CN106973990B - fumigation method for preventing and controlling entomophthora in grains - Google Patents

fumigation method for preventing and controlling entomophthora in grains Download PDF

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CN106973990B
CN106973990B CN201610033963.0A CN201610033963A CN106973990B CN 106973990 B CN106973990 B CN 106973990B CN 201610033963 A CN201610033963 A CN 201610033963A CN 106973990 B CN106973990 B CN 106973990B
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fumigant
fumigation
radical
grain
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CN106973990A (en
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姜标
张琛
陶黎明
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Shanghai Institute of Organic Chemistry of CAS
East China University of Science and Technology
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Shanghai Institute of Organic Chemistry of CAS
East China University of Science and Technology
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    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23BPRESERVING, e.g. BY CANNING, MEAT, FISH, EGGS, FRUIT, VEGETABLES, EDIBLE SEEDS; CHEMICAL RIPENING OF FRUIT OR VEGETABLES; THE PRESERVED, RIPENED, OR CANNED PRODUCTS
    • A23B9/00Preservation of edible seeds, e.g. cereals
    • A23B9/16Preserving with chemicals
    • A23B9/18Preserving with chemicals in the form of gases, e.g. fumigation; Compositions or apparatus therefor
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C309/00Sulfonic acids; Halides, esters, or anhydrides thereof
    • C07C309/78Halides of sulfonic acids
    • C07C309/79Halides of sulfonic acids having halosulfonyl groups bound to acyclic carbon atoms
    • C07C309/84Halides of sulfonic acids having halosulfonyl groups bound to acyclic carbon atoms of a carbon skeleton substituted by carboxyl groups
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23VINDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2200/00Function of food ingredients
    • A23V2200/10Preserving against microbes
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23VINDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2300/00Processes
    • A23V2300/30Ion-exchange

Abstract

The invention discloses a fumigation method for preventing and treating entomophthora of grains, which comprises the following steps of placing fumigant below or/and around a grain stack in an environment of room temperature to 40 ℃, wherein the fumigant is a compound with a chemical structure shown in a general formula I: or a general formula II:

Description

Fumigation method for preventing and controlling entomophthora in grains
Technical Field
The invention relates to a fumigation method for preventing and controlling entomophthora in grains, and belongs to the technical field of grain preservation.
Background
At present, the annual grain loss and waste amount of China is about 1000 million jin, which is about equivalent to the grain yield of one year in the first major grain-producing province of China, namely Heilongjiang province. According to measurement and calculation, the total loss and waste amount of the grains in circulation links such as storage, transportation, processing and the like in postpartum of China reaches about 700 jin, wherein the loss of the grain storage link in the circulation link is about 400 jin. The loss of food mildewed every year in China varies considerably, and the pollution of fungi and toxins seriously threatens the food safety in China. According to the introduction of Liuyang by researchers of agricultural product processing institute of Chinese academy of agricultural sciences: "China invests billions of yuan in full force every year to strive for 1% of grain yield increase, but the grain postpartum loss caused by mildew every year is up to 2100 million tons, which accounts for 4.2% of the total grain yield in China, and the direct economic loss caused is about 180 hundred million to 240 million yuan. "
In addition, mycotoxin pollution also severely restricts foreign trade in China. In recent years, safety events caused by food polluted by mycotoxin frequently occur, so that the health of people and livestock in China is seriously threatened, and the outward trade of agricultural products in China is also restricted. After the illegal event of the edible agricultural products exported from the European Union in the last 10 years of 2002-2011 is statistically analyzed, the following findings are found: among the factors restricting foreign trade in China, such as heavy metal, pesticide and veterinary drug residue, the overproof mycotoxin is the most main reason, and the illegal events caused by the mycotoxin reach 28.6%. It is understood that mycotoxins are the most dangerous food pollutants occurring in nature, whereas aflatoxins, which are 10 times as toxic as potassium cyanide and 68 times as toxic as arsenic, are one of the most prominent causes of liver cancer. The mycotoxin is mainly generated in the process of grain storage after production, and in the process of grain storage in China, the mould mainly comprises aspergillus flavus, fusarium asia and fusarium graminearum; in European and American countries, besides Aspergillus flavus and Fusarium graminearum, there are also Aspergillus parasiticus and Fusarium flavum. Meanwhile, compared with the characteristics of short storage period, single source, small quantity and the like of grain storage in Europe and America, the grain storage in China is mainly characterized by high bacteria carrying capacity, long storage period, wide source, various varieties, impurity and large quantity. In addition, the grains lost due to insect damage in the granary and the transportation process are not small and varied, and after the grains are eaten by the insect damage, the broken grains are increased, and the germination rate of the seeds is reduced; in addition, the pests can block the grains when spinning. The odor liquid secreted by the insect feces, the insect corpses and some pests pollutes the grains and even generates toxin, so that the grains are heated and mildewed. Common pests in the granary include weevils, silverbeetles, clothianworms, clothianthes, wheat moths, tobacco beetles, cockroaches, and Indian meal moth, among others. At present, most grain depots adopt modes such as grain surface pesticide application, bag burying, pipe probing fumigation and insect killing, the used fumigants mainly comprise phosphine, ethylene oxide, methyl bromide and sulfuryl fluoride, and along with the improvement of environmental protection and safety consciousness of people, the limitations of the fumigants are gradually reflected, such as: phosphine is strongly toxic, damages lung, heart, liver, kidney, central nervous system and skeleton, causes asthma, pneumonia or pulmonary fibrosis diseases due to over exposure, and is easy to burn by itself; the denaturing and explosive nature of ethylene oxide; the destructive nature of methyl bromide to atmospheric stratospheric ozone and the direct generation of toxic effects on humans have attracted a great deal of attention. Since the ninth Montreal protocol of 1997 was the meeting of contracting countries, developed countries have agreed to stop using methyl bromide disinfectant gradually from 2005, and China officially signed the Montreal protocol of Copenhagen amendment in 4 months of 2003, and agreed to stop using methyl bromide in agriculture, storage, tobacco and other industries before 1 day of 1 month of 2015. Of course, this promise will also be implemented in food sterilization; sulfuryl fluoride is colorless, toxic and strong irritant gas at normal temperature and pressure, and acute toxicity mainly damages the central nervous system to cause convulsion; in addition, it is deposited in human bone and has accumulated poisoning risk. The latest research finds that the chemical fumigant sulfuryl fluoride becomes a strong greenhouse gas after being emitted into the air, and the effect of one kilogram of sulfuryl fluoride discharged into the atmosphere on global warming is 4800 times that of one kilogram of carbon dioxide; although sulfuryl fluoride is present in air in very small quantities, about 1.5 ppm, i.e., only 1.5 sulfuryl fluoride per million air molecules, it is increasing at a rate of 5% per year, and the atmospheric greenhouse effect caused by the use of sulfuryl fluoride as a substitute for methyl bromide will be a sufficient value!
