CN113729035B - Glyphosate compound aqueous solution and preparation method and application thereof - Google Patents
Glyphosate compound aqueous solution and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a glyphosate compound aqueous solution, which comprises the following main active ingredients: glyphosate, walnut leaf water extract, vinca alkaloid; the compound water agent comprises the following raw materials in parts by weight: 15-20 g of glyphosate, 5-8 g of walnut leaf water extract, 4-6 g of vinca alkaloid, 1-2 g of solubilizer, 0.5-1 g of stabilizer and 500-600 mL of water; meanwhile, a preparation method of the glyphosate compound aqueous solution and application of the glyphosate compound aqueous solution are also disclosed. The invention not only reduces the using amount of chemical pesticide, but also overcomes the defects of slow biological pesticide and higher using cost, effectively protects crops from being damaged by pests, avoids much pollution and damage to the ecological environment, realizes the purposes of expanding weeding spectrum, increasing weeding effect and accelerating weeding speed of glyphosate, and has good market prospect.
Description
Technical Field
The invention belongs to the technical field of pesticide preparations, and particularly relates to a glyphosate compound aqueous solution, and a preparation method and application thereof.
Background
Glyphosate, chemical name is N- (phosphomethyl) glycine, chemical formula is C3H8NO5P is an environmentally-friendly systemic conduction type broad-spectrum biocidal herbicide and has a very good effect on perennial weeds and biennial grass weeds. Due to the excellent weed control activity, the wide weed control spectrum, the lower soil residue, the longer weed control time and the large-scale planting of the herbicide-resistant transgenic crops, the glyphosate becomes the first herbicide variety in the global market. However, in recent years, the long-term, single, continuous and widespread use of glyphosate has led to an increase in resistant weed individuals and populations year by year, a decrease in the control effect of herbicides, and an increase in the cost of weed control. Up to now, it has been published that weeds of over 31 organisms, such as goosegrass, horseweed, ryegrass, kochia, etc., develop resistance to glyphosate. In addition, the increase of the dosage of the glyphosate is easy to cause the phytotoxicity risk of crops and environmental pollution.
Currently, comprehensive management (IWM) of weeds becomes the principal principle of agricultural production, and the most important of IWM is diversity of chemical control, namely, reasonable compounding or alternative application of herbicides with different action modes, so that excessive use of a single active ingredient or different active ingredients with the same action mode is avoided; the purpose is to mutually synergize, expand the control spectrum, delay the generation of weed resistance, simultaneously realize the complementation of advantages and disadvantages and make up the deficiency of the effect of glyphosate on certain broadleaf weeds.
The compounding of different compounds has become an important direction for pesticide innovation, and the compounding registration of glyphosate and fomesafen is obtained in 2009 and 2010 by Zusanhuda company respectively, so that the compounded product can effectively prevent and kill some glyphosate-resistant weeds (such as amaranth weeds) in cotton fields and soybean fields, and can effectively prevent and kill morning glory and abutilon which are poor in effect when glyphosate is used alone. The united states FMC company, under the product name Broadway, obtained the registration of glyphosate and carfentrazone in australia in 2010, the two herbicide actives performed better than glyphosate alone. On one hand, the quick-acting performance of Broadway is superior to that of a single glyphosate agent; on the other hand, the product can prevent and kill broad-leaved weeds such as purslane, mallow and the like with strong glyphosate tolerance. Therefore, the combination of glyphosate and compounds with different action modes becomes an effective means for solving the problem of weed resistance. In China, 16 compound certificates exist in the aspect of glyphosate compound registration, and glyphosate compound has achieved certain effect, but all registered compound herbicides are presented by chemical agents, and the chemical pesticide components are increased and difficult to degrade, so that the problems of pesticide residues, plant phytotoxicity, environmental pollution and the like are increasingly severe.
Most of plant-derived pesticides are secondary metabolites generated by interaction with the environment in the long-term evolution process of plants, have reasonable degradation ways in the nature, are relatively safe to non-target organisms and the environment, and are increasingly paid more attention to research. Plant-derived pesticides are both mutually promoting and mutually inhibiting by biochemical substances (i.e. allelochemicals) which have been identified as mostly products of the shikimic acid and acetic acid pathways, such as phenols, cinnamic acid, tannins, flavonoids, terpenoids, alkaloids, steroids and quinones.
