Reduced prevention and control costs: The combination has the characteristics of increasing efficiency and reducing dosage and expanding the prevention and control spectrum, reducing the application frequency and dosage of pesticides, saving labor and time, and reducing the prevention and control costs of pests and diseases.

[0034] 4. Environmentally friendly: Biological pesticides made from plant extracts are safe for humans and animals, have low toxicity to non-target organisms, and have low residues in soil and water. DETAILED DESCRIPTION

[0035] The present invention refers to the industry standards NY / T 1154.7-2006 "Guidelines for Indoor Bioassay Tests of Pesticides - Insecticides - Part 7: Determination of Combined Effects of Mixtures" and NY / T 1156.6-2006 "Guidelines for Indoor Bioassay Tests of Pesticides - Fungicides - Part 6: Determination of Combined Effects of Mixtures". Based on a large number of indoor bioassays, formulation and field efficacy tests, the present invention is further completed by exploring the compounding of sanguinarine.

[0036] In order to better understand the essence of the present invention, the following examples further illustrate the present invention, but they should not be construed as limiting the present invention. The contents mentioned in the examples are not limitations of the present invention, and the selection of material formulations can be adapted to local conditions without having a substantial impact on the results. In these examples, unless otherwise stated, all percentages are weight percentages.

[0037] Indoor activity determination method:

[0038] The inventors demonstrated indoor activity determination using toxicity tests on citrus mite (Panonychus citri (McGregor)), apple spider mite (Panonychus ulmi (Koch)), diamondback moth (Plutella xylostella (Linnaeus)), southern root-knot nematode (Meloidogyne incongnita (Kofold & White) Chitwood) and melon powdery mildew (Sphaerotheca fuliginea. (Sch.) Poll) as examples.

[0039] Toxicity curve and co-toxicity coefficient

[0040] The test and calculation were conducted with reference to the Agricultural Industry Standards of the People's Republic of China NY / T 1154.7-2006 "Guidelines for Indoor Bioassay Tests of Pesticides - Insecticides - Part 7: Determination of the Combined Effects of Mixtures" and NY / T 1156.6-2006 "Guidelines for Indoor Bioassay Tests of Pesticides - Fungicides - Part 6: Determination of the Combined Effects of Mixtures":

[0041]

[0042] Theoretical toxicity index (TTI)

[0043] =Agent A's measured toxicity index × A's percentage in the mixture

[0044] + Actual toxicity index of agent B × percentage of agent B in the mixture

[0045]

[0046] The co-toxicity coefficient (CTC) of the mixture was calculated according to the Sun Yunpei method to evaluate the type of combined effect. A CTC ≥ 120 indicates a synergistic effect, a CTC ≤ 80 indicates an antagonistic effect, and a CTC between 80 and 120 indicates an additive effect.

[0047] Panonychus citri (McGregor) and Panonychus ulmi (Koch)

[0048] The test was conducted with reference to the modified method of the Agricultural Industry Standard of the People's Republic of China NY / T 1154.12-2008 "Guidelines for Indoor Bioassay Tests of Pesticides - Insecticides Part 12: Spider Mite Slide Dipping Method":

[0049] 1. Experimental purpose: To screen the indoor toxicity of different compound combinations to Panonychus citri;

[0050] 2. Experimental conditions

[0051] 2.1. Test Targets: Panonychus citri (McGregor) and Panonychus ulmi (Koch)

[0052] 2.2. Culture conditions: constant temperature and light incubator at 25°C, photoperiod L:D = 16:8h;

[0053] 2.3. Experimental instruments: electronic scale, microscope, culture dish, pipette, funnel, constant temperature and light incubator, writing brush;

[0054] 3. Test methods

[0055] 3.1. Select female adult mites of relatively consistent growth status and stage for indoor culture. Use a brush to pick up active, uniform-sized female mites. Place their backs on the adhesive backing of glass slides, 30 per slide. Place them on an enamel tray lined with moist filter paper and incubate in a constant-temperature incubator. After 2 hours, examine under a microscope. Remove any dead or injured individuals and replenish the remaining mites with 30.

[0056] 3.2. Dissolve the original drug in deionized water or an organic solvent (such as acetone, chloroform, ethanol, etc.), then dilute with an aqueous solution containing an appropriate amount of a surfactant (such as 0.1% Tween 80 or 0.1% Triton-X100). Prepare separate single-dose stock solutions and set a dilution concentration gradient for the test drug based on the purpose of the mixture and the drug's activity. Conduct preliminary tests on mixtures of varying ratios. Based on this, determine the test concentration range for each mixture. For each drug, set five concentrations based on the active ingredient content, with three replicates, and use a solvent solution containing no drug as a control.

[0057] 3.3. Tetranychus slide immersion method: Place the slide in the prepared solution and gently shake for 5 seconds. Remove the slide and remove the excess solution with absorbent paper. Place the slide on a white porcelain plate lined with wet filter paper and place in a constant temperature incubator for observation. Maintain humidity during the incubation period.

[0058] 4. Test investigation and calculation method:

[0059] 48 hours after drug application, check the death of insects (death is defined as the insects not moving when touched by their stingers), record the total number of insects surveyed and the number of dead insects in the treatment group and the control group, and calculate the corrected mortality rate.

[0060]

[0061]

[0062] Diamondback moth (Plutella xylostella (Linnaeus))

[0063] The test was conducted with reference to the Agricultural Industry Standard of the People's Republic of China NY / T 1154.2-2006 "Guidelines for Indoor Bioassay of Pesticides - Insecticides Part 2: Stomach Toxicity Test - Poisoned Leaf Method":

[0064] 1. Experimental purpose: To screen the indoor toxicity of different compound combinations to Plutella xylostella;

[0065] 2. Experimental conditions

[0066] 2.1. Test Target: Diamondback Moth (Plutella xylostella (Linnaeus))

[0067] 2.2. Culture conditions: constant temperature and light incubator at 25°C, photoperiod L:D = 16:8h;

[0068] 2.3. Experimental instruments: electronic scale, centrifuge, binoculars, incubation screen, culture dish, pipette, funnel, constant temperature and light incubator;

[0069] 3. Test methods

[0070] 3.1. Diamondback moths collected from the field were reared indoors to the F1 generation, and third-instar larvae of uniform size were selected for the experiment.

