CN111134119A - Nano chitosan-thiamethoxam water agent and preparation method and application thereof - Google Patents
Nano chitosan-thiamethoxam water agent and preparation method and application thereof Download PDFInfo
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- CN111134119A CN111134119A CN202010101047.2A CN202010101047A CN111134119A CN 111134119 A CN111134119 A CN 111134119A CN 202010101047 A CN202010101047 A CN 202010101047A CN 111134119 A CN111134119 A CN 111134119A
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/26—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests in coated particulate form
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
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- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/02—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing liquids as carriers, diluents or solvents
- A01N25/04—Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/30—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests characterised by the surfactants
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
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- A01N51/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds having the sequences of atoms O—N—S, X—O—S, N—N—S, O—N—N or O-halogen, regardless of the number of bonds each atom has and with no atom of these sequences forming part of a heterocyclic ring
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Abstract
The invention discloses a nano chitosan-thiamethoxam aqueous solution and a preparation method and application thereof. The preparation method comprises the following steps: emulsifying chitosan, adding HY-266, stirring, and mixing to obtain W-phase working solution; dissolving thiamethoxam, adding HY-266, and stirring and mixing to obtain O-phase working solution; and stirring and mixing the W-phase working solution and the O-phase working solution to obtain the nano chitosan-thiamethoxam aqueous solution. The nano chitosan-thiamethoxam water aqua disclosed by the invention has the advantages that the stability of thiamethoxam is improved, and the release speed of thiamethoxam is reduced, so that the pesticide effect period of thiamethoxam is prolonged, the water aqua can be applied to controlling bemisia tabaci, has the characteristics of good environmental compatibility and long control effect period, and is free from phytotoxicity to crops such as tomatoes and cucumbers.
Description
Technical Field
The invention relates to the technical field of biological macromolecular materials and chemical pesticides, in particular to a nano chitosan-thiamethoxam aqueous solution and a preparation method and application thereof.
Background
Bemisia tabaci (Gennadius) is a worldwide pest. The host range is quite wide, and the host plants are more than 500. Outbreaks have appeared since the 20 th century and the 90 th year of the year of invasion of China. At present, the bemisia tabaci is widely distributed in China, and all main provinces in China occur. The bemisia tabaci can directly prick and absorb plant juice to cause plant weakness, nymphs and adults can also secrete honeydew to induce the generation of sooty mould, and the photosynthesis of plants is seriously influenced. More importantly, bemisia tabaci can also transmit more than 70 viruses on 30 crops, such as Tomato Yellow Leaf Curl Virus (TYLCV) and Tomato chlorosis virus (Tomatochorosis virus) which are transmitted by bemisia tabaci in recent years, so that the bemisia tabaci causes outbreak of harm in main producing areas of solanaceae crops such as tomatoes in China and brings huge economic loss to the solanaceae crops such as tomatoes in China.
At present, the most main method for preventing and controlling the tobacco whitefly in production is to adopt chemical agents for prevention and control, and thiamethoxam is one of the main chemical agents for preventing and controlling the tobacco whitefly in production at present and has the characteristic of high prevention effect. However, the lasting period of the common thiamethoxam preparation for preventing and controlling the bemisia tabaci passes about 15-20 days, and the common thiamethoxam preparation needs to be applied for multiple times in one growing season of crops, so that the input amount of the pesticide is increased, the prevention and control cost is increased, and the yield of the crops is reduced.