In conclusion, the invention develops a novel, environment-friendly, natural and safe herbicide, which is prepared by compounding glyphosate and a botanical pesticide, so that the dosage of the chemical pesticide is reduced, the defects of slow biological pesticide and high use cost are overcome, the crops are effectively protected from being damaged by pests, a lot of pollution and damage to the ecological environment are avoided, and the herbicide has wide market prospect, economic benefit and social benefit.
Disclosure of Invention
In order to solve the problems, the invention aims to provide a glyphosate compound aqueous solution with high efficiency and remarkable use, and also provides a preparation method of the glyphosate compound aqueous solution and application of the glyphosate compound aqueous solution.
In order to achieve the purpose, the invention adopts the following technical scheme:
a glyphosate compound aqueous solution comprises the following main active ingredients: glyphosate, walnut leaf aqueous extract, vinca alkaloids; the compound water agent comprises the following raw materials in parts by weight: 15-20 g of glyphosate, 5-8 g of walnut leaf water extract, 4-6 g of vinca alkaloid, 1-2 g of solubilizer, 0.5-1 g of stabilizer and 500-600 mL of water.
Further, the walnut leaf aqueous extract is prepared according to the following steps: drying and crushing walnut leaves, adding water, soaking for 0.5-1.5 hours at normal temperature, wherein the material-liquid ratio of the walnut leaves to the water is 1g: 25-30 ml, filtering, extracting the filtrate for 3 times by using an extracting agent, merging organic phases, and performing desolventizing to obtain the walnut leaf water extract, namely the flavonoid compound.
Further, the above-mentioned extractant is dehydrated ether, ethyl acetate, chloroform, n-butanol or dichloromethane.
Further, the vinca alkaloid is prepared according to the following steps:
s1, placing the catharanthus roseus in an oven at 80-90 ℃ for drying for 2-3 h, crushing, extracting with ethanol with the mass percentage concentration of 70-95% at normal temperature, wherein the material-liquid ratio of the catharanthus roseus to the ethanol is 1g: 10-15 ml, the extraction time is 20-25 h, sequentially filtering with gauze and filter paper, and respectively collecting filtrate and filter residues;
s2, performing ultrasonic assisted extraction on the filter residue obtained in the step S1 for 20-30 min at the temperature of 60-80 ℃ by using 20-30% by mass of ethanol again, wherein the power of ultrasonic is 300-500W, the material-liquid ratio of the filter residue to the ethanol is 1g: 5-7 ml, filtering, collecting filtrate, and combining the filtrate and the filtrate obtained in the step S1 to obtain two extracting solutions; concentrating the extractive solution under reduced pressure with rotary evaporator to obtain ethanol extract;
s3, slowly pouring the ethanol extract obtained in the step S2 into macroporous resin for adsorption treatment, and eluting with n-hexane or petroleum ether until the eluent is colorless and transparent; eluting the macroporous resin with eluent, collecting the eluent, detecting by TLC method, and stopping collecting until no alkaloid is detected; concentrating and desolventizing to obtain the vinca alkaloid.
Further, in the above step S3, the macroporous resin is AB-8, D101, D201, D301, or HPD 100.
Further, in the step S3, the eluent is a mixed solution of a first solvent and a second solvent in a volume ratio of 1: 3-5, the first solvent is ethanol, methanol, or acetone, and the second solvent is n-hexane or petroleum ether.
Further, the solubilizer is one of beta-cyclodextrin, gamma-cyclodextrin, 2-hydroxyethyl-beta-cyclodextrin, 2-hydroxypropyl-beta-cyclodextrin and 2, 6-dimethyl-beta-cyclodextrin.
Further, the stabilizer is one of trimethyl phosphite, ethylene glycol and epichlorohydrin.
A preparation method of a glyphosate compound aqueous solution comprises the following steps: putting the glyphosate, the walnut leaf water extract, the vinca alkaloid, the solubilizer and the stabilizer into water according to the proportion, and stirring at a high speed of 500-800 r/min for 20-30 min at normal temperature to uniformly mix the materials to obtain the glyphosate compound aqueous solution.