[0071] 3.2. Dissolve the original drug in deionized water or an organic solvent (such as acetone, chloroform, ethanol, etc.), then dilute with an aqueous solution containing an appropriate amount of a surfactant (such as 0.1% Tween 80 or 0.1% Triton-X100). Prepare separate single-dose stock solutions and set a dilution concentration gradient for the test drug based on the purpose of the mixture and the drug's activity. Conduct preliminary tests on mixtures of varying ratios. Based on this, determine the test concentration range for each mixture. For each drug, set five concentrations based on the active ingredient content, with three replicates, and use a solvent solution containing no drug as a control.

[0072] 3.3. After removing the main veins from fresh broccoli leaves, punch them into 10 mm diameter discs using a hole punch. Immerse these discs in different concentrations of the drug solution for 30 seconds, remove them, air dry, and place them in a 24-well plate. Inoculate the plates with 30 third-instar larvae of uniform growth status, covering each treatment with sterilized toilet paper to maintain moisture. After 48 hours, examine each treatment group for the number of dead larvae. Three replicates were established, and a treatment without the drug served as a control.

[0073] 4. Test investigation and calculation method:

[0074] 48 hours after drug application, check the mortality of the third-instar larvae (death is defined as the insect not moving when touched by the stinger), record the total number of insects surveyed and the number of dead insects, and calculate the corrected mortality rate.

[0075]

[0076]

[0077] Southern root-knot nematode (Meloidogyne incongnita (Kofold & White) Chitwood)

[0078] The test was conducted with reference to the Agricultural Industry Standard of the People's Republic of China NY / T 1154.6-2006 "Guidelines for Indoor Bioassay Tests of Pesticides - Insecticides Part 6: Insecticide Activity Test - Immersion Method":

[0079] 4. Experimental purpose: To screen the indoor toxicity of different compound combinations to root-knot nematodes;

[0080] 5. Experimental conditions

[0081] 2.1. Test Target: Southern Root-Knot Nematode (Meloidogyne incongnita (Kofold & White) Chitwood)

[0082] 2.2. Culture conditions: constant temperature and light incubator temperature 16.0°C, photoperiod L:D = 16:8h;

[0083] 2.3. Experimental instruments: electronic scale, centrifuge, binoculars, incubation screen, culture dish, pipette, funnel, constant temperature and light incubator, multi-well biochemical test plate;

[0084] 6. Test methods

[0085] 3.1. Select tomato root nodules that are relatively consistent in growth status and stage during indoor culture for the experiment. Using a binocular microscope, select white egg masses and place them in an incubation sieve at 25°C. After microscopic examination, adjust the nematode suspension to a concentration of 100 nematodes / mL (based on the number of second-instar larvae) and set aside.

[0086] 3.2. Dissolve the original drug in deionized water or an organic solvent (such as acetone, chloroform, ethanol, etc.), then dilute with an aqueous solution containing an appropriate amount of a surfactant (such as 0.1% Tween 80 or 0.1% Triton-X100). Prepare separate single-dose stock solutions and set a dilution concentration gradient for the test drug based on the purpose of the mixture and the drug's activity. Conduct preliminary tests on mixtures of varying ratios. Based on this, determine the test concentration range for each mixture. For each drug, set five concentrations based on the active ingredient content, with three replicates, and use a solvent solution containing no drug as a control.

[0087] 3.3. Using the immersion method, pipette 3 mL of the drug solution, starting from low to high concentration, into each test tube. Then, pipette an equal volume of 3 mL of the prepared nematode suspension into the test tube. Mix the drug solution and nematode suspension equally. Pipette 3 mL of this mixture into the wells of a multi-well biochemical assay plate, seal, and incubate. Set up three replicates, and include a treatment without the drug as a control.

[0088] 4. Test investigation and calculation method:

[0089] 24 hours after application, check the death of second-instar larvae of root-knot nematodes (death is defined as the absence of bending when the insect pin is touched). Take 1 mL of the mixture from each treatment and observe the death of nematodes under a dissecting microscope. Record the total number of nematodes surveyed and the number of dead nematodes to calculate the corrected mortality rate.

[0090]

[0091]

[0092] Melon powdery mildew (Sphaerotheca fuliginea.(Sch.)Poll)

[0093] The test was conducted with reference to the Agricultural Industry Standard of the People's Republic of China NY / T 1156.11-2008 "Guidelines for Indoor Bioassay Tests of Pesticides - Fungicides Part 11: Pot Method for Control of Cucumber Powdery Mildew". The test was conducted using the leaf disc dip method improved by Hao Yongjuan et al. [Hao Yongjuan, Wang Wanli, Liu Chunyan, Wang Yong. Improvement of Bioassay Technology for Cucumber Powdery Mildew [J]. Tianjin Agricultural Science, 2005, 11(3): 37-40.]

[0094] 1. Experimental purpose: To screen the indoor toxicity of different compound combinations against powdery mildew of melons;

[0095] 2. Experimental conditions

[0096] 2.1. Test target: Melon powdery mildew fungus (Sphaerotheca fuliginea. (Sch.) Poll)

[0097] 2.2. Culture conditions: Constant temperature incubator, temperature 24°C, photoperiod L:D = 16:8h;

[0098] 2.3. Experimental instruments: electronic balance, shaking incubator, culture dish, conical flask, pipette, constant temperature incubator;

[0099] 3. Test methods

[0100] 3.1. Prepare cucumber seedlings cultured at different times for strain transfer. Shake the new strain into powder or brush it onto healthy cucumber leaves with a wet brush, place it in a culture dish with water at the bottom, cover it and place it in a constant temperature incubator.

