CN115886040A - Aquilaria sinensis extract herbicide and application - Google Patents

Aquilaria sinensis extract herbicide and application Download PDF

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CN115886040A
CN115886040A CN202211272607.6A CN202211272607A CN115886040A CN 115886040 A CN115886040 A CN 115886040A CN 202211272607 A CN202211272607 A CN 202211272607A CN 115886040 A CN115886040 A CN 115886040A
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herbicide
aquilaria sinensis
extract
sinensis extract
aquilaria
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CN115886040B (en
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吴华
王显
周海玉
王勇
冯俊涛
马志卿
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Northwest A&F University
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Abstract

The invention provides a aquilaria sinensis extractive herbicide and application thereof, and the aquilaria sinensis extractive is applied to preparing the herbicide. The aquilaria sinensis extract is an alcohol extract of aquilaria sinensis. The preparation method of the aquilaria sinensis extract comprises the following steps: extracting the powdery material with ethanol under reflux to obtain crude extract, and concentrating under reduced pressure to obtain extract; the leaching temperature is 50-80 ℃, and the leaching time is 6-12 h. The weight percentage content of the aquilaria sinensis extractive in the herbicide is 10-50%. The aquilaria sinensis extractive herbicide has a control effect on barnyard grass and cyperus rotundus, has an obvious control effect on common weeds such as alternanthera philoxeroides, purslane and green bristlegrass, and has potential application and popularization values.

Description

Aquilaria sinensis extract herbicide and application
Technical Field
The invention belongs to the technical field of pesticides, particularly relates to a pesticide and preparation thereof, and particularly relates to a aquilaria sinensis extract herbicide and application thereof.
Background
The weeds and the crops compete for fertilizer, light and space, so that the yield and the quality of the crops are seriously influenced. And some weeds are intermediate hosts of crop pests or are laid on the field for overwintering, so that the spread and spread of the pests are facilitated. Thus, to ensure a good harvest of the crop, weeding extends throughout the entire process from sowing to harvesting. Weeds in ornamental lawns not only affect the beauty but also hinder the growth of turf grass, and therefore, weeding is also required.
With the continuous development of lawn career in China, the requirement of environment beautification is increasingly improved, and weed control becomes an important link in the process of lawn maintenance and management. In the early years, the weeding is mainly carried out manually, and the manual weeding is time-consuming and labor-consuming and has low efficiency. With the popularization of science and technology, the application of herbicide pesticides has become more and more common. Herbicide pesticides are synthetic chemicals used to destroy or control weed growth, protect crops and ornamental lawns. The herbicide has the characteristics of rapidness, high efficiency and economy, can greatly improve the labor productivity, is an essential advanced technology for realizing the agricultural modernization, becomes an important guarantee for the stable yield and high yield of the agriculture, and has very important significance for the improvement of the existing cultivation system.
At present, methods for controlling weeds mainly rely on chemical control methods. The chemical prevention method uses chemical pesticide and is applied by a medical instrument, so that the effect is fast, the efficiency is high, the using method is simple and convenient, and the application advantage is unique. However, the use of chemical pesticides in large quantities can cause damage to the ecological environment, and pesticide residues can often cause damage to non-target organisms. The biological control method has the characteristics of environmental friendliness, safety to beneficial organisms in the nature and the like, and is a new idea for urgently seeking to solve the problem of weed control.