Further, the mass percentage of the glyphosate in the glyphosate compound aqueous solution is 2.0-4.0%.
The invention also aims to provide the application of the glyphosate compound aqueous solution prepared by the preparation method as a herbicide.
A weeding activity test method of a glyphosate compound aqueous solution comprises the following steps: uniformly placing 20-30 weed seeds in culture dishes with filter paper, adding 5-8 mL of glyphosate compound aqueous solution into each culture dish, wherein the mass percentage concentration of glyphosate in the glyphosate compound aqueous solution is 2-4%, and placing the culture dish into an intelligent plant incubator with the temperature of 25 +/-2 ℃, the illumination time of 10-12 h and the humidity of 70-80% for culturing for 7 days; the root length and stem length of the weeds were measured and compared with a blank control group treated with distilled water and a positive control group treated with a 10% glyphosate single-dose solution by mass.
The walnut plant has allelopathy and juglone can inhibit the growth of plant, and no weed grows under the walnut wood. Through research, the walnut leaf water extract contains phenols, flavonoids, phytosterol and terpenoids, wherein the content of the flavonoids is as high as 7.26%, and the flavonoid is also a main component of the walnut leaf water extract for expressing the herbicidal activity, and provides a basis for developing pollution-free botanical pesticides.
Vinca rosea contains alkaloids such as vinblastine, vincristine and vinblastine epoxide, and the vinblastine ring of the substance is a nine-membered ring structure formed by connecting piperidine ring and indole structure. The piperidine and indole heterocyclic compounds have wide biological activities such as insecticidal, bactericidal, herbicidal and plant virus resistant activities, and have the characteristics of good selectivity, high activity, low toxicity and the like. Therefore, the vinca alkaloid with piperidine and indole heterocyclic structures has good development prospect in the aspect of agricultural herbicides.
Because the vinca alkaloid is alkaline, when the vinca alkaloid is compounded with glyphosate, the amino group and the glyphosate carboxyl group on the vinca alkaloid structure form salt to enhance the water solubility of the vinca alkaloid, and can also enhance the long-acting property of the alkaloid release, the concentration of the alkaloid can maintain a stable state for a long time, and the durability of weed control is enhanced.
Due to the adoption of the technical scheme, the invention has the following advantages:
the glyphosate compound aqueous solution disclosed by the invention is wide in raw material source, low in cost and simple in compound operation, takes glyphosate as a basic raw material, utilizes walnut leaf water extract taking flavone as a main component and vinca alcohol extract taking alkaloid as a main component as a synergist, has outstanding synergistic effect and small toxic and side effects, is matched with a solubilizer and a stabilizer, fully exerts the synergistic effect of the two through compound and fusion, forms a strong-effect glyphosate compound aqueous solution, and can realize the purposes of expanding a weeding spectrum, increasing (resistant weeds) weeding effect and accelerating the weeding speed of glyphosate; the glyphosate compound aqueous solution is used for treating weed seeds (amaranthus retroflexus and barnyard grass) subjected to impurity removal and disinfection, the inhibition effect of the compound agent on weeds is determined by a seed germination method, compared with a glyphosate single agent, the inhibition rate of the glyphosate compound aqueous solution on roots and stems of the weeds can be respectively improved by 40-50%, the effect is obvious, and the glyphosate compound aqueous solution has a good market prospect.
Detailed Description
The present invention will be described in further detail with reference to the following examples; however, the following examples are merely illustrative, and the present invention is not limited to these examples.