In order to prolong the lasting period of chemical agents, the chemical agents are released slowly, which is the most important technical method at present, wherein the nano biomacromolecule material is combined with the chemical agents to form nano biomacromolecule material-pesticide microspheres, so that the release period of the chemical agents can be prolonged, and novel pesticide formulations can be prepared according to the characteristics of different nano biomacromolecule materials, thereby improving the prevention and control efficiency of the pesticides. Biomacromolecule chitosan is also called deacetylated chitin, is obtained by chemically treating chitin (chitin) widely existing in nature, has excellent performances of good safety, biocompatibility, good water solubility and the like, and is widely researched and applied to the field of plant protection.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a nano chitosan-thiamethoxam aqueous solution, compared with commercially available formulations such as thiamethoxam water dispersible granules and the like, the nano chitosan-thiamethoxam aqueous solution has the advantages of improved stability, environmental friendliness and simple preparation method, can be applied to control Bemisia tabaci, prolongs the pesticide effect period for controlling Bemisia tabaci, and can reduce the control times of thiamethoxam, thereby reducing the using amount of thiamethoxam and saving the pesticide application cost.
In order to solve the technical problems, the invention provides a nano chitosan-thiamethoxam aqueous solution which comprises nano chitosan and thiamethoxam, wherein the thiamethoxam is wrapped in chitosan nanoparticles.
Furthermore, the oil-in-water type nano chitosan-thiamethoxam aqueous solution is formed by taking a chitosan solution as a water phase and taking a thiamethoxam solution as an oil phase.
Further, the mass volume concentration of the chitosan solution is 0.2-0.4%, and the mass volume concentration of the thiamethoxam solution is 25-50%.
Based on a general technical concept, the invention also provides a preparation method of the nano chitosan-thiamethoxam aqueous solution, which comprises the following steps:
s1, emulsifying chitosan, adding an emulsifier HY-266, and stirring and mixing to obtain a W-phase working solution;
s2, dissolving thiamethoxam, adding HY-266, and stirring and mixing to obtain O-phase working solution;
and S3, stirring and mixing the W-phase working solution and the O-phase working solution to obtain the nano chitosan-thiamethoxam aqueous solution.
In the preparation method of the nano chitosan-thiamethoxam aqueous solution, further, in S1, the specific process of emulsifying the chitosan is as follows: dissolving chitosan in NaAc buffer solution, adding sodium polyphosphate, stirring and mixing until opalescence appears to obtain an emulsified chitosan solution.
In the preparation method of the nano chitosan-thiamethoxam water aqua, the mass volume concentration of the sodium polyphosphate is 0.005-0.008%; the rotating speed of the stirring is 1000 rpm-2000 rpm.
In the preparation method of the nano chitosan-thiamethoxam water aqua, furthermore, in the S1, the HY-266 is 0.003-0.006% by mass volume concentration.
In the preparation method of the nano chitosan-thiamethoxam water aqua, furthermore, in S2, the mass volume concentration of HY-266 is 0.003-0.006%; the rotating speed of stirring and mixing is 1000 rpm-2000 rpm, and the stirring time is 8 min-15 min.
In the preparation method of the nano chitosan-thiamethoxam water aqua, further, in the S3, the rotation speed of stirring and mixing is 1000 rpm-2000 rpm, and the time is 1.5 h-3 h.
Based on a general technical concept, the invention also provides an application of the nano chitosan-thiamethoxam water aqua in controlling bemisia tabaci.
The application is further characterized in that the application method comprises the following steps: the nano chitosan-thiamethoxam water aqua is diluted by 2000-3000 times and is sprayed on tomato and cucumber leaves.
Compared with the prior art, the invention has the advantages that:
(1) the invention provides a nano chitosan-thiamethoxam water aqua, which is prepared by wrapping thiamethoxam with nano chitosan to form a chitosan-emulsifier-thiamethoxam nano particle, so that the stability of thiamethoxam is improved, the release speed of thiamethoxam is reduced, and the pesticide effect period of thiamethoxam is prolonged; in addition, the chitosan has better water solubility and wraps the thiamethoxam, so that the prevention and control effect of the thiamethoxam on the bemisia tabaci is improved, the number of times of using the thiamethoxam is reduced, the effects of reducing the using amount of the thiamethoxam and improving the crop planting yield are achieved, the prevention and control effect of the bemisia tabaci is improved, and the crop production efficiency is improved. Compared with other dosage forms, the aqueous solution has better environmental safety.