[0101] 3.2. Inoculation of spore suspension: Collect fresh powdery mildew leaves and moisturize them for culture. After the spores are fully developed, brush them into sterile water containing 0.5% Tween 80 with a brush and adjust the spore concentration of the bacterial suspension to (6-10)×10 4 / mL, spray evenly on the leaves for inoculation.

[0102] 3.3 Dissolve the original drug in deionized water or an organic solvent (such as acetone, chloroform, ethanol, etc.), then dilute with an aqueous solution containing an appropriate amount of surfactant (such as 0.1% Tween 80 or 0.1% Triton-X100). Prepare separate single-dose stock solutions and set a dilution concentration gradient for the test drug based on the purpose of the mixture and the drug's activity. Conduct preliminary tests on mixtures of varying ratios. Based on this, determine the test concentration range for each mixture. For each drug, set five concentrations based on the active ingredient content, with three replicates, and use a solvent solution containing no drug as a control.

[0103] 3.4. Leaf disc dip method: Soak leaf discs in different concentrations of the drug solution, let them dry, and place them face up on filter paper soaked in the drug solution. Cover and place them in a light incubator for 7-10 days, then observe the disease status.

[0104] 4. Test investigation and calculation method:

[0105] Lesion grading standards:

[0106]

[0107] Calculation method of drug efficacy:

[0108]

[0109]

[0110] Indoor activity assay Example 1: Sanguinarine and d-limonene against Panonychus citri

[0111] The inventors conducted a large number of mixing experiments and demonstrated the toxicity of five ratios of sanguinarine to d-limonene, 39:1, 19:1, 1:1, 1:19, and 1:39. Five ratios and five doses of sanguinarine to d-limonene were used to test the efficacy of the spider mite slide dip method on Panonychus citri. The toxicity baseline and LC of each ratio were obtained through data analysis. 50 The evaluation of their combined effects on Panonychus citri is shown in Table 1:

[0112] Table 1 Evaluation of the combined effects of five combinations of sanguinarine and d-limonene on Panonychus citri

[0113]

[0114] As shown in Table 1, sanguinarine and d-limonene have insecticidal activity against Panonychus citri. 50 The LC value of d-limonene's insecticidal activity against Panonychus citri was 8.828 mg / L. 50 It is 16.29 mg / L.

[0115] As shown in Table 1, the co-toxicity coefficients of the five ratios of sanguinarine and d-limonene ranged from 113.39 to 128.25. Among them, the co-toxicity index values ​​of the sanguinarine: d-limonene ratios of 39:1 and 19:1 were 128.25 and 124.42, respectively, showing a synergistic effect.

[0116] Indoor activity assay Example 2: Sanguinarine and d-limonene against apple spider mites

[0117] The inventors conducted a large number of mixing tests and demonstrated the toxicity of five ratios of sanguinarine to d-limonene, 39:1, 19:1, 9:1, 1:1, and 1:9. Five ratios and five doses of sanguinarine to d-limonene were used to test the efficacy of the spider mite slide dip method on apple spider mites. The toxicity baseline and LC values ​​of each ratio were obtained through data analysis.50 The evaluation of their combined effects on apple spider mites is shown in Table 2:

[0118] Table 2 Evaluation of the combined effects of five combinations of sanguinarine and d-limonene on apple spider mites

[0119]

[0120] As shown in Table 2, sanguinarine and d-limonene have insecticidal activity against apple spider mites. 50 The LC value of d-limonene's insecticidal activity against apple spider mites is 8.385 mg / L. 50 It is 19.80mg / L.

[0121] As shown in Table 2, the co-toxicity coefficients of the five ratios of sanguinarine and d-limonene ranged from 99.51 to 123.79. Among them, the co-toxicity index values ​​of the sanguinarine: d-limonene ratios of 19:1 and 39:1 were 122.05 and 123.79, respectively, showing a synergistic effect.

[0122] Indoor activity assay Example 3: Sanguinarine and d-limonene against Plutella xylostella

[0123] The inventors conducted a large number of mixing experiments and demonstrated the toxicity of five ratios of sanguinarine to d-limonene, 1:1, 1:19, 1:39, 1:59, and 1:99. Five ratios and five doses of sanguinarine to d-limonene were used to test the efficacy of the leaf clip method on the diamondback moth. The toxicity baseline and LC value of each ratio were obtained through data analysis. 50 The combined effect evaluation on the diamondback moth is shown in Table 2:

[0124] Table 3 Evaluation of the combined effects of five combinations of sanguinarine and d-limonene on Plutella xylostella

[0125]

[0126]

[0127] As shown in Table 3, sanguinarine and d-limonene have insecticidal activity against Plutella xylostella. 50 The LC value of d-limonene's insecticidal activity against Plutella xylostella is 249.8 mg / L. 50 It is 83.29 mg / L.

[0128] As shown in Table 3, the co-toxicity coefficients of the five ratios of sanguinarine and d-limonene ranged from 84.48 to 134.33. Among them, the co-toxicity index values ​​of the sanguinarine:d-limonene ratios of 1:39 and 1:59 were 124.86 and 134.33, respectively, showing a synergistic effect.