Example 1
(1) Preparing the aqueous extract of walnut leaves
Drying and crushing walnut leaves, adding water to soak for 0.5h at normal temperature, wherein the mass ratio of the walnut leaves to the water is 1g: 25ml, filtering, extracting the filtrate with anhydrous ether for 3 times, combining organic phases, and desolventizing to obtain folium Juglandis flavone extract; standby;
(2) and preparation of vinca alkaloids
S1, drying catharanthus roseus in an oven at 80 ℃ for 2h, crushing, extracting with 70% ethanol at normal temperature, wherein the material-liquid ratio of the catharanthus roseus to the ethanol is 1g to 10ml, the extraction time is 20h, filtering with gauze and filter paper, and collecting filtrate and filter residue respectively;
s2, performing ultrasonic assisted extraction on the filter residue obtained in the step S1 for 20min at the temperature of 60 ℃ by using 20% ethanol in percentage by mass, wherein the power of ultrasonic is 300W, the material-liquid ratio of the filter residue to the ethanol is 1g:5ml, filtering, collecting filtrate, and combining the filtrate and the filtrate obtained in the step S1 to obtain two extracting solutions; concentrating the extractive solution under reduced pressure with rotary evaporator to obtain ethanol extract;
s3, slowly pouring the ethanol extract obtained in the step S2 into AB-8 type macroporous resin for adsorption treatment, and eluting by using normal hexane to remove substances with small polarity and partial pigments until the eluent is colorless and transparent; eluting the macroporous resin by using a mixed solution of ethanol and n-hexane in a volume ratio of 1:3 as an eluent, collecting the eluent, detecting by using a TLC (thin layer chromatography) method, and stopping collecting until no alkaloid is detected; concentrating and desolventizing to obtain Catharanthus roseus alkaloid; standby;
(3) and (2) preparing glyphosate compound aqueous solution by using walnut leaf aqueous extract and vinca alkaloid obtained in the steps (1) and (2) respectively
Adding 15g of glyphosate, 5g of walnut leaf water extract, 4g of vinca alkaloid, 1g of beta-cyclodextrin and 0.8g of trimethyl phosphite into 600mL of water; and stirring the mixture on a magnetic stirrer for 20min at the stirring speed of 500r/min at normal temperature to obtain the glyphosate compound aqueous solution of uniform solution.
The weeding activity test method of the glyphosate compound aqueous solution comprises the following steps: respectively taking 20 amaranthus retroflexus and barnyard grass seeds, uniformly placing the seeds in culture dishes attached with 2 layers of filter paper, adding 5mL of glyphosate compound aqueous solution into each culture dish, wherein the mass percentage concentration of glyphosate in the glyphosate compound aqueous solution is 2.4%, and placing the culture dish into an intelligent plant incubator with the temperature of 25 ℃, the illumination time of 10 hours and the humidity of 70% for culturing for 7 days; by measuring the root length and stem length of the weeds amaranthus retroflexus and barnyard grass, comparing the growth inhibition effect of the glyphosate compound aqueous solution on the barnyard grass and the amaranthus retroflexus, and comparing the growth inhibition effect with a blank control group treated by distilled water and a positive control group treated by a glyphosate single-agent solution with the mass percentage concentration of 10%, the result shows that: after the treatment of the glyphosate compound aqueous solution with the glyphosate mass percentage concentration of 2.4%, the root length of the barnyard grass is 3.8cm, the stem length is 7.5cm, the root length of the Amaranthus retroflexus is 5.2cm, and the stem length is 6.4 cm.
Example 2
(1) Preparing the aqueous extract of walnut leaves
Drying and crushing walnut leaves, adding water to soak for 0.8h at normal temperature, wherein the mass ratio of the walnut leaves to the water is 1g: 25ml, filtering, extracting the filtrate with ethyl acetate for 3 times, combining organic phases, and desolventizing to obtain folium Juglandis flavone extract; standby;
(2) and preparation of vinca alkaloids
S1, drying the catharanthus roseus in an oven at 83 ℃ for 2.2h, crushing, extracting with 75% ethanol by mass at normal temperature, wherein the material-liquid ratio of the catharanthus roseus to the ethanol is 1g to 11ml, the extraction time is 20h, filtering with gauze and filter paper, and respectively collecting filtrate and filter residue;
s2, carrying out ultrasonic assisted extraction on the filter residue obtained in the step S1 for 20min at the temperature of 65 ℃ by using 22% ethanol in percentage by mass again, wherein the power of ultrasonic is 350W, the material-liquid ratio of the filter residue to the ethanol is 1g:5.5ml, filtering, collecting filtrate, and combining the filtrate and the filtrate obtained in the step S1 to obtain two extracting solutions; concentrating the extractive solution under reduced pressure with rotary evaporator to obtain ethanol extract;
s3, slowly pouring the ethanol extract obtained in the step S2 into D101 type macroporous resin for adsorption treatment, and eluting by using normal hexane to remove substances with small polarity and partial pigments until the eluent is colorless and transparent; eluting the macroporous resin by using a mixed solution of methanol and n-hexane in a volume ratio of 1:3 as an eluent, collecting the eluent, detecting by using a TLC (thin layer chromatography) method, and stopping collecting until no alkaloid is detected; concentrating and desolventizing to obtain Catharanthus roseus alkaloid; standby;
(3) and (2) preparing glyphosate compound aqueous solution by using walnut leaf aqueous extract and vinca alkaloid obtained in the steps (1) and (2) respectively
Adding 17g of glyphosate, 6g of walnut leaf water extract, 4g of vinca alkaloid, 1.2g of gamma-cyclodextrin and 0.5g of ethylene glycol into 500mL of water; and stirring the mixture on a magnetic stirrer for 25min at the stirring speed of 700r/min at normal temperature to obtain the glyphosate compound aqueous solution with a uniform system.