Lignum Aquilariae Resinatum (Syringga pinnatifolia Hemsl. Var. Alashanensis Ma et S.Q. Zhou) is a plant of Syzygium of Oleaceae, and is called Syzygium hybridum. The aquilaria sinensis mainly grows in hybrid forests and shrubs in mountainous regions of Heilan, roots and branches are used as medicines, the medicines are harvested at the early spring and late autumn, the outer skin is removed, the core material is taken, dried in the sun and split into small pieces for later use. The lignum Aquilariae Resinatum has pungent and bitter taste, cold, heavy, soft, dry, greasy, dull and soft property, has effects of relieving pain, relieving asthma and clearing heat, and can be used for treating heart heat, cardiodynia, dizziness, insomnia, cardiopalmus, asthma and Heryi disease in Mongolian medicine. The content of volatile oil in lignum Aquilariae Resinatum varies with the growth time, harvesting time, and storage time of the medicinal materials, and the longer the storage time of the medicinal materials, the lower the extraction amount of volatile oil. The composition and content of the chemical components in the volatile oil are also different from medicinal materials, and the volatile oil components are mainly reported to be benzoic acid, camphor, isopropyl benzoic acid, anethole, isobutyl balophenol, alpha-myrcene, cis-caryophyllene, humulene, calamenene, gamma-myrcene, citronene, alpha-cedrene, beta-guaiene, 2-3 methoxy-4- (2-propenyl) phenol acetate, alpha-ylacene, beta-gulene, cadinenol and the like. During the last decade, related pharmacological and chemical component researches are carried out successively by a plurality of domestic teams, and the effects of the volatile oil, the total extract, the separation part and the monomer component of the aquilaria sinensis on myocardial ischemia, cerebral ischemia, tranquilizing and allaying excitement and the like are explained, and sesquiterpenes and lignans are revealed as main chemical components. The sesquiterpenes are used as chemical classification indexes, so that the aquilaria sinensis can be significantly distinguished from other species in the genus. Recently, researchers further isolated and identified 11 new sesquiterpene components from the aquilaria sinensis, wherein the sesquiterpene components relate to 7 types of lupane, lupane (3-5), secolupane, guaiane, caryophyllane, secoeremophilane and isodaucane. Although the aquilaria sinensis is researched and developed rapidly in the field of traditional Chinese medicine, at present, the research on the weed control aspect of the aquilaria sinensis is not reported.
Disclosure of Invention
Experiments show that the aquilaria sinensis extract has herbicidal activity, and a specific medicament formula is provided in field application.
In order to realize the task, the invention adopts the technical scheme that:
application of lignum Aquilariae Resinatum extract in preparing herbicide is provided.
Optionally, the lignum aquilariae resinatum extract is an alcohol extract of lignum aquilariae resinatum.
Optionally, the preparation method of the aquilaria sinensis extract comprises the following steps: extracting the powdery material with ethanol under reflux to obtain crude extract, and concentrating under reduced pressure to obtain extract; the leaching temperature is 50-80 ℃, and the leaching time is 6-12 h.
Optionally, the leaching temperature is 75 ℃.
Optionally, the mass percentage content of the aquilaria sinensis extract in the herbicide is 10-50%.
The active component of the herbicide is the aquilaria sinensis extract, and the content of the aquilaria sinensis extract in the herbicide is 10-50% by mass percent.
Optionally, the herbicide is in a form of a soluble liquid agent, and the soluble liquid agent is prepared from the following raw materials in percentage by mass:
and (3) extracting lignum aquilariae sinensis: 10% -50%, organic solvent: 30-60%, surfactant: 5% -20%, antifreeze: 4 to 10 percent, and the sum of the weight percentages of the raw materials is 100 percent.
Optionally, the herbicide is in the form of microemulsion, and the microemulsion is prepared from the following raw materials in percentage by mass:
and (3) extracting lignum aquilariae sinensis: 10-20%, organic solvent: 30-60%, surfactant: 10% -30%, antifreeze: 4 to 10 percent, and the balance of water, wherein the sum of the weight percentages of the raw materials is 100 percent.
Optionally, the herbicide is in a form of a soluble liquid, and the soluble liquid is prepared from the following raw materials in percentage by mass:
weighing 10-50 kg of aquilaria sinensis extract, 15-35 kg of ethyl acetate and 55-0 kg of sec-butyl acetate, mixing and dissolving, adding 15-10 kg of sodium dodecyl benzene sulfonate and 5kg of ethylene glycol under stirring, and uniformly stirring to obtain 100kg of 10% aquilaria sinensis extract soluble liquid.
Optionally, the herbicide is in the form of microemulsion, and the microemulsion is prepared from the following raw materials in percentage by mass:
weighing 20kg of lignum aquilariae resinatum extract, dissolving in 40kg of ethyl acetate, adding 15kg of calcium dodecyl benzene sulfonate and 5kg of agricultural emulsion 500 under stirring, adding 4kg of ethylene glycol, heating the solution to 40 ℃, and adding 16kg of water under high-speed stirring; stirring for 45min after the dripping is finished, and cooling to obtain the 20% aquilaria sinensis extract microemulsion.
The invention has the following advantages:
the aquilaria sinensis extract provided by the invention has a good weed control effect, has the advantages of environmental protection, high safety, low toxicity, low residue, difficulty in generating drug resistance and the like, and can be used as a potential medicament for preventing and treating diseases caused by phytopathogens.
Detailed Description
In order to better understand the technical content of the present invention, specific examples are provided below to further explain the present invention.
Application of lignum Aquilariae Resinatum extract in preparing herbicide is provided.
