CN111183986A

CN111183986A - Pesticide containing diatomite and spinetoram and preparation method thereof

Info

Publication number: CN111183986A
Application number: CN202010114288.0A
Authority: CN
Inventors: 陈瑞明
Original assignee: Benson Huizhou Biotechnology Co Ltd
Current assignee: Benson Huizhou Biotechnology Co Ltd
Priority date: 2020-02-25
Filing date: 2020-02-25
Publication date: 2020-05-22

Abstract

The invention relates to the field of pesticides, in particular to a pesticide containing diatomite and spinetoram, which comprises a pharmaceutical composition, a wetting agent, a dispersing agent and a filler, wherein the pharmaceutical composition accounts for 30-90 wt% of the pesticide, the pesticide comprises the diatomite and the spinetoram in a weight ratio of (1: 40) - (100: 1), the microstructure of the diatomite is a sawtooth structure, the wetting agent is a sulfonate surfactant, and the pesticide is in the form of wettable powder or water dispersing agent. The pesticide provided by the invention solves the problems that diatomite has no surface activity, is poor in spreading, adhesion and permeation on the surface of a plant, slow in effect taking and serious in duration due to wind power and rainwater scouring, realizes the decrement and synergism of the pesticide, and is quick in effect taking, long in duration and not easy for pests to generate resistance.

Description

Pesticide containing diatomite and spinetoram and preparation method thereof

Technical Field

The invention relates to the field of pesticides, in particular to a pesticide containing diatomite and spinetoram and a preparation method thereof.

Background

The diatomite is a natural component, is completely different from the mechanism of the existing chemical pesticide, belongs to a physical pesticide, has white powder in an apparent state, low density, multiple pores and rough feeling, can penetrate the body surface of pests if being adhered to the body surface when the insects climb over the diatomite powder, invade the epidermis of the pests and even enter the body of the pests, can cause the disorders of systems such as respiration, digestion, reproduction, movement and the like of the pests, and can absorb water which is 3 to 4 times of the weight of the pests, so that the body fluid of the pests is sharply reduced and die, and in addition, the diatomite can also absorb and destroy the wax layer on the body surface of the pests, so that the pests die by dehydration. The diatomite is used for killing insects in a mechanical mode, so that the insects cannot generate antibodies to the diatomite, and the diatomite is non-toxic and cannot harm human and natural environment.

The applicant of the invention finds that the diatomite with the special sawtooth structure can be used as a physical insecticide and has a good insecticidal effect, but at present, no research on the physical insecticide with the special structure exists in China, and the diatomite does not have surface activity, so that when the diatomite is used as the pesticide alone, the dosage is large, the spreading, viscosity and infiltration effects on the surface of a plant are poor, the effect is slow, and the lasting period is seriously washed by wind power and rainwater.

Disclosure of Invention

In order to solve the technical problems, the invention provides a pharmaceutical composition in a first aspect, wherein the pharmaceutical composition comprises diatomite and spinetoram.

As a preferable technical scheme, the weight ratio of the diatomite to the spinetoram in the pharmaceutical composition is (1: 40) - (100: 1).

The invention provides a pesticide containing diatomite and spinetoram in a second aspect, and the pesticide comprises the pharmaceutical composition, wherein the pharmaceutical composition accounts for 30-94 wt% of the pesticide.

In a preferred embodiment of the present invention, the diatomite has a saw-tooth structure in its microstructure.

As a preferable technical scheme of the invention, the pesticide also comprises a wetting agent, a dispersing agent and a filler.

In a preferred embodiment of the present invention, the wetting agent is a sulfonate surfactant.

As a preferred technical solution of the present invention, the wetting agent is dioctyl sodium sulfosuccinate.

In a preferred embodiment of the present invention, the dispersant is at least one selected from lignosulfonate, naphthalene sulfonate formaldehyde condensate, alkylphenol polyoxyethylene formaldehyde condensate sulfate, and polycarboxylate.

As a preferable technical scheme of the invention, the pesticide is in the form of wettable powder or water dispersant.

The third aspect of the invention provides a preparation method of the pesticide containing diatomite and spinetoram, which comprises the following steps: and (2) putting the dispersing agent, the wetting agent, the filler and the spinetoram into a container, crushing and mixing, then adding the diatomite, stirring and mixing, and performing post-treatment to obtain the pesticide.