The weeding activity test method of the glyphosate compound aqueous solution comprises the following steps: respectively taking 20 amaranthus retroflexus seeds and barnyard grass seeds, respectively and uniformly placing the seeds in culture dishes attached with 2 layers of filter paper, adding 6mL of glyphosate compound aqueous solution into each culture dish, wherein the mass percentage concentration of glyphosate in the glyphosate compound aqueous solution is 3.2%, and placing the culture dishes into an intelligent plant incubator with the temperature of 23 ℃, the illumination time of 12 hours and the humidity of 75% for culturing for 7 days; by measuring the root length and stem length of the weeds amaranthus retroflexus and barnyard grass, the growth inhibition effect of the glyphosate compound aqueous solution on the barnyard grass and the amaranthus retroflexus is compared, and the results of the comparison with a blank control group treated by distilled water and a control group treated by a glyphosate single-agent solution with the mass percentage concentration of 10% show that: after the treatment of the glyphosate compound aqueous solution with the glyphosate mass percentage concentration of 3.2%, the root length of the barnyard grass is 2.8cm, the stem length is 6.9cm, and the root length of the amaranthus retroflexus is 4.2cm and the stem length is 5.5 cm.
Example 3
(1) Preparing the aqueous extract of walnut leaves
Drying and crushing walnut leaves, adding water to soak the walnut leaves for 1.0 hour at normal temperature, wherein the mass ratio of the walnut leaves to the water is 1g: 28ml, filtering, extracting the filtrate with ethyl acetate for 3 times, combining organic phases, and desolventizing to obtain folium Juglandis flavone extract; standby;
(2) and preparation of vinca alkaloids
S1, drying catharanthus roseus in an oven at 85 ℃ for 2.5h, crushing, extracting with 80% ethanol at normal temperature, wherein the material-liquid ratio of the catharanthus roseus to the ethanol is 1g:13ml, the extraction time is 22h, filtering with gauze and filter paper, and respectively collecting filtrate and filter residue;
s2, performing ultrasonic assisted extraction on the filter residue obtained in the step S1 for 25min at the temperature of 70 ℃ by using 25% by mass of ethanol again, wherein the power of ultrasonic is 400W, the material-liquid ratio of the filter residue to the ethanol is 1g:6ml, filtering, collecting filtrate, and combining the filtrate and the filtrate obtained in the step S1 to obtain two extracting solutions; concentrating the extractive solution under reduced pressure with rotary evaporator to obtain ethanol extract;
s3, slowly pouring the ethanol extract obtained in the step S2 into D201 type macroporous resin for adsorption treatment, and eluting with petroleum ether to remove substances with low polarity and part of pigments until the eluent is colorless and transparent; eluting the macroporous resin by using a mixed solution of methanol and petroleum ether with a volume ratio of 1:4 as an eluent, collecting the eluent, detecting by using a TLC (thin layer chromatography) method, and stopping collecting until no alkaloid is detected; concentrating and desolventizing to obtain Catharanthus roseus alkaloid; standby;
(3) and (2) preparing glyphosate compound aqueous solution by using walnut leaf aqueous extract and vinca alkaloid obtained in the steps (1) and (2) respectively
Adding 16g of glyphosate, 5g of walnut leaf water extract, 6g of vinca alkaloid, 1.8g of 2-hydroxyethyl-beta-cyclodextrin and 1g of trimethyl phosphite into 510mL of water; and stirring the mixture on a magnetic stirrer for 30min at the stirring speed of 500r/min at normal temperature to obtain the glyphosate compound aqueous solution of uniform solution.