In conclusion, solving the problem of food mildew becomes a great demand for guaranteeing national food safety, and exploring an effective prevention and control method suitable for the insect mildew in food storage in China becomes a research subject which is urgently needed to be solved at present.
Disclosure of Invention
Aiming at the problems and the requirements in the prior art, the invention aims to provide a green, environment-friendly, safe and effective fumigation method for preventing and controlling insect and mold of grains.
In order to achieve the purpose, the invention adopts the following technical scheme:
Fumigation for preventing and treating entomophthora in grainsThe steaming method comprises the following operations: placing the fumigant below or/and around the grain heap at room temperature to 40 ℃; the fumigant is of the general formula I:Or formula II:A compound of the chemical structure shown, wherein, in the general formula I: x is halogen or hydroxy; y is1And Y2Each is independently selected from H or F; r1Is R3substituted C1-C10Alkyl radical, R3Substituted C2-C10Alkylene radical, R3Substituted phenyl, R3Substituted benzyl, R3Substituted C3-C8Cycloalkyl radical, R3Substituted C3-C8Cycloalkenyl radical or R3Substituted adamantyl; the R is3Selected from hydrogen, hydroxy, halogen, C1-C3Alkyl radical, C2-C3At least one of alkylene groups; in the general formula II: x is halogen or hydroxy; r2is R4Substituted C1-C4Alkyl radical, R4Substituted C2-C4alkylene radical, R4Substituted phenyl, R4Substituted benzyl, R4Substituted C3-C8Cycloalkyl radical, R4substituted C3-C8Cycloalkenyl radical or R4Substituted adamantyl; the R is4Selected from hydrogen, hydroxy, halogen, C1-C3Alkyl radical, C2-C3At least one olefin group.
Preferably, in the formula I: x is F, Cl, Br or OH; y is1And Y2simultaneously being F or Y1、Y2One of them is F; r1Is R3Substituted C1-C10Alkyl radical, R3Substituted C2-C10Alkylene radical, R3Substituted phenyl, R3Substituted benzyl, R3substituted C3-C6Cycloalkyl radical, R3Substituted C3-C6Cycloalkenyl radical or R3Substituted adamantyl; the R is3At least one selected from hydrogen, hydroxyl, fluorine, chlorine, bromine, methyl, ethyl, isopropyl and allyl.
As a further preferable embodiment, in the general formula I: x is F or Cl; y is1And Y2And is simultaneously F; r1Is R3Substituted C1-C4Alkyl radical, R3Substituted C2-C4Alkylene radical, R3Substituted phenyl or R3Substituted C3-C6a cycloalkyl group; the R is3At least one selected from hydrogen, hydroxyl, fluorine and chlorine.
As a still further preferred embodiment, in said general formula I: x is F; y is1And Y2And is simultaneously F; r1Is C1-C4Alkyl radical, C2-C4Alkylene, phenyl or C3-C7Cycloalkyl (i.e.: R)3Is hydrogen).
Preferably, in the formula II: x is F, Cl, Br or OH; r2Is R4Substituted C1-C4Alkyl radical, R4Substituted C2-C4alkylene radical, R4Substituted phenyl, R4Substituted benzyl, R4Substituted C3-C7Cycloalkyl radical, R4substituted C3-C7Cycloalkenyl radical or R4Substituted adamantyl; the R is4at least one selected from hydrogen, hydroxyl, fluorine, chlorine, bromine, methyl, ethyl, isopropyl and allyl.
As a further preferable mode, in the general formula II: x is F or Cl; r2Is R4Substituted C1-C4Alkyl radical, R4Substituted C2-C4Alkylene radical, R4Substituted C3-C7cycloalkyl or R4Substituted phenyl; the R is4At least one selected from hydrogen, hydroxyl, fluorine and chlorine.
