CN111449077B - Metiram compound bactericide and application thereof - Google Patents

Metiram compound bactericide and application thereof Download PDF

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CN111449077B
CN111449077B CN202010471727.3A CN202010471727A CN111449077B CN 111449077 B CN111449077 B CN 111449077B CN 202010471727 A CN202010471727 A CN 202010471727A CN 111449077 B CN111449077 B CN 111449077B
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metiram
berberine
compound bactericide
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CN111449077A (en
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葛喜珍
刘金蓉
田平芳
李映
孔超杰
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Beijing Union University
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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
    • A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
    • A01N47/08—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having one or more single bonds to nitrogen atoms
    • A01N47/10—Carbamic acid derivatives, i.e. containing the group —O—CO—N<; Thio analogues thereof
    • A01N47/12—Carbamic acid derivatives, i.e. containing the group —O—CO—N<; Thio analogues thereof containing a —O—CO—N< group, or a thio analogue thereof, neither directly attached to a ring nor the nitrogen atom being a member of a heterocyclic ring
    • A01N47/14—Di-thio analogues thereof
    • 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
    • A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/90—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having two or more relevant hetero rings, condensed among themselves or with a common carbocyclic ring system

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Abstract

The invention discloses a metiram compound bactericide and application thereof. The compound bactericide comprises metiram and berberine, and the balance of auxiliary agents; wherein, the content of the metiram is 50 to 70 percent by weight percent, and the weight ratio of the metiram to the berberine is 24 to 99: 1. The compound bactericide is used for preventing and treating crop fungal diseases, in particular brown rot of peach. The compound bactericide of the invention takes metiram as a main component, and berberine is added as a synergist, so that the control effect of the metiram can be obviously improved, and pathogenic bacteria are not easy to generate drug resistance to the compound bactericide. The compound bactericide can effectively prevent and treat the ring spot of the apple, and the prevention effect is improved by more than 18 percent.