(2) The invention provides a preparation method of a nano chitosan and thiamethoxam aqueous solution, which is simple in process and environment-friendly. The sodium polyphosphate is added into the chitosan, so that the capacity of dissolving the chitosan and stabilizing the dissolved solution can be increased, and in addition, the sodium polyphosphate has a buffering effect and can stabilize the pH value of the solution. The emulsifier HY-266 can be combined with hydrophilic chitosan to form amphiphilic HY-266-chitosan emulsified particles. HY-266 is capable of forming very small emulsified particles.
(3) The invention provides an application of a nano chitosan-thiamethoxam aqueous solution in controlling Bemisia tabaci, wherein the control effects of the nano chitosan-thiamethoxam aqueous solution on Bemisia tabaci on tomatoes and cucumbers are respectively 98.79% and 98.47% at most, and the effect is good; the drug effect period is prolonged by 15 days compared with that of the conventional thiamethoxam water dispersible granule.
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In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention.
Fig. 1 is a scanning electron microscope image of the aqueous nano chitosan-thiamethoxam formulation of example 1 of the present invention.
FIG. 2 is a spectrum of LC-MS detection of thiamethoxam content.
Detailed Description
The invention is further described below with reference to the drawings and specific preferred embodiments of the description, without thereby limiting the scope of protection of the invention.
The materials and equipment used in the following examples are commercially available.
Example 1
The invention relates to a nano chitosan-thiamethoxam water aqua, which takes a 0.4% chitosan solution as a water phase and a 50% thiamethoxam solution as an oil phase to form an oil-in-water type nano chitosan-thiamethoxam water aqua.
A preparation method of the nano chitosan-thiamethoxam water aqua comprises the following steps:
(1) chitosan was dissolved in NaAc buffer at 0.4% (W/V), then sodium polyphosphate was added at 0.0067% (W/V) and stirred at 1500 rpm until opalescence appeared.
(2) Then HY-266 (alcohol ether sulfate as main component) is added according to 0.005% (W/V), and the mixture is stirred at 1500 rpm for 2 h to obtain water phase (W phase) working solution.
(3) Dissolving thiamethoxam in acetone according to the proportion of 50% (W/V), adding HY-266 according to the proportion of 0.005% (W/V), and stirring at 1500 rpm for 10 min to obtain hydrophobic phase (O phase) working solution.
(4) And mixing the W-phase working solution and the O-phase working solution in equal proportion, and stirring at 1500 rpm for 2 h to obtain the nano chitosan-thiamethoxam water aqua.
Scanning the nano chitosan-thiamethoxam water agent by using a scanning electron microscope. The results are shown in FIG. 1, from which it can be seen that: the diameter of the prepared nano chitosan-thiamethoxam microsphere is less than 500 nm (95%).
Comparative example 1
A thiamethoxam water dispersible granule is purchased from Jiangsu southeast plant protection Co.
Investigation of thiamethoxam release rate:
the nano chitosan-thiamethoxam water aqua in the embodiment 1 and the thiamethoxam water dispersible granule in the comparative example 1 are respectively prepared into 5.0 mg/L solution, the solution is sprayed on the front and back sides of tomatoes, tomato leaves are taken at regular time, and the content of thiamethoxam is measured by an LC-MS method.
The LC-MS method for determining thiamethoxam comprises the following steps: weighing 10 g (accurate to 0.01 g) of tomato sample into a 100 mL centrifuge tube, adding 20 mL acetonitrile (containing 0.1% acetic acid), homogenizing and extracting for 0.5 min at 15000 r/min with a high speed homogenizer, shaking, ultrasonically extracting for 30 min at 40 ℃, and centrifuging for 10 min at 4000 r/min. Taking 1 mL of the supernatant, placing the supernatant in a microcentrifuge tube filled with 50 mg of PSA, 10 mg of GCB and 150 mg of magnesium sulfate, shaking vigorously for 1 min, centrifuging at 12000 r/min for 4 min, filtering the supernatant through a 0.2-micron filter membrane, and carrying out high performance liquid chromatography and mass spectrometry detection.