The weeding activity test method of the glyphosate compound aqueous solution comprises the following steps: respectively and uniformly placing 20 amaranthus retroflexus and barnyard grass seeds in culture dishes attached with 2 layers of filter paper, adding 7mL of glyphosate compound aqueous solution into each culture dish, wherein the mass percentage concentration of glyphosate in the glyphosate compound aqueous solution is 2.9%, and placing the culture dish into an intelligent plant incubator with the temperature of 26 ℃, the illumination time of 11h and the humidity of 78% for culturing for 7 days; by measuring the root length and stem length of the weeds amaranthus retroflexus and barnyard grass, the growth inhibition effect of the glyphosate compound aqueous solution on the barnyard grass and the amaranthus retroflexus is compared, and the results are shown in the following comparison with a blank control group treated by distilled water and a control group treated by a glyphosate single-agent solution with the mass percentage concentration of 10 percent: after the treatment of the glyphosate compound aqueous solution with the glyphosate mass percentage concentration of 2.9%, the root length of the barnyard grass is 3.4cm, the stem length is 7.1cm, the root length of the amaranthus retroflexus is 4.0cm, and the stem length is 6.1 m.
Example 4
(1) Preparing the aqueous extract of walnut leaves
Drying and crushing walnut leaves, adding water, and soaking for 1.3 hours at normal temperature, wherein the mass ratio of the walnut leaves to the water is 1g: 30ml, filtering, extracting the filtrate with chloroform for 3 times, combining organic phases, and desolventizing to obtain folium Juglandis flavone extract; standby;
(2) and preparation of vinca alkaloids
S1, drying the catharanthus roseus in an oven at 88 ℃ for 3h, crushing, extracting at normal temperature by using 88% ethanol in percentage by mass, wherein the material-liquid ratio of the catharanthus roseus to the ethanol is 1g:14ml, the extraction time is 25h, filtering by using gauze and filter paper, and respectively collecting filtrate and filter residue;
s2, performing ultrasonic assisted extraction on the filter residue obtained in the step S1 for 30min at the temperature of 75 ℃ by using 28% ethanol in percentage by mass, wherein the power of ultrasonic is 450W, the material-liquid ratio of the filter residue to the ethanol is 1g:7ml, filtering, collecting filtrate, and combining the filtrate and the filtrate obtained in the step S1 to obtain two extracting solutions; concentrating the extractive solution under reduced pressure with rotary evaporator to obtain ethanol extract;
s3, slowly pouring the ethanol extract obtained in the step S2 into D301 macroporous resin for adsorption treatment, and eluting by using normal hexane to remove substances with small polarity and partial pigments until the eluent is colorless and transparent; eluting the macroporous resin by using a mixed solution of acetone and n-hexane in a volume ratio of 1:5 as an eluent, collecting the eluent, detecting by using a TLC (thin layer chromatography) method, and stopping collecting until no alkaloid is detected; concentrating and desolventizing to obtain Catharanthus roseus alkaloid; standby;
(3) and (2) preparing glyphosate compound aqueous solution by using walnut leaf aqueous extract and vinca alkaloid obtained in the steps (1) and (2) respectively
Adding 18g of glyphosate, 6g of walnut leaf water extract, 6g of vinca alkaloid, 1.8g of 2, 6-dimethyl-beta-cyclodextrin and 1g of epichlorohydrin into 550mL of water; stirring the mixture on a magnetic stirrer for 20min at the stirring speed of 800r/min under the condition of normal temperature to obtain the glyphosate compound aqueous solution of uniform solution.