Description

Metiram compound bactericide and application thereof
Technical Field
The invention relates to a metiram compound bactericide and application thereof, belonging to the field of agriculture and chemical industry.
Background
The wide application of chemical pesticide plays a great role in ensuring the high and stable yield of crops. However, the 3R problem caused by long-term large-scale unreasonable use of traditional chemical pesticides, namely, the residue, resistance and rampant are getting worse and worse, which causes general social attention. The need to find and develop new pesticides that are safe to human health and ecological environment is more and more urgent. From 2015, the Ministry of agriculture formally starts the action of reducing weight and reducing pesticide to make the utilization rate of pesticide reach more than 40%, so as to realize zero increase of the use amount of chemical fertilizer and pesticide of crops. The reduction of the using amount of the pesticide and the improvement of the control effect are one of the effective methods for solving the zero growth of the pesticide.
Apple ring rot damages apple branches and fruits, and the bactericidal active substances are searched from traditional Chinese medicines to reduce the usage amount of chemical pesticides, so that the method is an important way and a research hotspot for creating novel bactericides. Particularly, after the scientific compounding of various components, the bactericidal activity of the pesticide is obviously improved.
Metiram, alias: ethylene dithiocarbamate (including zinc Fucozeb, mancozeb, zinc ethylphenyl dithiocarbamate, copper (II) bis (2-hydroxyethyl) dithiocarbamate, lead diethyldithiocarbamate and the like) is an excellent protective bactericide, and belongs to low-toxicity pesticides. Because the bactericide has wide sterilization range and is not easy to generate resistance, the prevention and treatment effect is obviously superior to that of other similar bactericides, and the bactericide is a large-tonnage product all the time internationally. Most of the domestic compound bactericides are prepared by processing mancozeb and the like, but the long-term use of a large amount of the mancozeb preparation can cause the accumulation of trace elements of crops and cause poisoning. The effective measure for solving the manganese-zinc poisoning is to reduce the using amount of the metiram and improve the control effect.
Berberine is quaternary amine isoquinoline alkaloid mainly contained in Coptidis rhizoma, Phellodendri cortex of Rutaceae, and Berberis of berberidaceae. Researches prove that the berberine has better control effect on a plurality of diseases such as apple ring spot, peach brown rot, powdery mildew, gray mold, downy mildew and the like; indoor bioassay and field pesticide effect measurement results show that berberine has good control effects on powdery mildew, angular leaf spot, leaf mold, ring spot, phytophthora root rot, and the like.
Some literature compounded with metiram is known at present, for example, patent literature CN110839647A discloses a bactericidal composition containing pyraclostrobin and metiram and a preparation method thereof, wherein the pyraclostrobin and the metiram are compounded; patent document CN109601544A discloses a pesticide composition containing metiram and trifloxystrobin and its application, and these patent documents describe most combinations of several chemical pesticides. Patent document CN108174859A discloses a metiram-containing bactericidal composition, which is a combination of metiram, kasugamycin and tetraconazole. The applicant does not find the literature and application that the plant source active ingredients can increase the metiram control effect.
The patent documents of berberine as agricultural fungicide mainly include: patent document CN103975962A discloses a wettable powder for preventing and treating fruit and vegetable brown rot and aphid and a preparation method thereof, wherein the effective components of the wettable powder are szechwan chinaberry fruit extract and berberine; patent document CN103814916A discloses berberine pesticide and its preparation method, the formulation comprises berberine and matrine; patent document CN103548849A discloses a synergistic botanical fungicide consisting of eugenol and berberine; patent document CN103503919A discloses a high adhesion jujube fruit shrink disease emulsion comprising active ingredients (streptomycin, instant boron, berberine), adhesive (chitosan, sodium carboxymethylcellulose CMC-NA-glycerol) and emulsifier (tween 80); patent document CN103444729A discloses a bactericidal pharmaceutical composition and its application, the bactericidal pharmaceutical composition includes two active ingredients: berberine and amino-oligosaccharins; patent document CN102940000A discloses botanical broad-spectrum bactericide comprising berberine, astragalus polysaccharides, radix tetrastigme extract, aloe extract, and fructus Gleditsiae Abnormalis; patent document CN102894002A discloses a compound bactericide consisting of berberine and polyoxin; the compound algistat disclosed in patent document CN102771484A mainly contains berberine and artemisinin; patent document CN102119703A discloses a botanical fungicide composed of rhubarb, rosin, aloe, berberine, Chinese honeylocust fruit and chinaberry root; two effective components of the botanical fungicide disclosed in patent document CN101961019A are berberine and osthole; the raw materials of berberine botanical insecticide disclosed in patent document CN101940229A relate to barberry root, phellodendron bark, perilla, castor bean; the active ingredients of the microemulsion for killing Monilinia fructicola disclosed in patent document CN101695301A are berberine and salicylic acid; patent document CN101574083A discloses sustained-release microcapsules and composite membranes for inhibiting monilinia fructicola, which mainly comprise chitosan and berberine. The patent document CN 104488923B discloses a botanical synergistic compound bactericide which uses berberine and physcion as main components. The research of the berberine used as the synergist for improving the drug effect of the metiram has not been reported.
In conclusion, patents, documents and products related to improvement of control of crop diseases and insect pests by metiram by berberine are not reported in a public way.
Based on the technology, the method is characterized in that the method comprises the following steps of' 2019 Hubei province major scientific and technological project-major scientific and technological achievement conversion project-project number: 19026517Z and funding "2018 university of Beijing Union university talent reinforced optimization plan" to complete the invention.
Disclosure of Invention
The invention aims to provide a metiram compound bactericide, which is added with a synergist, can obviously improve the metiram control effect, has protection and treatment effects, and can effectively prevent and treat apple ring spot.
The invention also aims to provide application of the metiram compound bactericide in preventing and treating apple ring rot.
In order to achieve the purpose, the invention adopts the following technical scheme:
a metiram compound bactericide, which comprises metiram and berberine, and the balance of auxiliary agents; wherein, the content of the metiram is 50 to 70 percent by weight percent, and the weight ratio of the metiram to the berberine is 24 to 99: 1.
The compound bactericide is in the form of liquid or solid, and can be soluble liquid, aqueous solution, missible oil, suspending agent or wettable powder.
As a soluble liquid agent, the auxiliary agent comprises: surfactant, emulsifier and organic solvent, wherein the soluble liquid contains 5-15 wt% of surfactant and 5-20 wt% of emulsifier. The surfactant and emulsifier are respectively selected from one or more of alkyl benzene sulfonate, alkylphenol polyoxyethylene ether, phenethyl phenol polyoxyethylene ether polyoxypropylene ether, castor oil and ethylene oxide adduct or aralkyl phenol polyoxyethylene ether formaldehyde condensate.
The production method of the soluble liquid agent comprises the following steps: weighing the raw materials according to a formula, sequentially adding the raw materials into the reaction kettle, mixing the raw materials, stirring the mixture in the reaction kettle to be transparent, and carrying out quality inspection to obtain a finished product.
As wettable powder, the auxiliary agent comprises: a carrier and a dispersant. The carrier is one or more of bentonite, activated clay, kaolin or attapulgite clay; the dispersant is one or more of Poloxamer188, glyceryl monostearate (Gelucire), sodium dodecyl benzene sulfonate and calcium dodecyl benzene sulfonate.
The production method of the wettable powder comprises the following steps: weighing raw materials according to a formula, sequentially adding and mixing, crushing in an ultrafine crusher, sieving by a 200-mesh sieve, and performing quality inspection to obtain a finished product.
An application of the metiram compound bactericide in preventing and treating apple ring rot.
The invention has the advantages that:
the compound bactericide of the invention takes metiram as a main component, and berberine is added as a synergist, so that the control effect of the metiram can be obviously improved, the compound bactericide has both protection and treatment effects, and can effectively prevent and treat apple ring spot.
1. The berberine is a natural active substance, is easy to degrade in the environment, has low toxicity to mammals such as human and livestock, is safe to natural enemies of pests and other beneficial organisms, and is not easy to generate drug resistance by pathogenic bacteria. The berberine serving as a synergist enhances the control effect of the berberine in cooperation with metiram by enhancing or inducing plant immunity.
2. The content of metiram in the compound bactericide is 50-70%, and the metiram and berberine (W/W) are 24-99: 1, so that the metiram control effect can be improved by more than 18%, and the dosage of zinc and manganese can be reduced by the same control effect.
3. The invention utilizes berberine which has antibacterial and immunoregulatory effects to play a role in health care of crops, so that the crops grow strongly and diseases are obviously reduced.
Drawings
FIG. 1 is a graph showing the inhibitory effect of metiram apple and berberine on physalospora piricola.
FIG. 2 is a graph showing the effect of berberine and metiram in synergistically inhibiting Physalospora malorum.
Detailed Description
The invention is further illustrated by the following examples and figures. The invention will be better understood from the following examples. However, those skilled in the art will readily appreciate that the specific material ratios, process conditions and results thereof described in the examples are illustrative only and should not be taken as limiting the invention as detailed in the claims.
Toxicity determination of metiram and berberine on apple ring spot
Apple ring rot (Botryosphaeria dothidea) is a gift given by professor of Pingfang in Beijing chemical industry and university fields. 98% berberine (BBR) is purchased from Shaanxi Huiyike biological development Co., Ltd. 70% metiram water dispersible granules from basf plant protection (Jiangsu) GmbH.
Selecting apple ring rot fungus growing on solid PDA culture medium for 5 days, punching bacterial cake on bacterial colony surface with hole puncher with diameter of 8mm, inoculating hypha downwards onto the PDA culture medium, culturing at 28 deg.C in constant temperature incubator for 48 hr, and culturing every 24 hrMeasuring the diameter of the inhibition zone by a cross method, calculating the inhibition rate, converting the inhibition rate into a rate value according to an inhibition rate value conversion table, drawing a standard curve by taking the logarithm of the concentration of the medicament as the abscissa and the rate value as the ordinate to obtain a toxicity regression equation and a related coefficient, and calculating the half-maximum Effect Concentration (EC) according to the toxicity regression equation50)。
The inhibition effect of berberine and metiram on physalospora piricola is respectively examined according to the method. PDA medium without agent was used as a blank (CK) control, with three replicates per agent concentration setting. The inhibition of the hypha growth of ring rot apple at 60h by various agents is shown in the following tables 1-2. The visual observation condition is shown in figure 1, wherein A shows the inhibition effect of berberine on the growth of the hyphae of the ring rot apple bacteria, and B shows the inhibition effect of metiram on the growth of the hyphae of the ring rot apple bacteria. Taking the logarithm of the concentration of the medicament as an abscissa and the rate of inhibition probability as an ordinate, drawing a standard curve to obtain a toxicity regression equation and related coefficients, and calculating the toxicity (EC) of various medicaments on the apple ring rot pathogen according to the toxicity regression equation50Value, EC of berberine and metiram for inhibiting physalospora malorum50The values were 8.85. mu.g/mL and 5.45. mu.g/mL, respectively.
TABLE 1 Berberine inhibition of mycelial growth of apple ring rot (60h)
Figure GDA0002962866970000041
TABLE 2 inhibition of mycelial growth of apple ring rot by metiram (60h)
Figure GDA0002962866970000042
Synergistic effect of berberine on metiram inhibition
The co-toxicity factor method is the most common method for evaluating the compounding effect. The co-toxicity factor method firstly designs a series of ratios, and then calculates the co-toxicity factors under each ratio to evaluate the effect.
The co-virulence factor (CTF) was calculated according to formula 1.
∑＝(H1-H0)/H0The
In formula 1:
H0a theoretical inhibition rate of the compound agent;
H1-actual inhibition rate of the combination;
sigma-co-virulence factors.
If the sigma is more than 20, the two single agents are compounded to generate a synergistic effect;
if sigma is less than-20, the two single agents are compounded to generate antagonism;
if-20 < ∑ < 20, it means that the two single agents combine to produce an additive effect.