As a still further preferred embodiment, the above-mentionedIn formula II: x is F; r2Is C1-C4Alkyl radical, C2-C4Alkenyl or phenyl (i.e. R)4Is hydrogen).
In particular, fumigants of the present invention include, but are not limited to, compounds having the following chemical structure:
(abbreviated as fumigant 1),(abbreviated as fumigant 2),(abbreviated as fumigant 3),(abbreviated as fumigant 4),(abbreviated as fumigant 5),(abbreviated as fumigant 6),(abbreviated as fumigant 7),(abbreviated as fumigant 8),(abbreviated as fumigant 9),(referred to as fumigant 10),(abbreviated as fumigant 11),(abbreviated as fumigant 12),(abbreviated as fumigant 13),(abbreviated fumigant 14),(abbreviated as fumigant 15),(abbreviated fumigant 16),(abbreviated fumigant 17),(abbreviated fumigant 18),(abbreviated fumigant 19),(abbreviated as fumigant 20),(abbreviated as fumigant 21),(abbreviated fumigant 22),(abbreviated fumigant 23);
(simple)Recorded as fumigant 24),(abbreviated as fumigant 25),(abbreviated fumigant 26),(abbreviated fumigant 27),(abbreviated fumigant 28),(abbreviated fumigant 29),(abbreviated fumigant 30),(abbreviated as fumigant 31),(abbreviated fumigant 32),(abbreviated fumigant 33),(abbreviated fumigant 33),(abbreviated as fumigant 35),(abbreviated fumigant 36),(simple)Recorded as fumigant 37),(abbreviated fumigant 38),(abbreviated fumigant 39),(abbreviated as fumigant 40),(abbreviated fumigant 41),(abbreviated fumigant 42),(abbreviated fumigant 43),(abbreviated fumigant 44),(abbreviated as fumigant 45),(abbreviated fumigant 46),(abbreviated fumigant 47),(abbreviated fumigant 48),(abbreviated fumigant 49),(abbreviated fumigant 50),(abbreviated fumigant 51),(abbreviated fumigant 52),(abbreviated fumigant 53),(abbreviated as fumigant 54).
Preferably, the fumigant is placed under or/and around the grain bulk in a closed environment at room temperature.
Preferably, the fumigant is loaded on a carrier material having an adsorption effect, and the carrier material includes, but is not limited to, filter paper, silica gel, filter membrane, cotton, sponge, cloth, or the like.
preferably, the fumigant-loaded carrier material is placed in a hollow device having an outwardly diffusing mouth or mesh surface, including but not limited to a box-like structure, cage-like structure or bag, etc.
As a further preferable mode, the hollow device has a fan and a speed regulation function.
As a further preferable mode, the hollow device has self-heating and temperature-adjusting functions.
Compared with the prior art, the invention has the following beneficial effects:
According to the invention, the compound with the structure of the general formula I or II is selected as the fumigant, so that the safe and effective control of common entomomycete diseases of grains is realized, the pollution to the environment is minimum, the problem of fumigant residue is avoided, and the fumigant has the advantages of environmental friendliness; particularly, the invention can realize one-time treatment of entomophthora diseases of various grains and various grains in the same fumigation environment, and the grains treated by the fumigation method can be placed in a granary environment or a transportation condition for at least more than half a year without the entomophthora diseases; in addition, the method has the advantages of simple operation, low cost, wide range of applicable grain varieties and insect mold diseases and the like, and has important value and profound and far-reaching significance for safe and long-term preservation of grains.
Detailed Description
the technical solution of the present invention is further described in detail by examples below.
Example 1: preparation of fumigants
1. Preparation of fumigant 15(2, 2-difluoro-2- (sulfonyl fluoro) acetic acid cyclopropyl ester):
Adding dichloromethane (10mL) into cyclopropanol (58mg), dropwise adding perfluorosulfonate (1mL) under cooling of an ice-water bath, naturally heating to room temperature after dropwise adding, adding water to quench the reaction after the reaction is completed, extracting with dichloromethane (100mL multiplied by 2), washing with water (10mL multiplied by 2), washing with saturated salt water (10mL multiplied by 2), drying with anhydrous sodium sulfate, and evaporating the solvent under pressure to obtain a crude fumigant 15(2, 2-difluoro-2- (sulfonyl fluoride group) cyclopropyl acetate) with a molar yield of 90%;1HNMR(CDCl3)δ(ppm)2.70(m,1H),0.60(m,2H),0.35(m,2H).LR-ESI:[M+H]+218.99。
2. Preparation of fumigants 16, 17, 18, 19, 20, 21, 22, 23:
Referring to the preparation method of fumigant 15 in fig. 1, cyclobutanol, cyclopentanol, menthol, isopulegol, dihydrocarveol, carveol, citronellol, and citric alcohol were reacted with perfluorosulfonate respectively, so that corresponding fumigants were prepared:
1HNMR(CDCl3)δ(ppm)4.23(m,1H),2.30(m,2H),1.91-2.08(m,4H).LR-ESI:[M+H]+233.0;
1HNMR(CDCl3)δ(ppm)4.12(m,1H),1.92(m,2H),1.46-1.63(m,6H).LR-ESI:[M+H]+247.02;