Has the advantages that: the invention provides a pesticide containing diatomite and spinetoram, which is characterized in that diatomite with a special sawtooth structure and spinetoram are compounded in a specific proportion, and a specific sulfonate surfactant is added as a wetting agent, so that the problems that the diatomite does not have surface activity, is poor in spreading, adhesion and permeation on the surface of a plant, slow in effectiveness and serious in scouring of a lasting period by wind power and rainwater are solved, the decrement and synergism of the pesticide are realized, the effect is fast, the lasting period is long, and pests are not easy to generate resistance.

Drawings

Fig. 1 is an optical microscope photograph of a specific-structure diatomaceous earth having a saw-toothed honeycomb structure in example 1 of the present invention.

FIG. 2 is an electron microscope image of diatomaceous earth having a specific structure of a saw-toothed honeycomb structure in example 1 of the present invention.

Detailed Description

The disclosure may be understood more readily by reference to the following detailed description of preferred embodiments of the invention and the examples included therein. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. In case of conflict, the present specification, including definitions, will control.

The terms "comprises," "comprising," "includes," "including," "has," "having," "contains," "containing," or any other variation thereof, as used herein, are intended to cover a non-exclusive inclusion. For example, a composition, process, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, process, method, article, or apparatus.

When an amount, concentration, or other value or parameter is expressed as a range, preferred range, or as a range of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, when a range of "1 to 5" is disclosed, the described range should be interpreted to include the ranges "1 to 4", "1 to 3", "1 to 2 and 4 to 5", "1 to 3 and 5", and the like. When a range of values is described herein, unless otherwise stated, the range is intended to include the endpoints thereof and all integers and fractions within the range.

In addition, the indefinite articles "a" and "an" preceding an element or component of the invention are not intended to limit the number requirement (i.e., the number of occurrences) of the element or component. Thus, "a" or "an" should be read to include one or at least one, and the singular form of an element or component also includes the plural unless the stated number clearly indicates that the singular form is intended.

In the present invention, the term "composition" means that the components of the composition are packaged in combination or separately and used together when used. Namely, in the invention, the diatomite and the spinetoram are mixed and packaged together, and are used together when in use; the product also comprises diatomite and spinetoram which are separately packaged and mixed together in proportion for use.

In some embodiments, the weight ratio of diatomaceous earth to spinetoram in the pharmaceutical composition is (1: 40) - (100: 1).

In a preferred embodiment, the weight ratio of the diatomite to the spinetoram in the pharmaceutical composition is 1: 40. 1: 30. 1: 20. 1: 10. 1: 1. 10: 1. 20: 1. 30: 1. 40: 1. 50: 1. 60: 1. 70: 1. 80: 1. 90: 1. 100, and (2) a step of: 1.

in a more preferred embodiment, the weight ratio of diatomaceous earth to spinetoram in the pharmaceutical composition is 1: 40. 1: 20. 1: 1. 50: 1. 100, and (2) a step of: 1.

the invention provides a pesticide containing diatomite and spinetoram in a second aspect, the pesticide comprises the pharmaceutical composition, and the pharmaceutical composition accounts for 30-94 wt% of the pesticide

In a preferred embodiment, the pharmaceutical composition comprises 65 to 85 wt% of the pesticidal agent.

In a more preferred embodiment, the pharmaceutical composition comprises 80 wt% of the pesticidal agent.

The diatomite is a physical pesticide, is white powder in appearance state, has low density, multiple pores and rough feeling, and has very sharp edges and thorns, so that when insects climb over the diatomite, the diatomite adheres to the body surface of the insects, can pierce through the body surface of the insects, invade the epidermis of the insects, even enter the bodies of the insects, can cause the respiratory, digestive, reproductive and movement systems of the insects to be disordered, can absorb water 3-4 times of the weight of the insects, so that the body fluid of the insects is sharply reduced and die, and in addition, the diatomite can absorb and damage the wax layer on the body surface of the insects, so that the insects die by dehydration. However, the diatomite can exert the physical insecticidal action only by inducing pests to contact with the diatomite, has slow effect taking, has a lasting period seriously washed by wind power and rainwater, and loses the efficacy once the plant leaves and other parts lose the surface protection.