[0129] Indoor activity assay Example 4: Sanguinarine and limonene against incognita root-knot nematodes

[0130] The inventors conducted a large number of mixing tests and demonstrated the toxicity of five ratios of sanguinarine to d-limonene, namely 9:1, 1:1, 1:9, 1:19, and 1:59. The five ratios and five doses of sanguinarine to d-limonene were used to test the efficacy of the southern root-knot nematode by the insect immersion method. The toxicity baseline and LC value of each ratio were obtained through data analysis. 50 The combined effect evaluation on southern root-knot nematode is shown in Table 2:

[0131] Table 4 Evaluation of the combined effects of five combinations of sanguinarine and d-limonene on the southern root-knot nematode

[0132]

[0133] As shown in Table 4, sanguinarine and d-limonene have insecticidal activity against southern root-knot nematodes. 50 The LC value of d-limonene's insecticidal activity against southern root-knot nematodes is 151.3 mg / L. 50 It is 180.3mg / L.

[0134] As shown in Table 4, the co-toxicity coefficients of the five ratios of sanguinarine and d-limonene ranged from 102.49 to 136.27. Among them, the co-toxicity index values ​​of the sanguinarine: d-limonene ratios of 1:1 and 1:9 were 134.75 and 136.27, respectively, showing a synergistic effect.

[0135] Indoor activity test example 5: Sanguinarine and limonene against powdery mildew fungus of melons

[0136] The inventors conducted extensive mixing experiments and demonstrated the toxicity of five ratios of sanguinarine to d-limonene (19:1, 1:1, 1:19, 1:39, and 1:99). The five ratios and five doses of sanguinarine to d-limonene were used to test the efficacy of powdery mildew on melons using the leaf disc dip method. The toxicity baseline and LC values ​​for each ratio were obtained through data analysis. 50 The evaluation of their combined effects on melon powdery mildew is shown in Table 2:

[0137] Table 5 Evaluation of the combined effects of five compound ratios of sanguinarine and d-limonene on powdery mildew of melons

[0138]

[0139] As shown in Table 5, sanguinarine and d-limonene have bactericidal activity against powdery mildew of melons. 50The EC value of d-limonene against powdery mildew of melons is 35.58 mg / L. 50 It is 29.26 mg / L.

[0140] As shown in Table 5, the co-toxicity coefficients of the five ratios of sanguinarine and d-limonene ranged from 88.80 to 130.06. Among them, the co-toxicity index values ​​of the sanguinarine:d-limonene ratios of 1:39 and 1:99 were 124.17 and 130.06, respectively, showing a synergistic effect.

[0141] According to the results of the toxicity test, the inventors prepared compound preparations and selected some of them to display the results.

[0142] Preparation Application Example 1: 10% sanguinarine·d-limonene wettable powder (0.5:9.5)

[0143] The composition of 10% sanguinarine·d-limonene wettable powder is shown in Table 6:

[0144] Table 6 Components of 10% sanguinarine·d-limonene wettable powder

[0145]

[0146] According to the components listed in Table 6, the carrier, active ingredient 1, and active ingredient 2 were mixed for 10 minutes using a zero-gravity mixer. A wetting agent, a dispersant, and a filler were added in order and mixed for 10 minutes. The mixture was then subjected to air flow milling until D98 was ≤ 30 μm to obtain a 10% sanguinarine·d-limonene wettable powder of the present invention. The composition was tested to meet all product standards and was a qualified product.

[0147] Preparation Application Example 2: 8% sanguinarine·d-limonene soluble solution (7.8:0.2)

[0148] The composition of 8% sanguinarine·d-limonene soluble solution is shown in Table 7:

[0149] Table 7 Components of 8% Sanguinarine·d-limonene soluble solution

[0150]

[0151] According to the components detailed in Table 7, active ingredient 2, a cosolvent, and an emulsifier were added to a stirred kettle in this order and mixed for 10 minutes. After the mixture was uniformly clarified, active ingredient 1, a defoamer, an antifreeze agent, and a solvent were added. Stirring was continued for 10 minutes until the mixture was completely uniform and clarified. This produced the 8% sanguinarine / d-limonene soluble solution of the present invention. Testing showed that the solution met all product standards and was qualified.

[0152] Preparation Application Example 3: 2% sanguinarine·d-limonene emulsifiable concentrate (1.9:0.1)

[0153] The composition of 2% sanguinarine·d-limonene emulsifiable concentrate is shown in Table 8:

[0154] Table 8 Components of 2% Sanguinarine·d-limonene emulsifiable concentrate

[0155]

[0156] According to the components detailed in Table 8, active ingredient 1, active ingredient 2, cosolvent, and solvent were placed in a stirred kettle in this order and stirred for 10 minutes until clear (heating was performed if necessary). An emulsifier was then added and stirred thoroughly for 10 minutes until the mixture was completely uniform and clear. This produced the 2% sanguinarine / d-limonene emulsifiable concentrate of the present invention. Testing showed that the concentrate met all product standards and was qualified.

[0157] Preparation Application Example 4: 20% sanguinarine·d-limonene wettable powder (19.5:0.5)

[0158] The composition of 20% sanguinarine·d-limonene wettable powder is shown in Table 9:

[0159] Table 9 Components of 20% Sanguinarine·d-limonene Wettable Powder

[0160]

[0161]

[0162] According to the components detailed in Table 9, the carrier, active ingredient 1, and active ingredient 2 were mixed in a zero-gravity mixer for 10 minutes. A wetting agent, dispersant, and filler were added in order and mixed for 10 minutes. The mixture was then subjected to airflow milling to a particle size D98 ≤ 30 μm to produce the 20% sanguinarine / d-limonene wettable powder of the present invention. Testing showed that the product met all product standards and was qualified.

[0163] Preparation Application Example 5: 30% sanguinarine·d-limonene soluble solution (0.5:29.5)

[0164] The composition of 30% sanguinarine·d-limonene soluble solution is shown in Table 10:

[0165] Table 10 Components of 30% Sanguinarine·d-limonene Soluble Solution

[0166]

[0167] According to the components detailed in Table 10, active ingredient 2, a cosolvent, and an emulsifier were added to a stirred kettle in this order and mixed for 10 minutes. After the mixture was uniformly clarified, active ingredient 1, a defoamer, an antifreeze agent, and a solvent were added. Stirring was continued for 10 minutes until the mixture was completely uniform and clarified. This produced the 30% sanguinarine / d-limonene soluble solution of the present invention. Testing showed that the solution met all product standards and was qualified.