1HNMR(CDCl3)δ(ppm)4.03(m,1H),1.85-1.98(m,2H),1.50-1.62(m,5H),1.20-1.29(m,2H),0.97(d,J=5.6Hz,3H),0.89(d,J=6.0Hz,6H).LR-ESI:[M+H]+317.10;
1HNMR(CDCl3)δ(ppm)5.10(s,1H),4.90(s,1H),4.04(m,1H),2.65(m,1H),1.90(s,3H),1.55-1.69(m,5H),1.25-1.35(m,2H),0.95(d,J=5.6Hz,3H).LR-ESI:[M]+314.08;
1HNMR(CDCl3)δ(ppm)5.11(s,1H),4.87(s,1H),4.08(m,1H),2.20(m,1H),2.10(m,1H),1.88(s,3H),1.56-1.72(m,4H),1.22-1.34(m,2H),0.94(d,J=5.6Hz,3H).LR-ESI:[M]+314.08;
1HNMR(CDCl3)δ(ppm)5.32(m,1H),5.15(s,1H),4.93(s,1H),4.32(m,1H),2.30(m,1H),1.75-1.90(m,4H),1.86(s,3H),1.82(s,3H).LR-ESI:[M+1]+313.06;
1HNMR(CDCl3)δ(ppm)5.22(s,1H),4.07(m,2H),2.01(m,2H),1.85(s,3H),1.73(s,3H),1.50-1.61(m,5H),0.98(d,J=6.0Hz,3H).LR-ESI:[M+1]+317.10;
1HNMR(CDCl3)δ(ppm)5.38(m,1H),5.22(m,1H),4.45(m,2H),2.10(m,2H),2.04(m,2H),1.90(s,3H),1.88(s,3H),1.80(s,3H).LR-ESI:[M+1]+315.08。
3. Preparation of the rest fumigants:
Since the rest fumigants are known compounds, the fumigants can be prepared according to respective disclosed preparation methods.
example 2: experiment of grain fumigation
Grain variety: corn, rice, wheat, soybean, broad bean, potato, sweet potato, etc
Disease: aspergillus, Penicillium, Trichoderma, Rhizopus cereus, Rhizopus, Trichoderma, Staphylococcus aureus, Escherichia coli, Bacillus megaterium, Bacillus subtilis, Pseudomonas fluorescens, etc
Fumigant: fumigant 24(CAS number: 677-25-8)
The fumigant is directly placed in a culture dish, and then the grain sample is placed above the culture dish (which can be realized by arranging a fixed frame), and is fumigated at room temperature.
Through sampling and monitoring, the following results are obtained: after 24 hours of fumigation, no mould grows on the grain sample after the fumigation treatment (detected by a microscope), and no fumigant residue exists on the grain sample after the fumigation treatment (detected and analyzed by a gas chromatography-mass spectrometer (GC-Ms)); in addition, the color of all the grain samples after the fumigation treatment is observed by a color difference meter without obvious change.
The grain sample treated by the fumigation in the embodiment is placed in a room temperature environment, and the mold and bacteria tracking detection is performed regularly, and the detection results are shown in the following table:
Storage time 0 month 1 month 3 months old 6 months old
growth of mold and bacteria No any mildew or fungus No any mildew or fungus No any mildew or fungus No any mildew or fungus
The invention can realize one-time treatment of various grains and various mildews and bacteria in the same fumigation environment.
Example 3: experiment of grain fumigation
Grain variety: corn, rice, wheat, soybean, broad bean, potato, sweet potato, etc
Disease: aspergillus, Penicillium, Trichoderma, Rhizopus cereus, Rhizopus, Trichoderma, Staphylococcus aureus, Escherichia coli, Bacillus megaterium, Bacillus subtilis, Pseudomonas fluorescens, etc
Fumigant: fumigant 25: (CAS number: 754-03-0)
Firstly, loading a fumigant on silica gel particles, then placing the silica gel particles in a bag with meshes on the surface, then placing the bag at the bottom of a glass jar, placing a grain sample above the bag (which can be realized by arranging a fixed frame in the glass jar), sealing the glass jar, and fumigating at room temperature.
Through sampling and monitoring, the following results are obtained: after the grains are fumigated for 36 hours, no mould grows on the fumigated grains (detected by a microscope), and no fumigant residue exists on the fumigated grains (detected and analyzed by a gas chromatography-mass spectrometer (GC-Ms)); in addition, the color of the grain sample after the fumigation treatment is observed by a color difference meter and is not obviously changed.
the grain sample treated by the fumigation in the embodiment is placed in a room temperature environment, and the mold and bacteria tracking detection is performed regularly, and the detection results are shown in the following table:
Storage time 0 month 1 month 3 months old 6 months old
Growth of mold and bacteria No any mildew or fungus No any mildew or fungus No any mildew or fungus No any mildew or fungus
The invention can realize one-time treatment of various grains and various mildews and bacteria in the same fumigation environment.
Example 4: experiment of grain fumigation
Grain variety: corn, rice, wheat, soybean, broad bean, potato, sweet potato, etc
Disease: aspergillus, Penicillium, Trichoderma, Rhizopus cereus, Rhizopus, Trichoderma, Staphylococcus aureus, Escherichia coli, Bacillus megaterium, Bacillus subtilis, Pseudomonas fluorescens, etc
Fumigant: fumigant 27(CAS number: 260417-57-0)
firstly, loading a fumigant on cyclodextrin, then placing the cyclodextrin in a bag with meshes on the surface, then placing the bag at the bottom of a glass jar, placing a grain sample above the bag (which can be realized by arranging a fixed frame in the glass jar), sealing the glass jar, and fumigating at room temperature.