The lignum Aquilariae Resinatum extract is alcoholic extract of lignum Aquilariae Resinatum. Specifically, the aquilaria sinensis extract is powder obtained by drying and crushing stems of aquilaria sinensis and sieving the dried stems with a 40-mesh sieve, the powder is extracted by 95% ethanol at 75 ℃ by a reflux method for 3 times, ethanol crude extract at the root of the aquilaria sinensis is obtained after 6 hours each time, and the pressure reduction and concentration are carried out to obtain the aquilaria sinensis extract.
The preparation method of the aquilaria sinensis extract comprises the following steps: extracting the powdery material with ethanol under reflux to obtain crude extract, and concentrating under reduced pressure to obtain extract; the leaching temperature is 50-80 ℃, and the leaching time is 6-12 h. Preferably, the leaching temperature is 75 ℃.
The application shows that the mass percentage content of the aquilaria sinensis extract in the herbicide is 10-50%.
The active ingredient of the aquilaria sinensis extractive herbicide is aquilaria sinensis extractive, and the content of the aquilaria sinensis extractive in the herbicide is 10-50% by mass percent.
The lignum Aquilariae Resinatum extract is prepared by pulverizing stems of lignum Aquilariae Resinatum, extracting with ethanol, and concentrating. More specifically, the temperature of alcohol extraction is 50-80 ℃, and the time of alcohol extraction is 6-12 h.
The preparation form of the herbicide is microemulsion which is prepared from the following raw materials in percentage by mass: and (3) extracting lignum aquilariae sinensis: 10-20%, organic solvent: 30-60%, surfactant: 10% -30%, antifreeze: 4 to 10 percent of water, and the balance of water, wherein the sum of the weight percentages of the raw materials is 100 percent.
The herbicide is in the form of soluble liquid, and the soluble liquid is prepared from the following raw materials in percentage by weight: and (3) extracting lignum aquilariae sinensis: 10% -50%, organic solvent: 30-60%, surfactant: 5% -20%, antifreeze: 4 to 10 percent, and the sum of the weight percentages of the raw materials is 100 percent.
The organic solvent is one or more of solvent oil No. 120, solvent oil No. 150, solvent oil No. 200, ethyl acetate, sec-butyl acetate, cyclohexanone, methyl oleate, and ethanol; the surfactant is one or more of alkyl benzene sulfonate, alkylphenol polyoxyethylene ether, phenethyl phenol polyoxyethylene ether and similar substances, castor oil and ethylene oxide adduct, and aralkyl phenol polyoxyethylene ether formaldehyde condensate; the antifreezing agent is ethylene glycol or glycerol; the thickener is one or more of polyvinyl alcohol, xanthan gum, sodium carboxymethylcellulose and magnesium aluminum silicate.
Further comprising: (1) Adding the auxiliary agent into the obtained aquilaria sinensis extract according to the formula amount, and uniformly mixing in a mixing kettle to obtain an aquilaria sinensis soluble liquid; (2) And (3) putting the obtained aquilaria sinensis extract and the auxiliary agent into a mixing kettle according to the formula amount, wherein the temperature of the mixing kettle is 35-60 ℃, the stirring time is 30min, and cooling after uniform stirring to obtain the aquilaria sinensis microemulsion.
The experimental methods used in the present invention are all conventional methods unless otherwise specified.
The experimental equipment and reagents used in the invention can be purchased and obtained if no special description is provided.
Example 1 preparation of extract of Aquilaria sinensis
Drying and crushing the stems of the aquilaria sinensis, sieving the dried stems with a 40-mesh sieve to obtain 100kg of aquilaria sinensis powder, adding 500kg of 95% ethanol into the powder, heating the mixture to 75 ℃, extracting the mixture for 6h, filtering the mixture, repeating the filtering for 3 times, combining the filtrates to obtain a crude extract of the rhizomes of the aquilaria sinensis, and concentrating the crude extract under reduced pressure to obtain 30kg of aquilaria sinensis extract.
Example 2 test of inhibitory Activity of Aquilaria sinensis extract on weed root growth and shoot growth
Seed germination tests were performed using a small cup method (petri dish). Washing with pure water for 3 times, and soaking for 1 hr. Laying 2 layers of filter paper in a 9cm culture dish, accurately adding 3mL of test solution respectively, adding 3mL of 95% ethanol in a contrast, adding 5mL of distilled water after the solvent is volatilized, selecting target plant seeds with full seeds and uniform sizes, placing the target plant seeds in the culture dish paved with the 2 layers of filter paper, and placing 10 seeds in each culture dish. Each set of treatments was set to 3 replicates. After 7d, the length of the root and the bud of each culture dish is counted, and the inhibition rate is calculated. During primary screening, dissolving the extract of the aquilaria sinensis extract by using 95% ethanol to prepare a solution with the concentration of 500 mu g/mL, sucking 3mL, dropwise adding the solution into a culture dish for spreading old seeds, and measuring after 7d, wherein the test result is shown in table 1.