Liquid phase conditions: a chromatographic column: ACQUITY UPLC HST 3 (2.1X 100 mm, 1.8 μm); column temperature: 35 ℃; flow rate: 0.3 mL/min; sample introduction amount: 10 mu L of the solution; the mobile phase is methanol/0.1% formic acid water (V/V) solution, and the gradient elution is as follows: 0-1.0 min, 10% methanol; 3.0-6.0 min, 95% methanol; 6.1-8.0 min, 10% methanol.
Mass spectrum conditions: type of ion source: ESI+(ii) a Ion source temperature: 120 ℃; capillary voltage 3.0 kV; temperature of the desolventizing gas: 350 ℃; removing solvent gas: nitrogen gas, 600L/hr; the collision gas is argon gas, and the volume is 0.1 mL/min; cone hole back blowing gas flow: 50L/hr; multiple Reaction Monitoring (MRM) mass spectrometry acquisition parameters are shown in table 1.
The extraction part of the thiamethoxam is more suitable for extracting the thiamethoxam from the nano particles.
Table 1: thiamethoxam mass spectrometry parameters
See also fig. 2: by adopting the detection method, the retention time of the thiamethoxam is 3.91 min.
The half-life period of thiamethoxam in tomato leaves adopts a first-order kinetic equationC t =C 0 e-kt，
Half-life of thiamethoxam: (t 1/2) By using a derivation formulat 1/2= ln2/k calculation.
In the equationC t Represents the thiamethoxam mass concentration (mg/L) at t,C 0 representing the starting mass concentration of thiamethoxam (mg/L), k representing the degradation rate constant, t representing the time,t 1/2the half-life is indicated.
The half-life results of thiamethoxam from tomato leaves are shown in table 2:
table 2: half-life period of thiamethoxam in tomato leaves
The results from table 2 show that: compared with thiamethoxam water dispersible granules, the half-life period of the thiamethoxam of the nano chitosan-thiamethoxam water agent is prolonged by 2.86 days. The nano chitosan coated thiamethoxam is shown to reduce the release rate of thiamethoxam, so that the half-life period of the thiamethoxam is prolonged.
Example 2
The invention relates to an application of a nano Chitosan (CSA) -thiamethoxam water aqua in the embodiment 1 of the invention in controlling bemisia tabaci, wherein a field plot experiment refers to part 43 of pesticide field efficacy test criteria: the specific application methods of the pesticide for preventing and controlling vegetable bemisia tabaci (NY/T1464.43-2012), the CSA-thiamethoxam water aqua in example 1 and the thiamethoxam water dispersible granule in comparative example 1 are as follows:
the two agents are diluted 3000 times according to 4 g/mu of thiamethoxam effective component, and the front and back sides of cucumber and tomato leaves are sprayed by a conventional sprayer according to the water consumption of 45 kg/mu. The base number before the application of the pesticide was investigated, and the control effect on the bemisia tabaci was calculated by investigating according to tables 3 and 4 after the application of the pesticide.
Table 3: prevention and control effect of nano chitosan combined with thiamethoxam preparation on tomato bemisia tabaci
Table 4: prevention and control effect of nano chitosan-thiamethoxam preparation on cucumber bemisia tabaci
From the results of tables 3 and 4, it can be seen that: the control effect of the CSA-thiamethoxam water agent and the thiamethoxam water dispersible granule on the bemisia tabaci is very high; the early-stage control effect of the CSA-thiamethoxam water agent is lower than that of a thiamethoxam preparation; however, the control period of the CSA-thiamethoxam water agent is longer than that of thiamethoxam. 30 days, the control effect of the CSA-thiamethoxam preparation on Bemisia tabaci on tomatoes and cucumbers still reaches 92.74 percent and 94.49 percent respectively, and is obviously higher than that of thiamethoxam water dispersible granules.