According to a co-toxicity factor method, the adding amount of metiram is a, the adding amount of berberine is b, the dosing culture medium is prepared according to the compounding ratio of 199: 1, 149: 1, 99: 1, 97: 3 and 96: 4 of a: b respectively, a PDA culture medium without medicament is used as a blank control, three parallel cells are arranged in each compounding ratio, then apple ring rot bacteria which is picked up by a puncher with the diameter of 8mm is inoculated to the center of the culture medium in a mode that hyphae face down, after 48 hours of culture at 28 ℃, the diameter of a bacteriostasis ring is measured by a cross method every 24 hours, the inhibition situation of the berberine and metiram compounding on the growth of the apple ring rot bacteria at 60 hours is shown in the following table 3, and the visual observation situation is shown in the figure 2.
TABLE 3 inhibition of mycelial growth of ring rot apple by berberine and metiram combination (60h)
Figure GDA0002962866970000051
And calculating the actual inhibition rate of the compound agent, calculating the theoretical inhibition rate of the compound agent according to a toxicity regression equation, calculating the co-toxicity factor according to the formula 1, and evaluating the antibacterial effect of the compound agent.
The interaction between the single agents is different, so that the compound agent has additive, antagonistic or synergistic effect on pathogenic bacteria, and the synergistic effect of the berberine on metiram is shown in figure 2. In the figure, in order from left to right: 1: CK; 2: a to b is 199 to 1, and antagonism is generated; 3: a: b 149: 1, antagonism is produced, 4: a to b is 99 to 1, and additive effect is generated; 5: a, b is 97: 3, so that additive effect is generated; 6: the ratio of a to b is 96: 4, and the result of the data is shown in the table 4.
TABLE 4 evaluation of the efficacy of berberine and metiram combination on Phyllostachys malorum
Compounding ratio H0(％) H1(％) ∑ Effect
199∶1 48.5 32.2 -33.6 Antagonism of
149∶1 51.8 21.7 -58.1 Antagonism of
99∶1 54.6 48.6 -11.0 Adding
97∶3 54.6 58.6 7.3 Adding
96∶4 51.4 63.3 23.2 Synergistic effect
Example 1
At room temperature, 50 parts of metiram and 1 part of berberine are taken, 10 parts of sodium dodecyl benzene sulfonate (dispersant) is added, and 100 parts of bentonite is used for supplementing. Crushing in a superfine crusher, and sieving with a 200-mesh sieve to obtain 50% wettable metiram powder.
Example 2
At room temperature, 57 parts of metiram and 3 parts of berberine are taken, 10 parts of calcium dodecyl benzene sulfonate (dispersant) is added, and 100 parts of activated clay is used for supplementing. Crushing in a superfine crusher, and sieving with a 200-mesh sieve to obtain 57% wettable metiram powder.
Comparative example 1
At room temperature, 50 parts of metiram is taken, no berberine is added, 10 parts of sodium dodecyl benzene sulfonate (dispersing agent) is added, and 100 parts of bentonite is used for supplementing. Crushing in a superfine crusher, and sieving with a 200-mesh sieve to obtain 50% wettable metiram powder.
Example 3
At room temperature, 49 parts by weight of metiram is taken, 0.5 part of berberine is added, 10 parts of sodium dodecyl benzene sulfonate and 10 parts of phenethyl phenol polyoxyethylene ether are sequentially added. Make up to 100 parts with dimethylformamide. Stirring the mixture in a reaction kettle at the stirring speed of 200 revolutions per minute for 70 minutes, and stirring the mixture for transparency to obtain 49 percent of metiram soluble liquid.
Example 4
At room temperature, 60 parts of metiram is taken according to parts by weight, 6 parts of berberine are added, 10 parts of calcium dodecylbenzene sulfonate and 8 parts of castor oil are sequentially added. Make up to 100 parts with dimethylformamide. Stirring the mixture in a reaction kettle at the stirring speed of 200 revolutions per minute for 70 minutes, and stirring the mixture for transparency to obtain the 60 percent metiram soluble liquid.
Comparative example 2
At room temperature, according to the parts by weight, 50 parts of metiram are taken, no berberine is added, 10 parts of sodium dodecyl benzene sulfonate and 10 parts of phenethyl phenol polyoxyethylene ether are sequentially added. Make up to 100 parts with dimethylformamide. Stirring the mixture in a reaction kettle at the stirring speed of 200 revolutions per minute for 70 minutes, and stirring the mixture for transparency to obtain 50 percent of metiram soluble liquid.
Comparative example 3
At room temperature, 20 parts of berberine are taken according to the parts by weight, 10 parts of sodium dodecyl benzene sulfonate (dispersant) are added, and 100 parts of bentonite is used for supplementing. Pulverizing in a superfine pulverizer, and sieving with 200 mesh sieve to obtain 20% berberine wettable powder.
Field efficacy test of synergistic sterilization on apple ring spot
In order to clarify the field efficacy situation of the embodiment of the invention, the field plot efficacy test of apple ring spot on the embodiment medicament was carried out in the Beijing cisterm area in 2017. The cell test is randomly arranged, repeated for 3 times, 5 plants per cell, and adopts a conventional spraying method, the dosage of the test agent is 90mg a.i./L, the test agent is sprayed for 7 times, and clear water blank control is set. And (3) surveying when the apples are collected, wherein one branch is taken from each of the south, the west and the north of the fruit trees, 420 and 450 fruits are surveyed, the number of the fruits which are developed and healthy is recorded, and the occurrence condition of apple ring spot is calculated.
Disease fruit rate (%) (number of investigated disease fruits/total number of investigated fruits) × 100
Control effect (%) [ (blank control area fruit disease rate-treatment area fruit disease rate)/blank control area fruit disease rate ] × 100
Test results and statistics: the field control of apple ring spot was tested for the above examples and comparative examples and the results are shown in table 5.
TABLE 5 prevention and treatment of apple ring rot in different examples
Treatment of Number of surveys (one) Number of diseased fruits The rate of fruit diseases% Control effect (%)
CK (Water) 425 86 20.24 -
Example 1 436 12 2.75 86.40
Example 2 447 14 3.13 84.53
Comparative example 1 443 30 6.77 66.54
Example 3 439 8 1.82 91.00
Example 4 444 12 2.70 86.65
Comparative example 2 448 31 6.92 65.81
Comparative example 3 431 35 8.12 59.88
As can be seen from Table 5, the bactericide compounded by metiram and berberine serving as a synergist (examples 1, 2, 3 and 4) prepared by the invention has the control effect on apple ring spot of 84.53-91.00%, and has a remarkably different control effect compared with 65.81-66.54% of a control medicament (comparative examples 1 and 2 without berberine serving as a synergist) and 59.88% of the control effect with berberine only (comparative example 3). The same control effect of the metiram can be achieved, and the dosage of zinc and manganese can be reduced. In addition, berberine is taken as an effective component in Chinese medicaments of coptis and phellodendron, is natural and is easy to degrade in the environment. The use of the trace berberine can greatly improve the control effect of metiram, reduce the cost and is friendly to non-target organisms and environment.