Through sampling and monitoring, the following results are obtained: after 30 hours of fumigation, no mould grows on the grain sample after the fumigation treatment (detected by a microscope), and no fumigant residue exists on the grain sample after the fumigation treatment (detected and analyzed by a gas chromatography-mass spectrometer (GC-Ms)); in addition, the color of the grain sample after the fumigation treatment is observed by a color difference meter and is not obviously changed.
The grain sample treated by the fumigation in the embodiment is placed in a room temperature environment, and the mold and bacteria tracking detection is performed regularly, and the detection results are shown in the following table:
Storage time 0 month 1 month 3 months old 6 months old
Growth of mold and bacteria No any mildew or fungus No any mildew or fungus no any mildew or fungus No any mildew or fungus
The invention can realize one-time treatment of various grains and various mildews and bacteria in the same fumigation environment.
Example 5: experiment of grain fumigation
grain variety: corn, rice, wheat, soybean, broad bean, potato, sweet potato, etc
disease: aspergillus, Penicillium, Trichoderma, Rhizopus cereus, Rhizopus, Trichoderma, Staphylococcus aureus, Escherichia coli, Bacillus megaterium, Bacillus subtilis, Pseudomonas fluorescens, etc
Fumigant:
Fumigant 1(CAS number: 680-15-9);
Fumigant 10(CAS number: CAS: 309-21-7);
Firstly, loading fumigant 1 or 10 on filter paper, then placing the filter paper at the bottom of a glass jar, placing a grain sample above the filter paper, sealing the glass jar, and fumigating at room temperature.
Through sampling and monitoring, the following results are obtained: after 24 hours of fumigation, no mould grows on the grain sample fumigated by any fumigant (detected by a microscope), and no fumigant residue exists on the grain sample fumigated by any fumigant (detected and analyzed by a gas chromatography-mass spectrometer (GC-Ms)); in addition, the color of the grain sample fumigated by any one of the fumigants is not obviously changed through observation of a color difference meter.
The grain sample fumigated by any one of the fumigants in this embodiment is placed in a room temperature environment, and mould and fungus tracking detection is performed regularly, and the following detection results are obtained:
Storage time 0 month 1 month 3 months old 6 months old
Growth of mold and bacteria No any mildew or fungus no any mildew or fungus No any mildew or fungus No any mildew or fungus
The invention can realize one-time treatment of various grains and various mildews and bacteria in the same fumigation environment.
Example 6: experiment of grain fumigation
Grain variety: corn, rice, wheat, soybean, broad bean, potato, sweet potato, etc
disease: aspergillus, Penicillium, Trichoderma, Rhizopus cereus, Rhizopus, Trichoderma, Staphylococcus aureus, Escherichia coli, Bacillus megaterium, Bacillus subtilis, Pseudomonas fluorescens, etc
Fumigant: fumigant 9(CAS number: 113591-64-3)
Firstly, loading a fumigant on silica gel particles, then placing the silica gel particles in a bag with meshes on the surface, then placing the bag at the bottom of a glass jar, placing a grain sample above the bag (which can be realized by arranging a fixed frame in the glass jar), sealing the glass jar, and fumigating at the ambient temperature of 40 ℃.
Through sampling and monitoring, the following results are obtained: after 20 hours of fumigation, no mould grows on the grain sample after the fumigation treatment (detected by a microscope), and no fumigant residue exists on the grain sample after the fumigation treatment (detected and analyzed by a gas chromatography-mass spectrometer (GC-Ms)); in addition, the color of the grain sample after the fumigation treatment is observed by a color difference meter and is not obviously changed.
The grain sample treated by the fumigation in the embodiment is placed in a room temperature environment, and the mold and bacteria tracking detection is performed regularly, and the detection results are shown in the following table:
Storage time 0 month 1 month 3 months old 6 months old
Growth of mold and bacteria no any mildew or fungus no any mildew or fungus No any mildew or fungus No any mildew or fungus
The invention can realize one-time treatment of various grains and various mildews and bacteria in the same fumigation environment.
Example 7: experiment of grain fumigation
Grain variety: corn, rice, wheat, soybean, broad bean, potato, sweet potato, etc
Disease: aspergillus, Penicillium, Trichoderma, Rhizopus cereus, Rhizopus, Trichoderma, Staphylococcus aureus, Escherichia coli, Bacillus megaterium, Bacillus subtilis, Pseudomonas fluorescens, etc
Fumigant: fumigant 15
Firstly, loading a fumigant on cyclodextrin, then placing the cyclodextrin in a bag with meshes on the surface, then placing the bag at the bottom of a glass jar, placing a grain sample above the bag (which can be realized by arranging a fixed frame in the glass jar), sealing the glass jar, and fumigating at the ambient temperature of 30 ℃.
Through sampling and monitoring, the following results are obtained: after 24 hours of fumigation, no mould grows on the grain sample after the fumigation treatment (detected by a microscope), and no fumigant residue exists on the grain sample after the fumigation treatment (detected and analyzed by a gas chromatography-mass spectrometer (GC-Ms)); in addition, the color of the grain sample after the fumigation treatment is observed by a color difference meter and is not obviously changed.