The weeding activity test method of the glyphosate compound aqueous solution comprises the following steps: respectively taking 20 amaranthus retroflexus seeds and barnyard grass seeds, respectively and uniformly placing the seeds in culture dishes attached with 2 layers of filter paper, adding 8mL of glyphosate compound aqueous solution into each culture dish, wherein the mass percentage concentration of glyphosate in the glyphosate compound aqueous solution is 3.1%, and placing the culture dish into an intelligent plant incubator with the temperature of 25 ℃, the illumination time of 11h and the humidity of 78% for culturing for 7 days; by measuring the root length and stem length of the weeds amaranthus retroflexus and barnyard grass, the growth inhibition effect of the glyphosate compound aqueous solution on the barnyard grass and the amaranthus retroflexus is compared, and the results are shown in the following comparison with a blank control group treated by distilled water and a control group treated by a glyphosate single-agent solution with the mass percentage concentration of 10 percent: after the treatment of the glyphosate compound aqueous solution with the glyphosate mass percentage concentration of 3.1%, the root length of the barnyard grass is 3.1cm, the stem length is 6.9cm, the root length of the amaranthus retroflexus is 4.4cm, and the stem length is 5.8 cm.
Example 5
(1) Preparing the aqueous extract of walnut leaves
Drying and crushing walnut leaves, adding water to soak the walnut leaves for 1.5 hours at normal temperature, wherein the mass ratio of the walnut leaves to the water is 1g: 30ml, filtering, extracting the filtrate with anhydrous ether for 3 times, combining organic phases, and desolventizing to obtain folium Juglandis flavone extract; standby;
(2) and preparation of vinca alkaloids
S1, drying catharanthus roseus in an oven at 90 ℃ for 2h, crushing, extracting with 95% ethanol at normal temperature, wherein the material-liquid ratio of the catharanthus roseus to the ethanol is 1g:15ml, the extraction time is 25h, filtering with gauze and filter paper, and respectively collecting filtrate and filter residue;
s2, performing ultrasonic assisted extraction on the filter residue obtained in the step S1 for 30min at 80 ℃ by using 30% ethanol in percentage by mass, wherein the power of ultrasonic is 500W, the material-liquid ratio of the filter residue to the ethanol is 1g:7ml, filtering, collecting filtrate, and combining the filtrate and the filtrate obtained in the step S1 to obtain two extracting solutions; concentrating the extractive solution under reduced pressure with rotary evaporator to obtain ethanol extract;
s3, slowly pouring the ethanol extract obtained in the step S2 into HPD100 type macroporous resin for adsorption treatment, and eluting by using normal hexane to remove substances with small polarity and partial pigments until the eluent is colorless and transparent; eluting the macroporous resin by using a mixed solution of acetone and petroleum ether in a volume ratio of 1:5 as an eluent, collecting the eluent, detecting by using a TLC (thin layer chromatography) method, and stopping collecting until no alkaloid is detected; concentrating and desolventizing to obtain Catharanthus roseus alkaloid; standby;
(3) and (2) preparing glyphosate compound aqueous solution by using walnut leaf aqueous extract and vinca alkaloid obtained in the steps (1) and (2) respectively
Adding 20g of glyphosate, 8g of walnut leaf water extract, 6g of vinca alkaloid, 2g of 2-hydroxypropyl-beta-cyclodextrin and 1g of trimethyl phosphite into 500mL of water; and stirring the mixture on a magnetic stirrer for 30min at the stirring speed of 800r/min at normal temperature to obtain the glyphosate compound aqueous solution of uniform solution.
The weeding activity test method of the glyphosate compound aqueous solution comprises the following steps: respectively taking 20 amaranthus retroflexus seeds and barnyard grass seeds, respectively and uniformly placing the seeds in culture dishes attached with 2 layers of filter paper, adding 8mL of glyphosate compound aqueous solution into each culture dish, wherein the mass percentage concentration of glyphosate in the glyphosate compound aqueous solution is 3.7%, and placing the culture dishes into an intelligent plant incubator with the temperature of 27 ℃, the illumination time of 12 hours and the humidity of 80% for culture for 7 days; by measuring the root length and stem length of the weeds amaranthus retroflexus and barnyard grass, the growth inhibition effect of the glyphosate compound aqueous solution on the barnyard grass and the amaranthus retroflexus is compared, and the results are shown in the following comparison with a blank control group treated by distilled water and a control group treated by a glyphosate single-agent solution with the mass percentage concentration of 10 percent: after the treatment of the glyphosate compound aqueous solution with the glyphosate mass percentage concentration of 3.7%, the root length of barnyard grass is 2.0cm, the stem length is 6.0cm, the root length of amaranthus retroflexus is 3.5cm, and the stem length is 5.0 cm.