The Spinetoram is a new spinosyn insecticide produced by the Dow agricultural company, is a new member of spinosyn insecticides, is obtained by chemically modifying natural products of spinosyn, belongs to a bionic pesticide, and in the spinosyn insecticides, Spinetoram is a brand-new and unique effective component, is a high-efficiency and spectral insecticide, has the action mechanism of acting on a nicotine-type acetylcholine receptor and a gamma-aminobutyric acid receptor in insect nerves, leads the insects to be insensitive to excitatory and inhibitory signal transmission reactions, influences normal nervous activities until death, has stomach toxicity and contact killing effects, can be used for preventing and controlling pests such as vegetable diamond back moths, beet armyworms, prodenia litura, vegetable thrips, rice leaf rollers and the like, has quick insecticidal speed and long lasting period, Has little influence on beneficial organisms such as bees and the like, and belongs to a novel environment-friendly biological pesticide. However, when it is used alone on plants, it has a slightly poor insecticidal effect and is liable to cause the pests to produce antibodies after long-term use.

The applicant finds that spinetoram is compounded in diatomite, chemical effects of spinetoram on stomach toxicity, contact poisoning and the like of pests are utilized, physical effects of diatomite on penetration, adsorption and the like of the pests are combined, the pests are attacked in multiple directions, the insecticidal effect is fast, the better systemic effect of spinetoram is utilized, the spinetoram can be rapidly diffused to all parts in a plant body when acting on the surface of the plant, the problem that the diatomite has no surface activity and loses the drug effect due to wind power and rain wash in the lasting period is solved, the resistance mechanism of the pests is disturbed due to the multiple-direction attack, the pesticide resistance is difficult to form, and the lasting period of the pesticide is further prolonged.

In some embodiments, the diatomaceous earth has a microstructure that is a saw tooth structure. Conventional diatomaceous earthMainly contains silicon dioxide, and also contains a small amount of Al₂O₃、Fe₂O₃The diatomite is diatomite which is purified and mainly contains silicon dioxide with a sawtooth structure, and can be obtained commercially, for example, the diatomite with the sawtooth structure can be obtained commercially, and the diatomite with the sawtooth structure comprises but is not limited to diatomite with the trade name of Celite610 which is purchased from Yirui stone company, France, as shown in figures 1 and 2, and the diatomite has a clear sawtooth structure under an optical microscope and an electron microscope.

The applicant unexpectedly finds that the diatomite with the sawtooth structure and the spinetoram are compounded for use, and compared with the method of singly using the spinetoram or compounding common diatomite and the spinetoram, the diatomite composite pesticide has the advantages of good insecticidal effect and small pesticide consumption. The probable reason is presumed to be that the special honeycomb-shaped sawtooth structure of the diatomite increases the specific surface area of the diatomite, is beneficial to adsorbing on the body surface of pests, enhances the penetration effect of the diatomite on the body surface of the pests, effectively protects the spinetoram, promotes the spinetoram to penetrate into the bodies of the pests more quickly and better, acts on nicotinic acetylcholine receptors and gamma-aminobutyric acid receptors in the nerves of the pests, interferes with the nervous activities of the pests to kill the pests, and realizes the decrement and efficiency increase effect by compounding the two.

In some embodiments, the pesticidal insecticide further comprises a wetting agent, a dispersing agent, and a filler.

In a preferred embodiment, the wetting agent is a sulfonate surfactant.

In a more preferred embodiment, the wetting agent is sodium diisooctyl succinate sulfonate.

In some embodiments, the wetting agent comprises 3 to 10 wt% of the pesticidal insecticide; preferably, the wetting agent comprises 8 wt% of the pesticidal insecticide.

Sodium diisooctyl succinate sulfonate, CAS number 577-11-7, is commercially available, for example commercially available sodium diisooctyl succinate sulfonate includes, but is not limited to, the product sold by break Thailand chemical Co., Ltd, manufactured in Nantong, model number HTOT-75.