Claims (6)

1. A metiram compound bactericide is characterized in that the compound bactericide comprises metiram and berberine, and the balance of auxiliary agents; wherein, the content of the metiram is 50 to 70 percent by weight percent, and the weight ratio of the metiram to the berberine is 24: 1.
2. The metiram compound bactericide as claimed in claim 1, wherein the form of the compound bactericide is liquid or solid.
3. The metiram compound bactericide as claimed in claim 2, wherein the formulation of the compound bactericide is soluble liquid, aqueous solution, emulsifiable concentrate, suspending agent or wettable powder.
4. The metiram compound bactericide as claimed in claim 3, wherein the formulation of the compound bactericide is wettable powder, and the auxiliary agent comprises: a carrier and a dispersant.
5. The metiram compound bactericide as claimed in claim 4, wherein the carrier is one or more of bentonite, activated clay, kaolin or attapulgite clay; the dispersant is one or more of Poloxamer188, glyceryl monostearate, sodium dodecyl benzene sulfonate and calcium dodecyl benzene sulfonate.
6. The application of the metiram compound bactericide of any one of claims 1 to 5, which is used for preventing and treating apple ring spot.
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CN108633891A (en) * 2018-04-10 2018-10-12 合肥红佳科技信息有限公司 A kind of bactericidal composition containing jamaicin and Boscalid
CN110547298A (en) * 2018-06-04 2019-12-10 中国农业大学 Application of berberine as bactericidal synergist in prevention and treatment of plant gray mold

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108633891A (en) * 2018-04-10 2018-10-12 合肥红佳科技信息有限公司 A kind of bactericidal composition containing jamaicin and Boscalid
CN110547298A (en) * 2018-06-04 2019-12-10 中国农业大学 Application of berberine as bactericidal synergist in prevention and treatment of plant gray mold

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