The glyphosate compound aqueous solution of the invention has the following performance indexes:
the above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (5)
1. A glyphosate compound aqueous solution is characterized in that: the main active ingredients are as follows: glyphosate, walnut leaf water extract, vinca alkaloid; the compound water agent comprises the following raw materials in parts by weight: 15-20 g of glyphosate, 5-8 g of walnut leaf water extract, 4-6 g of vinca alkaloid, 1-2 g of solubilizer, 0.5-1 g of stabilizer and 500-600 mL of water; the mass percentage of the glyphosate in the glyphosate compound aqueous solution is 2.0-4.0%;
the walnut leaf water extract is prepared by the following steps: drying and crushing walnut leaves, adding water, soaking for 0.5-1.5 hours at normal temperature, wherein the material-liquid ratio of the walnut leaves to the water is 1g: 25-30 ml, filtering, extracting the filtrate for 3 times by using an extracting agent, combining organic phases, and performing desolventizing to obtain a walnut leaf water extract, namely a flavonoid compound; wherein the extractant is anhydrous ether, ethyl acetate or chloroform;
the vinca alkaloid is prepared according to the following steps:
s1, placing the catharanthus roseus in an oven at 80-90 ℃ for drying for 2-3 h, crushing, extracting with ethanol with the mass percentage concentration of 70-95% at normal temperature, wherein the material-liquid ratio of the catharanthus roseus to the ethanol is 1g: 10-15 ml, the extraction time is 20-25 h, sequentially filtering with gauze and filter paper, and respectively collecting filtrate and filter residues;
s2, performing ultrasonic assisted extraction on the filter residue obtained in the step S1 for 20-30 min at the temperature of 60-80 ℃ by using 20-30% by mass of ethanol again, wherein the power of ultrasonic is 300-500W, the material-liquid ratio of the filter residue to the ethanol is 1g: 5-7 ml, filtering, collecting filtrate, and combining the filtrate and the filtrate obtained in the step S1 to obtain two extracting solutions; concentrating the extractive solution under reduced pressure with rotary evaporator to obtain ethanol extract;
s3, slowly pouring the ethanol extract obtained in the step S2 into macroporous resin for adsorption treatment, and eluting with n-hexane or petroleum ether until the eluent is colorless and transparent; eluting the macroporous resin with eluent, collecting the eluent, detecting by TLC method, and stopping collecting until no alkaloid is detected; concentrating and desolventizing to obtain Catharanthus roseus alkaloid; wherein the model of the macroporous resin is AB-8, D101, D201, D301 or HPD 100; the eluent is a mixed solution of a first solvent and a second solvent in a volume ratio of 1: 3-5, wherein the first solvent is ethanol, methanol or acetone, and the second solvent is n-hexane or petroleum ether.
2. The glyphosate complex water aqua of claim 1 is characterized in that: the solubilizer is one of beta-cyclodextrin, gamma-cyclodextrin, 2-hydroxyethyl-beta-cyclodextrin, 2-hydroxypropyl-beta-cyclodextrin and 2, 6-dimethyl-beta-cyclodextrin.
3. The glyphosate compound aqueous solution agent of claim 1, which is characterized in that: the stabilizer is one of trimethyl phosphite, glycol and epichlorohydrin.
4. A preparation method of the glyphosate complex water agent as claimed in any one of claims 1 to 3, which is characterized by comprising the following steps: the method comprises the following steps: putting the glyphosate, the walnut leaf water extract, the vinca alkaloid, the solubilizer and the stabilizer into water according to the proportion, and stirring at a high speed of 500-800 r/min for 20-30 min at normal temperature to uniformly mix the materials to obtain the glyphosate compound aqueous solution.
5. The application of the glyphosate compound aqueous solution as defined in any one of claims 1 to 3 as a herbicide.
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