The applicant unexpectedly finds that the spreading property of the pesticide liquid on the surface of the plant can be improved by adding the sulfonate surfactant into the pesticide, and particularly, when the diisooctyl sulfosuccinate is added, the contact angle of the pesticide liquid on the surface of the plant is smaller, the spreading property is good, and the pesticide effect is further improved. Presumably, the main component of diatomaceous earth is amorphous colloidal SiO₂The surface tension of the diatomite with a sawtooth structure is obviously reduced particularly when the diatomite with the sawtooth structure is used, and when the sulfonate surfactant is sodium diisooctyl succinate, a semi-cavity structure formed by symmetrical long molecular chains enhances the permeation of liquid medicine in plants, so that the medicine effect is improved.

In some embodiments, the dispersant is selected from at least one of lignosulfonates, naphthalene sulfonate formaldehyde condensates, alkyl phenol polyoxyethylene ether formaldehyde condensate sulfates, polycarboxylates.

In some embodiments, the dispersant comprises 3 to 8 wt% of the pesticidal insecticide; preferably, the dispersant constitutes 5 wt% of the pesticidal insecticide.

In some embodiments, the filler is selected from at least one of kaolin, talc, precipitated calcium carbonate, bentonite, attapulgite, and silica.

In some embodiments, the filler comprises 5 to 10 wt% of the pesticidal insecticide; preferably, the filler comprises 7 wt% of the pesticidal insecticide.

In some embodiments, the formulation of the pesticidal insecticide is a wettable powder or an aqueous dispersion.

In the invention, in order to avoid damaging the sawtooth structure of the diatomite, the diatomite is added, the diatomite is not mechanically crushed, the diatomite and other components are mixed by adopting conventional shaking and stirring, after uniform mixing, if the pesticide is prepared into wettable powder, the mixed powder does not need post-treatment, sampling detection and analysis are qualified, the pesticide is prepared, if the pesticide is prepared into water dispersion agent, the mixed powder is granulated by adopting a conventional method, and then the pesticide is prepared after detection and analysis are qualified.

Examples

Example 1

This example provides a joint virulence determination for citrus red spiders by compounding diatomaceous earth, the microstructure of which is a saw-tooth structure, and the trade name of which is Celite610 purchased from yirui stone, france, as shown in fig. 1 and 2, with spinetoram purchased from shanxi huichi biotechnology limited.

Referring to the method in NY/T1154.13-2008 standard, a leaf spray method was used. Cleaning and wiping the smooth citrus leaves with the same size, sticking the citrus leaves onto wet sponge with the leaf surfaces facing upwards, enclosing the leaves with wet small cotton slivers to prevent test mites from escaping, putting the wet sponge into a culture dish with the diameter of 9cm, adding water into the culture dish, and slightly lowering the water level to be lower than the height of the sponge. Inoculating indoor cultured nymphs to leaves, each leaf having no less than 30 heads. Placing the culture dish on a bottom plate of a Potter spraying tower for spraying, wherein the spraying amount is 1mL, taking out the culture dish after the liquid medicine is settled for 1min, and transferring the culture dish to a breeding condition for breeding. Each treatment was repeated 4 times and a blank control was run.

After 48h, the death of the test insects was examined under a dissecting mirror and recorded. The judgment standard of the death of the test insects is as follows: death was counted as no response when the test insects were gently touched by tweezers.

Example 2

The embodiment provides a combined toxicity determination method for citrus icerya purchasi by compounding diatomite and spinetoram, wherein the microstructure of the diatomite is a sawtooth structure, the trademark of the diatomite 610 purchased from Yirui stone, France is Celite, and the trademark is shown in figures 1 and 2, and the spinetoram is purchased from Shanxi Huichi Biotechnology Co.

The method in NY/T1154.6-2006 is referred to, and the insect-soaking method is adopted. Dipping the trimmed citrus leaves with citrus arrowhead scales in a test solution for 10 seconds, taking out the citrus leaves, absorbing redundant liquid medicine around the leaves and the insects by using filter paper, putting the citrus leaves and the insects into a culture dish (with the diameter of 90mm) filled with moisturizing filter paper, wrapping petioles by using wet cotton balls for moisturizing, repeating the steps for 4 times per concentration, covering the dish cover after the treatment is finished, and placing the dish cover in an observation room for culturing.

After 72d, checking the death condition of the test insects by using a dissecting mirror, and recording, wherein the death judgment standard of the test insects is fresh and alive, and the test insects are regarded as live insects in yellow or light yellow; the dead insects are considered to be dead insects if the body of the insects is shriveled and the color is dark.