[0168] Preparation Application Example 6: 40% sanguinarine·d-limonene soluble solution (1:39)

[0169] The composition of 40% sanguinarine·d-limonene soluble solution is shown in Table 11:

[0170] Table 11 Component details of 40% sanguinarine·d-limonene soluble solution

[0171]

[0172] According to the components detailed in Table 11, active ingredient 2, a cosolvent, and an emulsifier were added to a stirred kettle in this order and mixed for 10 minutes. After the mixture was uniformly clarified, active ingredient 1, a defoamer, an antifreeze agent, and a solvent were added. Stirring was continued for 10 minutes until the mixture was completely uniform and clarified. This produced the 40% sanguinarine / d-limonene soluble solution of the present invention. Testing showed that the solution met all product standards and was qualified.

[0173] Preparation Application Example 7: 40% sanguinarine·d-limonene wettable powder (2:38)

[0174] The composition of 40% sanguinarine·d-limonene wettable powder is shown in Table 12:

[0175] Table 12 Components of 40% Sanguinarine·d-Limonene Wettable Powder

[0176]

[0177] According to the components detailed in Table 12, the carrier, active ingredient 1, and active ingredient 2 were mixed in a zero-gravity mixer for 10 minutes. A wetting agent, dispersant, and filler were added in order and mixed for 10 minutes. The mixture was then subjected to airflow milling to a particle size D98 ≤ 30 μm to produce the 40% sanguinarine / d-limonene wettable powder of the present invention. Testing showed that the composition met all product standards and was qualified.

[0178] Preparation Application Example 8: 27% sanguinarine·d-limonene soluble solution (13.5:13.5)

[0179] The composition of 27% sanguinarine·d-limonene soluble solution is shown in Table 13:

[0180] Table 13 Component details of 27% sanguinarine·d-limonene soluble solution

[0181]

[0182] According to the components detailed in Table 13, active ingredient 2, a cosolvent, and an emulsifier were added to a stirred kettle in this order and mixed for 10 minutes. After the mixture was uniformly clarified, active ingredient 1, a defoamer, an antifreeze agent, and a solvent were added. Stirring was continued for 10 minutes until the mixture was completely uniform and clarified. This produced the 27% sanguinarine / d-limonene soluble solution of the present invention. Testing showed that the solution met all product standards and was qualified.

[0183] Preparation Application Example 9: 20% sanguinarine·d-limonene soluble solution (0.2:19.8)

[0184] The composition of 20% sanguinarine·d-limonene soluble solution is shown in Table 37:

[0185] Table 14 Component details of 20% sanguinarine·d-limonene soluble solution

[0186]

[0187]

[0188] According to the components detailed in Table 14, active ingredient 2, a cosolvent, and an emulsifier were added to a stirred kettle in this order and mixed for 10 minutes. After the mixture was uniformly clarified, active ingredient 1, a defoamer, an antifreeze agent, and a solvent were added. Stirring was continued for 10 minutes until the mixture was completely uniform and clarified. This produced the 20% sanguinarine / d-limonene soluble solution of the present invention. Testing showed that the solution met all product standards and was qualified.

[0189] Preparation Application Example 10: 4% sanguinarine·d-limonene soluble solution (0.1:3.9)

[0190] The composition of 4% sanguinarine·d-limonene soluble solution is shown in Table 39:

[0191] Table 15 Components of 4% Sanguinarine·d-limonene Soluble Solution

[0192]

[0193] According to the components detailed in Table 15, active ingredient 2, a cosolvent, and an emulsifier were added to a stirred kettle in this order and mixed for 10 minutes. After the mixture was uniformly clarified, active ingredient 1, a defoamer, an antifreeze agent, and a solvent were added. Stirring was continued for 10 minutes until the mixture was completely uniform and clarified. This produced a 4.4% sanguinarine / d-limonene soluble solution of the present invention. Testing showed that the solution met all product standards and was qualified.

[0194] Preparation Application Example 11: 40% sanguinarine·eugenol wettable powder (1:39)

[0195] The composition of 16% sanguinarine·eugenol wettable powder is shown in Table 16:

[0196] Table 16 Components of 40% Sanguinarine and Eugenol Wettable Powder

[0197]

[0198] According to the components listed in Table 16, the carrier, active ingredient 1, and active ingredient 2 were mixed for 10 minutes using a zero-gravity mixer. A wetting agent, a dispersant, and a filler were added in sequence and mixed for 10 minutes. The mixture was then subjected to air flow milling until D98 was ≤ 30 μm to obtain the 40% sanguinarine·eugenol wettable powder of the present invention. The powder was tested to meet all product standards and was a qualified product.

[0199] Preparation excipient example 12: 4% sanguinarine·carvacrol soluble solution (0.1:3.9)

[0200] The composition of 4% sanguinarine and carvacrol soluble solution is shown in Table 17:

[0201] Table 17 Component details of 4% sanguinarine and carvacrol soluble solution

[0202]

[0203] According to the components listed in Table 17, the active ingredient 2, the cosolvent, and the emulsifier were placed in a stirred kettle in order and mixed for 10 minutes. After the material was uniformly clarified, the active ingredient 1, the defoamer, the antifreeze, and the solvent were added. Stirring was continued for 10 minutes until the material was completely uniformly clarified. The 4% sanguinarine·carvacrol soluble solution of the present invention was obtained. After testing, it met all product standards and was a qualified product.