The grain sample treated by the fumigation in the embodiment is placed in a room temperature environment, and the mold and bacteria tracking detection is performed regularly, and the detection results are shown in the following table:
Storage time 0 month 1 month 3 months old 6 months old
Growth of mold and bacteria No any mildew or fungus No any mildew or fungus No any mildew or fungus No any mildew or fungus
The invention can realize one-time treatment of various grains and various mildews and bacteria in the same fumigation environment.
Example 8: experiment of grain fumigation
Grain variety: corn, rice, wheat, soybean, broad bean, potato, sweet potato, etc
Disease: aspergillus, Penicillium, Trichoderma, Rhizopus cereus, Rhizopus, Trichoderma, Staphylococcus aureus, Escherichia coli, Bacillus megaterium, Bacillus subtilis, Pseudomonas fluorescens, etc
Fumigant: fumigant 12(CAS number: 1397690-78-6)
firstly, a fumigant is loaded on filter paper, then the filter paper is placed in a hollow box body with meshes on the surface and a fan and a speed regulation function, then the box body is placed at the bottom of a glass cylinder, a grain sample is placed above the box body (which can be realized by arranging a fixed frame in the glass cylinder), the glass cylinder is sealed, and the fumigation is carried out under the condition that the fan is opened at room temperature (the wind speed is set to be high).
Through sampling and monitoring, the following results are obtained: after 20 hours of fumigation, no mould grows on the grain sample after the fumigation treatment (detected by a microscope), and no fumigant residue exists on the grain sample after the fumigation treatment (detected and analyzed by a gas chromatography-mass spectrometer (GC-Ms)); in addition, the color of the grain sample after the fumigation treatment is observed by a color difference meter and is not obviously changed.
The grain sample treated by the fumigation in the embodiment is placed in a room temperature environment, and the mold and bacteria tracking detection is performed regularly, and the detection results are shown in the following table:
Storage time 0 month 1 month 3 months old 6 months old
Growth of mold and bacteria no any mildew or fungus No any mildew or fungus No any mildew or fungus No any mildew or fungus
The invention can realize one-time treatment of various grains and various mildews and bacteria in the same fumigation environment.
Example 9: experiment of grain fumigation
Grain variety: corn, rice, wheat, soybean, broad bean, potato, sweet potato, etc
Disease: weevil, moth, clothe fish, wheat moth, tobacco beetle, cockroach and indian meal moth
fumigant:
Fumigant 5(CAS number: 120801-74-3);
fumigant 7(CAS number: 120801-74-3);
Fumigant 11(CAS number: 155820-78-3);
Fumigant 43(CAS number: 139631-62-2);
Loading any one of the fumigants on silica gel particles, placing the silica gel particles in a bag with meshes on the surface, placing the bag at the bottom of a glass jar, placing a grain sample above the bag (which can be realized by arranging a fixed frame in the glass jar), sealing the glass jar, and fumigating at room temperature; the death condition of pests in the soil is monitored by sampling regularly, and the following monitoring results are obtained:
The detection and analysis of the gas chromatograph and mass spectrometer (GC-Ms) show that: no fumigant residue exists on the grain sample fumigated by any fumigant; in addition, the color of the grain sample fumigated by any one of the fumigants is not obviously changed through observation of a color difference meter.
The grain sample fumigated by any one of the fumigants in the embodiment is placed in a room temperature environment, and the growth condition of pests is regularly tracked, so that the following detection results are obtained:
storage time 0 month 1 month 3 months old 6 months old
Survival and growth of pests Without any pest Without any pest Without any pest Without any pest
The invention can realize one-time treatment of various grains and various pests in the same fumigation environment.
Example 10: experiment of grain fumigation
Grain variety: corn, rice, wheat, soybean, broad bean, potato, sweet potato, etc
disease: weevil, moth, clothe fish, wheat moth, tobacco beetle, cockroach and indian meal moth
Fumigant:
Fumigant 42(CAS number: 76876-59-0);
Fumigant 53(CAS number: 187143-10-8);
Fumigant 54(CAS number: 700-25-4);
Loading any one of the fumigants on silica gel particles, placing the silica gel particles in a bag with meshes on the surface, placing the bag at the bottom of a glass jar, placing a grain sample above the bag (which can be realized by arranging a fixed frame in the glass jar), sealing the glass jar, and fumigating at the ambient temperature of 40 ℃; the death condition of pests in the soil is monitored by sampling regularly, and the following monitoring results are obtained:
The detection and analysis of the gas chromatograph and mass spectrometer (GC-Ms) show that: no fumigant residue exists on the grain sample fumigated by any fumigant; in addition, the color of the grain sample fumigated by any one of the fumigants is slightly changed by a color difference meter.
The grain sample fumigated by any one of the fumigants in the embodiment is placed in a room temperature environment, and the growth condition of pests is regularly tracked, so that the following detection results are obtained:
Storage time 0 month 1 month 3 months old 6 months old
Survival and growth of pests Without any pest Without any pest Without any pest Without any pest
The invention can realize one-time treatment of various grains and various pests in the same fumigation environment.