Example 3

The embodiment provides a combined toxicity test of western thrips by compounding diatomite and spinetoram, wherein the microstructure of the diatomite is a sawtooth structure, the trademark of the diatomite is Celite610 purchased from Yirui Stone company, France, as shown in figures 1 and 2, and the spinetoram is purchased from Shanxi Heichi Biotechnology Limited company.

According to the standard method NY/T1154.14-2008 of biological measurement, a leaf-soaking dish method is adopted. Beating the blades into leaf disks by a puncher with the diameter of 18mm, soaking the leaf disks in a test reagent solution for 10 seconds, putting the leaf disks into a culture dish (with the diameter of 90mm) padded with moisturizing filter paper, putting 5 leaf disks into each dish, naturally drying, then selecting the western flower thrips into the culture dish, sealing the mouth of the dish by a preservative film, pricking some small holes on the film by a needle for ventilation, repeating the treatment for 4 times, finishing the treatment, and placing the dish in an observation room for culture.

And (4) after 72h, checking and recording the death condition of the test insects, wherein the death judgment standard of the test insects is that the test insects are dead as the result of no response when the pointed writing brush is lightly contacted with the test insects.

Example 4

The embodiment provides a combined toxicity test of white whitefly by compounding diatomite and spinetoram, wherein the microstructure of the diatomite is a sawtooth structure, the trademark of the diatomite is Celite610 purchased from Yirui stone company, France, as shown in figures 1 and 2, and the spinetoram is purchased from Shanxi Heichi Biotechnology Co.

Referring to the method in NY/T1154.14-2008 standard, the leaf soaking method is adopted. After dissolving agar (1%) by heating, 20mL to 200mL of the solution was taken out of a beaker and condensed at room temperature for use. Soaking the leaves in a test solution for 10 seconds, taking out, naturally drying, sticking the leaves on the surface of the solidified agar solution, wrapping petioles with wet cotton balls, putting 3-4 leaves in each beaker, inoculating adult trialeurodes vaporariorum, covering 15 heads of each beaker with a preservative film, pricking small holes on the film with needles for ventilation, repeating the treatment for 4 times, and placing the beaker in an observation room for cultivation after the treatment.

And (4) after 72h, detecting the death condition of the test insects, and recording, wherein the death judgment standard of the test insects is that no response is calculated when the tweezers lightly contact the test insects.

Example 5

This example provides a joint virulence assay for the composite pairing of diatomaceous earth, with a saw tooth structure, purchased from Yirui Stone, France under the trade designation Celite610, as shown in FIGS. 1 and 2, and spinetoram, purchased from Whitech Biotechnology, Inc., Shaanxi.

Referring to the method in NY/T1154.13-2008 standard, spraying method is adopted. Transplanting potted cowpea pest-free seedlings into pest-raising cages, inoculating a certain amount of mated adult liriomyza huidonii, taking out bean seedlings with liriomyza huidonii eggs after 6h, placing the bean seedlings in another pest-raising cage, continuously raising the bean seedlings to 2-year larvae (ensuring that each disc contains no less than 80 larvae of 2-year larvae), then carrying out spraying treatment, naturally air drying, and transferring the bean seedlings to an artificial climate box for continuous raising. Each treatment was repeated 4 times and a blank control was run.

And (3) cutting bean seedlings from roots at the later stage of 3-year-old larvae, moisturizing the tail ends by using soaked cotton balls, putting the bean seedlings into plastic basins in an artificial climate box, pupating the bean seedlings, and counting the quantity of pupae in each dish.

Example 6

The embodiment provides a combined toxicity determination method for prodenia litura by compounding diatomite and spinetoram, wherein the microstructure of the diatomite is a sawtooth structure, the trademark of the diatomite is Celite610 purchased from Yirui Stone, France, as shown in figures 1 and 2, and the spinetoram is purchased from Shanxi Heichi Biotechnology Limited.

Referring to the method in NY/T1154.14-2008 standard, the leaf-dipping dish method is adopted. Beat the cabbage leaf into the leaf dish with the hole puncher of diameter 18mm, dip the leaf dish in the liquid of testing medicine for 10 seconds after, put into the culture dish (diameter 90mm) that has filled with the filter paper that moisturizes, 6 leaf dishes are put into to every dish, wait to dry the back naturally, select again and starve 4h twill noctuid 3 age larva to the culture dish in, every dish is not less than 10, 4 times are repeated, the processing finishes, covers the ware lid, arranges the indoor culture of observation in.