[0204] Preparation excipient example 13: 25% sanguinarine·citronellal water dispersible granules (0.5:24.5)

[0205] The composition of 25% sanguinarine·citronellal water dispersible granules is shown in Table 18:

[0206] Table 18 Component details of 25% sanguinarine·citronellal water dispersible granules

[0207]

[0208] According to the components listed in Table 18, active ingredient 1, active ingredient 2, dispersant, wetting agent, defoaming agent, and filler were placed in a screw mixer and mixed for 10 minutes. The above materials were subjected to air flow pulverization to a D90 value of ≤25 μm. The pulverized materials were mixed with water in a mixer. The mixed materials were extruded into columnar particles with a diameter of 1.0 mm and dried with hot air at 90° C. until the moisture content was less than 3%. The 25% sanguinarine·citronellal water-dispersible granules of the present invention were obtained. The granules met all product standards and were qualified products after testing.

[0209] Preparation excipient example 14: 5% sanguinarine·α-pinene soluble solution (0.1:4.9)

[0210] The composition of 5% sanguinarine·α-pinene soluble solution is shown in Table 19:

[0211] Table 19 Components of 5% Sanguinarine·α-pinene soluble solution

[0212]

[0213]

[0214] According to the detailed components in Table 19, the active ingredient 2, the cosolvent, and the emulsifier were placed into a stirred kettle in order and mixed for 10 minutes. After the material was uniformly clarified, the active ingredient 1, the defoamer, and the solvent were added. Stirring was continued for 10 minutes until the material was completely uniform and clarified. The 5% sanguinarine·α-pinene soluble solution of the present invention was obtained. After testing, it met all product standards and was a qualified product.

[0215] Preparation Application Example 15: 24% sanguinarine·citronellol wettable powder (0.6:23.4)

[0216] The composition of 24% sanguinarine·citronellol wettable powder is shown in Table 20:

[0217] Table 20 24% Sanguinarine·Citronellol Wettable Powder Ingredients

[0218]

[0219] According to the components listed in Table 20, the carrier, active ingredient 1, and active ingredient 2 were mixed for 10 minutes using a zero-gravity mixer. A wetting agent, a dispersant, and a filler were added in sequence and mixed for 10 minutes. The mixture was then subjected to air flow milling until D98 was ≤ 30 μm to obtain the 24% sanguinarine·citronellol wettable powder of the present invention. The powder met all product standards and was found to be a qualified product after testing.

[0220] Preparation excipient example 16: 8% sanguinarine·4-terpineol soluble solution (0.2:7.8)

[0221] The composition of 8% sanguinarine·4-terpineol soluble solution is shown in Table 21:

[0222] Table 21 Components of 8% Sanguinarine·4-terpineol soluble solution

[0223]

[0224] According to the components listed in Table 21, active ingredient 2, cosolvent, and emulsifier were added to a stirred kettle in order and mixed for 10 minutes. After the material was uniformly clarified, active ingredient 1, defoamer, and solvent were added. Stirring was continued for 10 minutes until the material was completely uniformly clarified. To obtain the 8% sanguinarine·4-terpineol soluble solution of the present invention, the product was tested to meet all product standards and was a qualified product.

[0225] Product field efficacy method:

[0226] Based on the product formulation application examples, the inventors conducted field efficacy tests on the above formulation. The inventors conducted field efficacy tests on Panonychus citri (McGregor), Panonychus ulmi (Koch), Plutella xylostella (Linnaeus), Meloidogyne incongnita (Kofold & White) Chitwood, and Sphaerotheca fuliginea (Sch.) Poll, respectively. The standard description is as follows:

[0227] Panonychus citri (McGregor) and Panonychus ulmi (Koch)

[0228] 1. Experimental purpose: To investigate the control effect of different compound combinations on Panonychus citri and Tetranychus apple in the field;

[0229] 2. Targets: Panonychus citri (McGregor) and Panonychus ulmi (Koch)

[0230] 3. Application method and water consumption: normal foliage spray, water consumption per hectare is 1500L (100L / 667㎡)

[0231] 4. Plot arrangement, area and repetition:

[0232] The plots are arranged in random blocks, depending on the site, with a plot area of ​​approximately 200m 2, repeat 3 times.

[0233] 5. Test investigation and calculation method:

[0234] 5.1. Survey time: Survey the insect population base before spraying, and survey once 1, 5, and 7 days after spraying.

[0235] 5.2 Survey Method: A fixed-point survey method was used. Two citrus trees were surveyed in each plot. Each tree was marked at five points: east, south, west, north, and center. Five leaves were sampled from a branch at each point, for a total of 50 leaves per plot. The number of live mites on leaves was determined by the presence of insect stings, which were not affected by excessive movement, to avoid causing them to fall.

[0236] 5.3. Calculation Method of Drug Efficacy

[0237]

[0238]

[0239] Diamondback moth (Plutella xylostella (Linnaeus))

[0240] 1. Experimental purpose: To investigate the control effect of different compound combinations on the diamondback moth in the field;

[0241] 2. Target of control: Diamondback moth (Plutella xylostella (Linnaeus))

[0242] 3. Application method and water consumption: normal foliage spray, water consumption per hectare is 600L (30L / 667㎡)

[0243] 4. Plot arrangement, area and repetition:

[0244] The plots are arranged in random blocks, depending on the site, with a plot area of ​​approximately 30m 2 , repeat 3 times.

[0245] 5. Test investigation and calculation method:

[0246] 5.1. Survey time: Survey the insect population base before spraying, and survey once every 3, 5, and 7 days after spraying.

[0247] 5.2 Survey Method: Use a fixed-point survey method. Mark five points in each plot using the "five-point sampling method," surveying 20 rapeseed plants at each point. Check and record the number of live insects on leaves (the number of insects that remain motionless when touched by their stinger and whose body color remains unchanged).