TABLE 1 Primary Screen inhibition Activity of Aquilaria sinensis extract on root and shoot growth of barnyard grass and purslane
Figure BDA0003895300600000051
Note: table 1 shows the data of the preliminary screening experiment. The concentration of the aquilaria sinensis extract is 500 mug/mL. Control agents: 115.4 mu g/mL of bensulfuron methyl (purslane) as a water dispersible granule; emulsifiable concentrate haloxyfop-methyl (barnyard grass) 10.8. Mu.g/mL.
Example 3 preparation of 10% soluble concentrate of Aquilaria sinensis extract
Weighing 10kg of aquilaria sinensis extract, 15kg of ethyl acetate and 55kg of sec-butyl acetate, dissolving, adding 15kg of sodium dodecyl benzene sulfonate and 5kg of ethylene glycol under stirring, and uniformly stirring to obtain 100kg of 10% aquilaria sinensis extract soluble liquid M1.
Example 4 preparation of 20% Aquilaria sinensis extract microemulsion
Weighing 20kg of lignum aquilariae resinatum extract, dissolving in 40kg of ethyl acetate, adding 15kg of calcium dodecyl benzene sulfonate and 5kg of agricultural emulsion 500 under stirring, adding 4kg of ethylene glycol, heating the solution to 40 ℃ in a homogenizer, and adding 16kg of deionized water under high-speed stirring; stirring for 45min after the dropwise addition, and cooling to obtain 20% lignum Aquilariae Resinatum extract microemulsion M2.
EXAMPLE 5 preparation of 50% soluble concentrate of Aquilaria sinensis extract
50kg of aquilaria sinensis extract and 35kg of ethyl acetate are weighed, 10kg of sodium dodecyl benzene sulfonate and 5kg of ethylene glycol are added under stirring, and 100kg of 50% aquilaria sinensis extract soluble liquid M3 is obtained after uniform stirring.
Example 6 M1 control of weeds in vegetable fields
In the greenhouse vegetable land of the five spring town of Yangling, 3 fields for planting perennial vegetables are selected, and each field is 667m 2 . The M1 produced in the example 3 is directly diluted by 500 times, the contrast medicament 20 percent of the napropamide missible oil is diluted by 1000 times and is mixed with water for spraying, and the result shows that the control effect of the M1 medicament on the pond of horse, green bristlegrass, xanthium and purslane reaches about 72.12 to 80.96 percent, and is slightly higher than the contrast medicament 20 percent of the napropamide missible oil treatment group, which is shown in the table 2.
Figure BDA0003895300600000052
TABLE 2 field test results for M1 control of dry land weeds
Figure BDA0003895300600000061
Example 7 M2 control of aquatic weeds
A large amount of barnyard grass, alternanthera philoxeroides, cyperus rotundus and other aquatic weeds exist in farmlands in Shaanxi purple Yang county, so that rice production is damaged. M2 prepared as in example 4 was sprayed on, the control agent was 10% bentazon as a water-based solution, and the results of the random plot test were as follows. Each cell 25m 2 5 surveys in each cell with a survey area of 1m 2 . The pesticide is sprayed in the 4-6 leaf stage of the rice, and the pesticide damage to the rice can not be caused. Specific results are shown in table 3, the effect of the bentazone aqua is investigated thirty days after the application, and when the M2 is used for 100 g/mu, the control effect reaches 60-70 percent and is obviously higher than 10 percent. The number of surviving plants is the average of 3 replicates per drug concentration treatment survey cell.
Figure BDA0003895300600000062
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TABLE 3 field test results for M2 control of farmland weeds
Figure BDA0003895300600000063
Example 8 M1, M2 and M3 control of weeds in corn fields
In the corn field from Zhou county in Shaanxi province, weeds are clustered in spring. Spraying M1, M2 and M3 preparations, using 30% glyphosate water solution as contrast agent, and dividing each cell into 4M cells by random cell test 2 4 survey points per cell, survey area 0.25m 2 . The number of surviving plants is the average of 3 replicates per drug concentration treatment survey cell.
Figure BDA0003895300600000064
As a result, as shown in table 4, the control effect of the agents M2 and M3 was higher than that of the agent control, and the control effect of the agent M1 was significantly lower than that of the agent control.