Example 7

The embodiment provides a combined toxicity determination method for a tea leafhopper by compounding diatomite and spinetoram, wherein the microstructure of the diatomite is a sawtooth structure, the trademark of the diatomite 610 purchased from Yirui stone, France is shown in figures 1 and 2, and the spinetoram is purchased from Shanxi Huichi Biotech limited.

Referring to the method in NY/T1154.11-2008 standard, the dipping method is adopted. Selecting 3 fresh tea tree sprouts, soaking in a test liquid for 30 seconds, taking out, naturally drying, wrapping the base parts of the sprouts with wet absorbent cotton to preserve moisture, sealing absorbent cotton balls with a preservative film, and placing in a glass test tube (phi 200 x 30mm) for 4 times of repetition at each concentration. Then, 3-year-old nymphs of tea lesser leafhoppers subjected to ether mild anesthesia treatment are inoculated into a brush pen, 15 +/-2 heads of each tube are used, and the mouth of each tube is sealed by white gauze. After the treatment, the sample is placed in an observation chamber.

Example 8

The embodiment provides a combined toxicity determination method of tea yellow thrips by compounding diatomite and spinetoram, wherein the microstructure of the diatomite is a sawtooth structure, the trademark of the diatomite is Celite610 purchased from Yirui Stone company, France, as shown in figures 1 and 2, and the spinetoram is purchased from Shanxi Huichi Biotechnology Limited.

According to the standard method NY/T1154.14-2008 of biological measurement, a leaf dipping method is adopted. Selecting 3 fresh tea tree sprout shoots with a certain amount of tea thrips (not less than 20), soaking in the test liquid for 10 seconds, taking out, naturally drying, wrapping the base parts of the sprout shoots with wet absorbent cotton to preserve moisture, sealing the absorbent cotton balls with a preservative film, and placing in a glass test tube (phi 200 x 30mm) for 4 times of concentration. The mouth of the test tube is sealed by a preservative film, and the small holes are punched for ventilation. After the treatment, the sample is placed in an observation chamber.

And after 72h, examining the death condition of the test insects under a dissecting mirror, and recording, wherein the death judgment standard of the test insects is that the test insects die because the test insects are not reacted when the pointed writing brush is lightly contacted with the test insects.

Example 9

This example provides a joint virulence determination for tea geometrid by compounding diatomaceous earth with spinetoram purchased from shancheng hecheng biotechnology limited, shakei, with a microstructure of saw-tooth structure and a trade designation of Celite610 purchased from france, and as shown in fig. 1 and 2.

Referring to the method in NY/T1154.14-2008 standard, the leaf soaking method is adopted. Selecting 3 fresh tea tree sprouts, soaking in the test liquid medicine for 30 seconds, taking out, naturally drying, wrapping the bases of the sprouts with wet absorbent cotton to preserve moisture, sealing absorbent cotton balls with a preservative film, and placing in a can bottle, wherein the concentration is repeated for 4 times. Then inoculating 2-year-old nymphs of tea geometrid with consistent size and liveness and health into a brush pen, wherein 15 +/-2 heads of each pot are sealed by white gauze. After the treatment, the sample is placed in an observation chamber.

Example 10

This example provides a combined virulence assay for the compounded pairing of diatomaceous earth, a saw tooth structure in its microstructure, and Celite610, a trademark of yirui corp, france, as shown in fig. 1 and 2, with spinetoram, a product of shancheng cheng biotechnology limited, shanxi.

Referring to the method in NY/T1154.11-2008 standard, a leaf spray method was used. The method comprises the steps of disinfecting, cleaning and airing fresh kidney beans by adopting an immersion method, cutting the kidney beans into 2-3 cm segments, immersing the kidney beans in liquid medicines with different concentrations for 30 seconds, airing the kidney beans under natural conditions, and then putting the kidney beans into transparent plastic boxes (6 cm in diameter and 7cm in height) with smooth air, wherein each box has two sections. Healthy and consistent 3-year-old nymphs of lygus lucorum were inoculated, 15 or so per box, repeated 4 times, and a blank control was set. And putting the plastic box into a light incubator for culturing.