The result shows that the drug effect period of the CSA-thiamethoxam is prolonged by 15 days compared with that of thiamethoxam water dispersible granules.
The foregoing is merely a preferred embodiment of the invention and is not intended to limit the invention in any manner. Although the present invention has been described with reference to the preferred embodiments, it is not intended to be limited thereto. Those skilled in the art can make many possible variations and modifications to the disclosed embodiments, or equivalent modifications, without departing from the spirit and scope of the invention, using the methods and techniques disclosed above. Therefore, any simple modification, equivalent replacement, equivalent change and modification made to the above embodiments according to the technical essence of the present invention are still within the scope of the protection of the technical solution of the present invention.
Claims (10)
1. The nano chitosan-thiamethoxam water aqua is characterized in that a chitosan solution is used as a water phase, a thiamethoxam solution is used as an oil phase, and the oil-in-water nano chitosan-thiamethoxam water aqua is formed.
2. The nanocrystallized chitosan-thiamethoxam aqueous solution according to claim 1, wherein the chitosan solution has a concentration of 0.2 to 0.4% by mass and the thiamethoxam solution has a concentration of 25 to 50% by mass.
3. The preparation method of the nano chitosan-thiamethoxam aqueous solution as claimed in claim 1 or 2, wherein the preparation method comprises the following steps:
s1, emulsifying chitosan, adding HY-266, and stirring and mixing to obtain W-phase working solution;
s2, dissolving thiamethoxam, adding HY-266, and stirring and mixing to obtain O-phase working solution;
and S3, stirring and mixing the W-phase working solution and the O-phase working solution to obtain the nano chitosan-thiamethoxam aqueous solution.
4. The method for preparing the nano chitosan-thiamethoxam aqueous solution according to claim 3, wherein in S1, the specific process of emulsifying the chitosan is as follows: dissolving chitosan in NaAc buffer solution, adding sodium polyphosphate, stirring and mixing until opalescence appears to obtain an emulsified chitosan solution.
5. The method for preparing the nano chitosan-thiamethoxam aqueous solution as claimed in claim 4, wherein the mass volume concentration of the sodium polyphosphate is 0.005-0.008%; the rotating speed of the stirring is 1000 rpm-2000 rpm.
6. The preparation method of the nano chitosan-thiamethoxam aqueous solution as claimed in claim 4 or 5, wherein in S1, the mass volume concentration of HY-266 is 0.003-0.006%.
7. The preparation method of the nano chitosan-thiamethoxam aqueous solution as claimed in claim 4 or 5, wherein in S2, the mass volume concentration of HY-266 is 0.003-0.006%; the rotating speed of stirring and mixing is 1000 rpm-2000 rpm, and the stirring time is 8 min-15 min.
8. The preparation method of the nano chitosan-thiamethoxam aqueous solution as claimed in claim 4 or 5, wherein in S3, the rotation speed of stirring and mixing is 1000 rpm-2000 rpm, and the time is 1.5 h-3 h.
9. The application of the nano chitosan-thiamethoxam aqueous solution as defined in claim 1 or 2 in controlling bemisia tabaci.
10. The application according to claim 9, wherein the application method is as follows: the nano chitosan-thiamethoxam water aqua is diluted by 2000-3000 times and is sprayed on tomato and cucumber leaves.
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|---|---|---|---|---|
| CN114304171A (en) * | 2022-01-11 | 2022-04-12 | 甘肃省科学院生物研究所 | Seed coating agent of ligularia virgaurea extract and preparation method and application thereof |
| CN114304171B (en) * | 2022-01-11 | 2023-11-28 | 甘肃省科学院生物研究所 | Ligularia virgaurea extract seed coating agent and preparation method and application thereof |
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| CN111134119B (en) | 2020-11-20 |
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