TABLE 4 results of field test for corn field weed control by M1, M2 and M3
Figure BDA0003895300600000071
Example 9 M1, M2 and M3 control of Soybean field weeds
In a certain rural area of a suburb of Sichuan province, a plurality of weeds grow in one 20 mu of soybean land,random cell experiments were used and the results are given below. Divide each cell into 64m 2 Investigation of 4 points per cell with investigation area of 1m 2 . The herbicide is used for fresh weight control effect tests of soybean field weeds, when the herbicide is applied, the soybean is applied in a 4-5 leaf stage, and the herbicide is applied in a 2-3 leaf stage of the weeds, and agents such as M1, M2, M3, 20% bromoxynil emulsifiable concentrate, 50% atrazine wettable powder and the like are sprayed, and the fresh weight control effect on the weeds is investigated 30 days after the herbicide is applied. The results are shown in Table 5.
Figure BDA0003895300600000072
TABLE 5 results of field test for controlling weeds in soybean fields with M1, M2 and M3
Figure BDA0003895300600000073
As can be seen from Table 5, the fresh weight inhibition effect of the M1, the M2 and the M3 for controlling the weeds in the soybean field is obviously higher than that of the control medicament, namely 20 percent bromoxynil emulsifiable solution and 50 percent atrazine wettable powder 30 days after the mixed herbs are treated, and the development potential is very high.
Although the invention has been described in detail hereinabove with respect to a general description and specific embodiments thereof, it will be apparent to those skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.

Claims (10)

1. Application of lignum Aquilariae Resinatum extract in preparing herbicide is provided.
2. The use of claim 1, wherein the aquilaria sinensis extract is an alcohol extract of aquilaria sinensis.
3. The use as claimed in claim 1 or 2, wherein the preparation method of the aquilaria sinensis extract comprises the following steps:
extracting the powdery material with ethanol under reflux to obtain crude extract, and concentrating under reduced pressure to obtain extract;
the leaching temperature is 50-80 ℃, and the leaching time is 6-12 h.
4. Use according to claim 3, wherein the leaching temperature is 75 ℃.
5. The use as claimed in claim 1 or 2, wherein the mass percentage of the aquilaria sinensis extract in the herbicide is 10-50%.
6. The aquilaria sinensis extract herbicide is characterized in that the active ingredient of the herbicide is the aquilaria sinensis extract, and the content of the aquilaria sinensis extract in the herbicide is 10-50% by mass percent.
7. The aquilaria sinensis extract herbicide as claimed in claim 6, wherein the herbicide is in the form of a soluble liquid, and the soluble liquid is prepared from the following raw materials in percentage by mass:
and (3) extracting lignum aquilariae sinensis: 10% -50%, organic solvent: 30-60%, surfactant: 5% -20%, antifreeze: 4 to 10 percent, and the sum of the weight percentages of the raw materials is 100 percent.
8. The aquilaria sinensis extract herbicide as claimed in claim 6, wherein the herbicide is in the form of a microemulsion, and the microemulsion is prepared from the following raw materials in percentage by mass:
and (3) extracting lignum aquilariae resinatum: 10-20%, organic solvent: 30-60%, surfactant: 10% -30%, antifreeze: 4 to 10 percent, and the balance of water, wherein the sum of the weight percentages of the raw materials is 100 percent.
9. The aquilaria sinensis extract herbicide as claimed in claim 6, wherein the herbicide is in the form of a soluble liquid, and the soluble liquid is prepared from the following raw materials in percentage by mass:
weighing 10-50 kg of aquilaria sinensis extract, 15-35 kg of ethyl acetate and 55-0 kg of sec-butyl acetate, mixing and dissolving, adding 15-10 kg of sodium dodecyl benzene sulfonate and 5kg of ethylene glycol under stirring, and stirring uniformly to obtain 100kg of 10% aquilaria sinensis extract soluble liquid.
10. The aquilaria sinensis extract herbicide as claimed in claim 6, wherein the herbicide is in the form of a microemulsion, and the microemulsion is prepared from the following raw materials in percentage by mass:
weighing 20kg of lignum aquilariae resinatum extract, dissolving in 40kg of ethyl acetate, adding 15kg of calcium dodecyl benzene sulfonate and 5kg of agricultural emulsion 500 under stirring, adding 4kg of ethylene glycol, heating the solution to 40 ℃, and adding 16kg of water under high-speed stirring; stirring for 45min after the dripping is finished, and cooling to obtain 20% of aquilaria sinensis extract microemulsion.
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