And after 48h, the death condition of the test insects in each box is checked, the bodies of the lygus lucorum are lightly touched by the brush tips, and the death judgment standard of the test insects is that no response is calculated when the tweezers lightly touch the test insects.

Example 11

The embodiment provides a combined toxicity determination method for grape aphids by compounding diatomite and spinetoram, wherein the microstructure of the diatomite is a sawtooth structure, the trademark of the diatomite is Celite610 purchased from Yirui Stone company, France, and the spinetoram is purchased from Heichi Biotechnology GmbH, Shanxi, as shown in figures 1 and 2.

The method in NY/T1154.6-2006 is referred to, and the insect-soaking method is adopted. Cutting leaves with a certain amount of grape aphids, soaking in the liquid medicine to be tested for 10 seconds, taking out, absorbing the liquid medicine around the insect body with absorbent filter paper, placing in a culture dish padded with moisturizing filter paper, moisturizing with a wet cotton ball, and covering the culture dish with wet gauze. Each 30 aphids were treated, 4 replicates and a blank treatment without drug (including solvent and emulsifier used) was used. After the treatment, the cells were transferred to an observation room for cultivation.

And (3) detecting the death condition of the test insects after 48h, and recording, wherein the judgment standard of the death of the test insects is as follows: the aphids were lightly touched with a writing brush, and the body was judged dead.

In the above examples, the co-toxicity coefficient (CTC) of each blend combination was determined by Sun & Johnson (1960) co-toxicity coefficient method (CTC) according to the standard bioassay method NY/T1154.7-2006, and the results are shown in tables 1 to 11, respectively. Generally, a co-toxicity coefficient greater than 120 indicates a synergistic effect, less than 80 indicates an antagonistic effect, and between 80 and 120 indicates an additive effect. The co-toxicity coefficient is calculated as follows

The Theoretical Toxicity Index (TTI) of the mixture is the toxicity index of the agent A x the percent (%) of the agent A + the toxicity index of the agent B x the percent (%) of the agent B

TABLE 1

TABLE 2

TABLE 3

TABLE 4

TABLE 5

TABLE 6

TABLE 7

TABLE 8

TABLE 9

Watch 10

TABLE 11

As can be seen from the results in tables 1-11, the diatomaceous earth with special saw tooth results and spinetoram in the present invention have synergistic effect, when the weight ratio of diatomaceous earth to spinetoram is 1: 40. 1: 20. 1: 1. 50: 1. 100, and (2) a step of: 1, the co-toxicity coefficient is more than 120, the synergistic effect is obvious, and the pesticide has a better control effect on citrus red spiders, citrus scale insects, frankliniella occidentalis, trialeurodes vaporariorum, liriomyza, prodenia litura, tea leafhopper, tea leaf thrips flavivis, tea leaf loopers, green plant bugs and grape aphids.

Example 12

The embodiment provides a pesticide containing diatomite and spinetoram, which is prepared from 80 wt% of a pharmaceutical composition, 8 wt% of a wetting agent, 5 wt% of a dispersing agent and 7 wt% of a filler, wherein the pharmaceutical composition comprises the diatomite and the spinetoram, and the weight ratio of the diatomite to the spinetoram is 100: 1, the wetting agent is diisooctyl succinate sodium sulfonate, the dispersing agent is sodium lignosulphonate, and the filler is kaolin.

The diatomite has a sawtooth structure, is purchased from Yirui Stone company of France and has the brand name of Celite 610; the spinetoram is purchased from Shanxi Huichi Biotechnology Co., Ltd; the sodium diisooctyl succinate sulfonate is purchased from break-Thai chemical Limited company in Nantong City, and has the model of HT OT-75; others are commercially available.

The embodiment also provides a preparation method of the pesticide, which comprises the following steps: weighing the dispersing agent, the wetting agent, the filler, the spinetoram and the diatomite according to the weight percentage, firstly putting the dispersing agent, the wetting agent, the filler and the spinetoram into a container for crushing and mixing, then adding the diatomite into the container, putting the container into a self-sealing bag for shaking, transferring the container into a flask after 10min, stirring and mixing the container for 30min by using a stirrer, and fully and uniformly mixing the container and the diatomite to obtain the pesticide, wherein the dosage form of the pesticide is wettable powder.