Example 11: experiment of grain fumigation
Grain variety: corn, rice, wheat, soybean, broad bean, potato, sweet potato, etc
Disease: weevil, moth, clothe fish, wheat moth, tobacco beetle, cockroach and indian meal moth
Fumigant: fumigant 12(CAS number: 1397690-78-6)
Firstly, loading a fumigant on cyclodextrin, then placing the cyclodextrin in a bag with meshes on the surface, then placing the bag at the bottom of a glass jar, placing a grain sample above the bag (which can be realized by arranging a fixed frame in the glass jar), sealing the glass jar, and fumigating at the ambient temperature of 30 ℃; the pest death was monitored by periodic sampling and detailed results are shown in the following table:
the detection and analysis of the gas chromatograph-mass spectrometer show that: no fumigant residue exists on the grain sample after the fumigation treatment; in addition, the color of the grain sample after the fumigation treatment is observed by a color difference meter and is not obviously changed.
The grain sample treated by the fumigation in the embodiment is placed in a room temperature environment, the growth condition of pests is tracked periodically, and the detection results are shown in the following table:
storage time 0 month 1 month 3 months old 6 months old
Survival and growth of pests without any pest Without any pest without any pest Without any pest
The invention can realize one-time treatment of various grains and various pests in the same fumigation environment.
Example 12: experiment of grain fumigation
Grain variety: corn, rice, wheat, soybean, broad bean, potato, sweet potato, etc
disease: weevil, moth, clothe fish, wheat moth, tobacco beetle, cockroach and indian meal moth
Fumigant: fumigant 28(CAS number: 847661-06-7)
Firstly, loading a fumigant on filter paper, then placing the filter paper in a hollow box body with meshes on the surface and a fan and a speed regulation function, then placing the box body at the bottom of a glass cylinder, placing a grain sample above the box body (which can be realized by arranging a fixed frame in the glass cylinder), sealing the glass cylinder, and opening the fan (setting the wind speed at a high speed) at room temperature for fumigation; the pest death was monitored by periodic sampling and detailed results are shown in the following table:
The detection and analysis of the gas chromatograph-mass spectrometer show that: no fumigant residue exists on the grain sample after the fumigation treatment; in addition, the color of the grain sample after the fumigation treatment is observed by a color difference meter and is not obviously changed.
The grain sample treated by the fumigation in the embodiment is placed in a room temperature environment, the growth condition of pests is tracked periodically, and the detection results are shown in the following table:
Storage time 0 month 1 month 3 months old 6 months old
Survival and growth of pests Without any pest Without any pest Without any pest Without any pest
The invention can realize one-time treatment of various grains and various pests in the same fumigation environment.
Example 13: experiment of grain fumigation
Grain variety: corn, rice, wheat, soybean, broad bean, potato, sweet potato, etc
Disease: weevil, moth, clothe fish, wheat moth, tobacco beetle, cockroach and indian meal moth
fumigant: fumigant 33(CAS number: 51849-05-9)
Firstly, loading a fumigant on filter paper, then placing the filter paper in a hollow box body with meshes on the surface and a fan and a speed regulation function, then placing the box body at the bottom of a glass jar, placing a grain sample above the box body (which can be realized by arranging a fixed frame in the glass jar), sealing the glass jar, and adjusting the temperature of the box body to 35 ℃ for fumigation; the pest death was monitored by periodic sampling and detailed results are shown in the following table:
the detection and analysis of the gas chromatograph-mass spectrometer show that: no fumigant residue exists on the grain sample after the fumigation treatment; in addition, the color of the grain sample after the fumigation treatment is observed by a color difference meter and is not obviously changed.
The grain sample treated by the fumigation in the embodiment is placed in a room temperature environment, the growth condition of pests is tracked periodically, and the detection results are shown in the following table:
Storage time 0 month 1 month 3 months old 6 months old
survival and growth of pests Without any pest Without any pest Without any pest Without any pest
The invention can realize one-time treatment of various grains and various pests in the same fumigation environment.
Example 14-1: experiment of grain fumigation
Grain variety: corn, rice, wheat, soybean, broad bean, potato, sweet potato, etc
Disease: aspergillus, Penicillium, Trichoderma, Rhizopus cerealis, Rhizopus, Trichoderma, Staphylococcus aureus, Escherichia coli, Bacillus megaterium, Bacillus subtilis, Pseudomonas fluorescens, weevil, Chrysomyiame gacephala, Chlamydomonas, Mylophaga, tobacco beetle, cockroach, Indian meal moth, etc
Fumigant: fumigant 24(CAS number: 677-25-8)
Firstly, directly placing a fumigant in a culture dish, then placing a grain sample above the culture dish, and fumigating at room temperature; the pest death was monitored by periodic sampling and detailed results are shown in the following table:
The detection and analysis of the gas chromatograph-mass spectrometer show that: no fumigant residue exists on the grain sample after the fumigation treatment; in addition, the color of the grain sample after the fumigation treatment is observed by a color difference meter and is not obviously changed.
The grain sample treated by the fumigation of the embodiment is placed in a room temperature environment, the growth conditions of mold, bacteria and pests are tracked periodically, and the detection results are shown in the following table:
Storage time 0 month 1 month 3 months old 6 months old
Survival and growth of pests Without any pest Without any pest Without any pest Without any pest
Growth of mold and bacteria No any mildew or fungus No any mildew or fungus No any mildew or fungus No any mildew or fungus
The invention can realize one-time treatment of various grains and various pests, mildews and bacteria in the same fumigation environment.