[0248] 5.3. Calculation Method of Drug Efficacy

[0249]

[0250]

[0251] Southern root-knot nematode (Meloidogyne incongnita (Kofold & White) Chitwood)

[0252] 1. Experimental purpose: To investigate the control effect of different compound combinations on cucumber root-knot nematodes in the field;

[0253] 2. Target of control: Southern root-knot nematode (Meloidogyne incongnita (Kofold & White) Chitwood)

[0254] 3. Application method and water consumption: Normal foliage spray, water consumption per hectare is 900L (60L / 667㎡)

[0255] 4. Plot arrangement, area and repetition:

[0256] The plots are arranged in random blocks, depending on the site, with a plot area of ​​approximately 30m 2 , repeat 3 times.

[0257] 5. Test investigation and calculation method:

[0258] 5.1. Survey time: Surveys should be conducted before spraying and before pulling out the seedlings (60-80 days after spraying).

[0259] 5.2. Survey method: In each plot, 10 plants were randomly surveyed using the “five-point sampling method” to investigate the occurrence of nematodes in the roots.

[0260] Grading standards:

[0261]

[0262] 5.3. Calculation Method of Drug Efficacy

[0263]

[0264]

[0265] Melon powdery mildew (Sphaerotheca fuliginea.(Sch.)Poll)

[0266] 1. Experimental purpose: To investigate the control effect of different compound combinations on powdery mildew in bitter melon;

[0267] 2. Target: Powdery mildew of melons (Sphaerotheca fuliginea. (Sch.) Poll)

[0268] 3. Application method and water consumption: Normal foliage spray, water consumption per hectare is 1125L (75L / 667㎡)

[0269] 4. Plot arrangement, area and repetition:

[0270] The plots are arranged in random blocks, depending on the site, with a plot area of ​​approximately 30m 2 , repeat 3 times.

[0271] 5. Test investigation and calculation method:

[0272] 5.1. Investigation time: Investigations should be conducted before spraying, 10 days after the first spraying, 10 days after the second spraying, and 10 days after the third spraying.

[0273] 5.2. Survey method: In each plot, the number of lesions on 5 leaves was randomly surveyed using the “five-point sampling method”, avoiding sampling at the edge of the plot.

[0274] Lesion grading standards:

[0275]

[0276] 5.3. Calculation Method of Drug Efficacy

[0277]

[0278]

[0279] Product Field Efficacy Example 1: Field Efficacy Test for Controlling Panonychus citri

[0280] This experiment was conducted in Lijiang City, Yunnan Province. Approximately 200 mu (approximately 1,000 hectares) of citrus (including Wogan and Meiren) were cultivated outdoors. Irrigation and drainage conditions were normal, and management was routine. Pesticides were applied 8-10 times annually to control citrus spider mites, but low incidence persisted. Each plot was 4.0 m x 4.0 m tall, with each plant measuring 4.0 m. Cultivation conditions (citrus variety, soil type, water and fertilizer management, transplanting period, planting density, growing season, and water management) were relatively uniform across all experimental plots.

[0281] The test was conducted on five-year-old mandarin orange trees in the spring shoot phase. No other acaricides were applied 20 days before or during the test. The inventors designed the test plan based on the above-mentioned experimental investigation and calculation method, calculated the mite population reduction rate, and analyzed the control effect, as shown in Table 22:

[0282] Table 22 Design and results of field efficacy test on Panonychus citri

[0283]

[0284]

[0285] As shown in Table 22, mixed products of sanguinarine and d-limonene at different ratios were more effective against powdery mildew in the field than single agents of sanguinarine and d-limonene. Product Formulation Application Example 2 achieved optimal control at a 2667-fold dilution and an active ingredient dosage of 30 mg / L, achieving an average 7-day control efficacy of 88.00%.

[0286] Product Field Efficacy Example 2: Field Efficacy Test for Controlling Apple Spider Mites

[0287] This experiment was conducted in Zhaotong City, Yunnan Province. Approximately 400 mu (apple varieties) (including Red General, Shensha, and Honglu) were cultivated outdoors. Irrigation and drainage conditions were normal, and management was routine. Pesticides were applied 8-10 times annually to control spider mites, though outbreaks occurred occasionally. The plots were 4.0 m x 6.0 m per plant. Cultivation conditions (apple variety, soil type, water and fertilizer management, transplanting period, planting density, growing season, and water management) were relatively uniform across all experimental plots.

[0288] The test was conducted on seven-year-old red dew trees in the spring shoot-out stage. No other acaricides were applied 20 days before or during the test. The inventors designed the test plan based on the above-mentioned experimental investigation and calculation method, calculated the mite population reduction rate, and analyzed the control effect, as shown in Table 23:

[0289] Table 23 Design and results of field efficacy test on apple spider mite

[0290]

[0291] As shown in Table 23, mixed products of sanguinarine and d-limonene at different ratios were more effective against powdery mildew in the field than single agents of sanguinarine and d-limonene. Product Formulation Application Example 3 achieved optimal control at a 667-fold dilution and an active ingredient dosage of 30 mg / L, achieving an average 7-day control efficacy of 91.28%.

[0292] Product Field Efficacy Example 3: Field Efficacy Test for Controlling Plutella xylostella

[0293] This experiment was conducted in Zhangzhou, Fujian Province, on approximately 10 mu (approximately 16 acres) of open-air rapeseed cultivation. Irrigation and drainage conditions were normal, and management was routine. Pesticides were applied 5-7 times per growing season to control the diamondback moth. The plots were 1.0 m x 6.0 m per ridge. Cultivation conditions (rape variety, soil type, water and fertilizer management, transplanting period, planting density, growing season, and water management) were relatively uniform across all plots.

[0294] The insecticide was applied to 2nd-3rd instar diamondback moth larvae. No other insecticides were applied for 7 days before or during the test. The inventors designed the test plan based on the above experimental investigation and calculation method, calculated the mite population reduction rate, and analyzed the control effect, as shown in Table 24:

[0295] Table 24 Design and results of field efficacy test on Plutella xylostella

[0296]

[0297] As shown in Table 24, mixed products of sanguinarine and d-limonene at different ratios were more effective against powdery mildew in the field than single agents of sanguinarine and d-limonene. Product Formulation Application Example 6 achieved optimal control at a 1778-fold dilution and an active ingredient dosage of 225 mg / L, achieving an average 7-day control efficacy of 87.63%.