Example 13

The diatomite is purchased from Junlian diatomite Co., Ltd in Yixing city; the spinetoram is purchased from Shanxi Huichi Biotechnology Co., Ltd; the sodium diisooctyl succinate sulfonate is purchased from break-Thai chemical Limited company in Nantong City, and has the model of HT OT-75; others are commercially available.

Example 14

The embodiment provides a pesticide containing diatomite and spinetoram, which is prepared from 80 wt% of a pharmaceutical composition, 8 wt% of a wetting agent, 5 wt% of a dispersing agent and 7 wt% of a filler, wherein the pharmaceutical composition comprises the diatomite and the spinetoram, and the weight ratio of the diatomite to the spinetoram is 100: 1, the wetting agent is sodium dodecyl sulfate, the dispersing agent is sodium lignosulphonate, and the filler is kaolin.

The diatomite has a sawtooth structure, is purchased from Yirui Stone company of France and has the brand name of Celite 610; the spinetoram is purchased from Shanxi Huichi Biotechnology Co., Ltd; others are commercially available.

Example 15

The agricultural chemical insecticides prepared in examples 12 to 15 were diluted with water to prepare 250-fold, 500-fold, and 1000-fold dilutions, and the surface tensions thereof were measured by a surface tension meter, and the results are shown in table 12.

TABLE 12

According to the experimental results in table 12, it can be seen that the diatomite with a saw-tooth structure is added into the pesticide, and the diisooctyl sulfosuccinate is used as a wetting agent, so that the spreading, adhesion and infiltration of the pesticide on the surface of a plant can be effectively improved, the insecticidal effect of the pesticide is further enhanced, and the pesticide has the advantages of quick response and long duration.

The foregoing examples are merely illustrative and serve to explain some of the features of the method of the present invention. The appended claims are intended to claim as broad a scope as is contemplated, and the examples presented herein are merely illustrative of selected implementations in accordance with all possible combinations of examples. Accordingly, it is applicants' intention that the appended claims are not to be limited by the choice of examples illustrating features of the invention. Also, where numerical ranges are used in the claims, subranges therein are included, and variations in these ranges are also to be construed as possible being covered by the appended claims.

Claims

1. A pharmaceutical composition comprising diatomaceous earth and spinetoram.

2. The pharmaceutical composition of claim 1, wherein the weight ratio of the diatomaceous earth to the spinetoram in the pharmaceutical composition is (1: 40) - (100: 1).

3. A pesticidal insecticide containing diatomaceous earth and spinetoram according to claim 1 or 2, wherein said pesticidal insecticide comprises the pharmaceutical composition according to claim 1 or 2, and said pharmaceutical composition accounts for 30 to 94 wt% of said pesticidal insecticide.

4. The pesticidal agent according to claim 3, which comprises diatomaceous earth and spinetoram, wherein the diatomaceous earth has a saw-tooth structure in its microstructure.

5. The agricultural chemical containing diatomaceous earth and spinetoram according to claim 3, further comprising a wetting agent, a dispersing agent, and a filler.

6. The pesticidal agent according to claim 5, which comprises diatomaceous earth and spinetoram, wherein the wetting agent is a sulfonate surfactant.

7. The pesticidal agent according to claim 5, which comprises diatomaceous earth and spinetoram, wherein the wetting agent is sodium diisooctyl sulfosuccinate.

8. A pesticidal insecticide containing diatomaceous earth and spinetoram according to claim 5, wherein said dispersant is at least one selected from the group consisting of lignosulfonate, naphthalenesulfonate formaldehyde condensate, alkylphenol polyoxyethylene ether formaldehyde condensate sulfate and polycarboxylate.

9. The pesticidal agent according to any one of claims 3 to 8, which comprises diatomaceous earth and spinetoram, and is in the form of a wettable powder or an aqueous dispersion.

10. A method for producing a pesticidal agent containing diatomaceous earth and spinetoram according to any one of claims 3 to 9, comprising the steps of: and (3) putting the dispersing agent, the wetting agent, the filler and the spinetoram into a container, crushing and mixing, then adding the diatomite, stirring and mixing, and carrying out post-treatment to obtain the pesticide.