[0298] Product Field Efficacy Example 4: Field Efficacy Test for Controlling Cucumber Root-Knot Nematodes

[0299] This experiment was conducted in Honghe Hani and Yi Autonomous Prefecture, Yunnan Province. Approximately 10 mu (approximately 16 acres) of vegetables (including tomatoes, zucchini, bitter melon, and cucumbers) were cultivated outdoors under normal irrigation and drainage conditions and managed properly. Powdery mildew, downy mildew, and angular leaf spot are common diseases. Cucumbers were planted in plots of approximately 9 ridges (16 plants per ridge), with a planting size of 1.0 m x 32.0 m per ridge and approximately 1.0 m spacing between ridges. Cultivation conditions (soil type, water and fertilizer management, transplanting period, planting density, growth period, and water layer management) were relatively uniform across all plots.

[0300] The insecticide was applied during the fruiting period. No other nematicides were applied for 20 days before or during the experiment. The inventors designed the experimental plan based on the above experimental investigation and calculation method, calculated the mite population reduction rate, and analyzed the control effect, as shown in Table 25:

[0301] Table 25 Experimental design and results of field efficacy test on cucumber root knot nematode

[0302]

[0303] As shown in Table 25, mixed products of sanguinarine and d-limonene in different ratios demonstrated superior field efficacy against cucumber root-knot nematodes compared to single doses of sanguinarine and d-limonene. Product Formulation Application Example 8 achieved optimal efficacy at a 1200-fold dilution and an active ingredient dosage of 225 mg / L, achieving an average efficacy of 79.21%.

[0304] Product Field Efficacy Example 5: Field Efficacy Test for Controlling Powdery Mildew of Bitter Melon

[0305] This experiment was conducted in Honghe Hani and Yi Autonomous Prefecture, Yunnan Province. Approximately 10 mu (approximately 1.5 acres) of vegetables (including tomatoes, zucchini, bitter melon, and cucumbers) were cultivated outdoors under normal irrigation and drainage conditions and managed properly. Powdery mildew, downy mildew, and angular leaf spot diseases frequently occur. Within each plot, approximately 20 bitter melon plants were planted per ridge, with a planting size of 1.0 m x 40.0 m per ridge, spaced approximately 1.0 m apart. Cultivation conditions (soil type, water and fertilizer management, transplanting period, planting density, growing season, and water layer management) were relatively uniform across all experimental plots.

[0306] The pesticides were applied during the young fruit stage. No other fungicides were applied for 20 days before or during the test. The inventors designed the test plan based on the above-mentioned test investigation and calculation method, calculated the mite population reduction rate, and analyzed the control effect, as shown in Table 26:

[0307] Table 26 Field efficacy test design and results of bitter melon powdery mildew

[0308]

[0309] As shown in Table 26, mixed products of sanguinarine and d-limonene at different ratios were more effective against powdery mildew in the field than single agents of sanguinarine and d-limonene. The product formulation in Example 9, diluted 3333 times and using an active ingredient dosage of 60 mg / L, achieved the best control effect, with an average control efficiency of 81.29%.

[0310] In summary, the present invention adopts a composition for controlling crop pests, mites, insects, nematodes and pathogenic fungi. Compared with existing preparations, it not only has obvious synergistic effects, but also has good control effects, and is worthy of promotion and application in agricultural production.

[0311] The above description is only a preferred embodiment of the present invention and does not limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the scope of protection of the present invention.

Claims

1. An agricultural composition, characterized in that The active ingredients of the composition include sanguinarine and d-limonene, the weight ratio of sanguinarine to d-limonene is 39:1-1:99, and the total weight percentage of sanguinarine and d-limonene in the composition is 0.1%-76%.

2. The composition according to claim 1, characterized in that The sanguinarine includes one or more of sanguinarine, sanguinarine inorganic salt or sanguinarine organic salt.

3. The composition according to claim 1, characterized in that The composition can be prepared into dosage forms including wettable powder, soluble powder, water-dispersible granules, soluble granules, tablets, emulsifiable concentrates, aqueous emulsions, microemulsions, suspoemulsions, suspensions, dispersible oil suspensions, microcapsule suspensions, soluble solutions and suspension seed coatings.

4. The composition according to claim 3, characterized in that The dosage form preparation process of the composition contains common auxiliary materials required for preparing pesticide formulations, and the auxiliary materials are one or a mixture of solvents, emulsifiers, wetting agents, dispersants, thickeners, pH regulators, stabilizers, defoamers, antifreeze agents and fillers.

5. A use of a composition containing sanguinarine and d-limonene, characterized in that: When used for controlling apple spider mites, the weight ratio of sanguinarine to d-limonene is 39:1-19:1; when used for controlling citrus panonychus mites, the weight ratio of sanguinarine to d-limonene is 39:1-19:1 or 1:19; when used for controlling apple spider mites, the weight ratio of sanguinarine to d-limonene is 39:1-19:1; when used for controlling diamondback moths, the weight ratio of sanguinarine to d-limonene is 1:39-1:99; when used for controlling southern root-knot nematodes, the weight ratio of sanguinarine to d-limonene is 9:1-1:9; when used for controlling powdery mildew of cucurbits, the weight ratio of sanguinarine to d-limonene is 1:39-1:

99.

6. The use of the composition according to claim 5, characterized in that Methods used for preventing and controlling diseases and insect pests in agriculture include seed mixing, root irrigation, flushing, soil mixing, fertilizer mixing, soaking, dripping, pouring, spraying, powdering or smoking.

Images