Example 14-2: experiment of grain fumigation
Grain variety: corn, rice, wheat, soybean, broad bean, potato, sweet potato, etc
Disease: aspergillus, Penicillium, Trichoderma, Rhizopus cerealis, Rhizopus, Trichoderma, Staphylococcus aureus, Escherichia coli, Bacillus megaterium, Bacillus subtilis, Pseudomonas fluorescens, weevil, Chrysomyiame gacephala, Chlamydomonas, Mylophaga, tobacco beetle, cockroach, Indian meal moth, etc
Fumigant: fumigant 24(CAS number: 677-25-8)
Firstly, loading a fumigant on filter paper, then placing the filter paper at the bottom of a glass jar, then placing a grain sample above the filter paper (which can be realized by arranging a fixed frame in the glass jar), sealing the glass jar, and fumigating at room temperature; the pest death was monitored by periodic sampling and detailed results are shown in the following table:
The detection and analysis of the gas chromatograph-mass spectrometer show that: no fumigant residue exists on the grain sample after the fumigation treatment; in addition, the color of the grain sample after the fumigation treatment is observed by a color difference meter and is not obviously changed.
The grain sample treated by the fumigation of the embodiment is placed in a room temperature environment, the growth conditions of mold, bacteria and pests are tracked periodically, and the detection results are shown in the following table:
Storage time 0 month 1 month 3 months old 6 months old
Survival and growth of pests Without any pest Without any pest Without any pest Without any pest
Growth of mold and bacteria No any mildew or fungus No any mildew or fungus No any mildew or fungus No any mildew or fungus
The invention can realize one-time treatment of various grains and various pests, mildews and bacteria in the same fumigation environment.
Example 14-3: experiment of grain fumigation
Grain variety: corn, rice, wheat, soybean, broad bean, potato, sweet potato, etc
Disease: aspergillus, Penicillium, Trichoderma, Rhizopus cerealis, Rhizopus, Trichoderma, Staphylococcus aureus, Escherichia coli, Bacillus megaterium, Bacillus subtilis, Pseudomonas fluorescens, weevil, Chrysomyiame gacephala, Chlamydomonas, Mylophaga, tobacco beetle, cockroach, Indian meal moth, etc
Fumigant: fumigant 24(CAS number: 677-25-8)
Firstly, loading a fumigant on filter paper, then placing the filter paper in a hollow box body with meshes on the surface and a fan and a speed regulation function, then placing the box body at the bottom of a glass cylinder, placing a grain sample above the box body (which can be realized by arranging a fixed frame in the glass cylinder), sealing the glass cylinder, and opening the fan at room temperature (the wind speed is set to be medium speed) for fumigation; the pest death was monitored by periodic sampling and detailed results are shown in the following table:
The detection and analysis of the gas chromatograph-mass spectrometer show that: no fumigant residue exists on the grain sample after the fumigation treatment; in addition, the color of the grain sample after the fumigation treatment is observed by a color difference meter and is not obviously changed.
The grain sample treated by the fumigation of the embodiment is placed in a room temperature environment, the growth conditions of mold, bacteria and pests are tracked periodically, and the detection results are shown in the following table:
Storage time 0 month 1 month 3 months old 6 months old
Survival and growth of pests Without any pest Without any pest Without any pest Without any pest
Growth of mold and bacteria No any mildew or fungus No any mildew or fungus No any mildew or fungus No any mildew or fungus
The invention can realize one-time treatment of various grains and various pests, mildews and bacteria in the same fumigation environment.
Examples 14 to 4: experiment of grain fumigation
Grain variety: corn, rice, wheat, soybean, broad bean, potato, sweet potato, etc
disease: aspergillus, Penicillium, Trichoderma, Rhizopus cerealis, Rhizopus, Trichoderma, Staphylococcus aureus, Escherichia coli, Bacillus megaterium, Bacillus subtilis, Pseudomonas fluorescens, weevil, Chrysomyiame gacephala, Chlamydomonas, Mylophaga, tobacco beetle, cockroach, Indian meal moth, etc
Fumigant: fumigant 24(CAS number: 677-25-8)
Firstly, loading a fumigant on filter paper, then placing the filter paper in a hollow box body with meshes on the surface and self-heating and temperature-adjusting functions, then placing the box body at the bottom of a glass jar, placing a grain sample above the box body (which can be realized by arranging a fixed frame in the glass jar), sealing the glass jar, and adjusting the temperature of the box body to 30 ℃ for fumigation; the pest death was monitored by periodic sampling and detailed results are shown in the following table:
The detection and analysis of the gas chromatograph-mass spectrometer show that: no fumigant residue exists on the grain sample after the fumigation treatment; in addition, the color of the grain sample after the fumigation treatment is observed by a color difference meter and is not obviously changed.
The grain sample treated by the fumigation of the embodiment is placed in a room temperature environment, the growth conditions of mold, bacteria and pests are tracked periodically, and the detection results are shown in the following table:
Storage time 0 month 1 month 3 months old 6 months old
Survival and growth of pests Without any pest Without any pest Without any pest Without any pest
Growth of mold and bacteria No any mildew or fungus No any mildew or fungus no any mildew or fungus no any mildew or fungus
The invention can realize one-time treatment of various grains and various pests, mildews and bacteria in the same fumigation environment.
Examples 14 to 5: experiment of grain fumigation
Grain variety: corn, rice, wheat, soybean, broad bean, potato, sweet potato, etc
Disease: aspergillus, Penicillium, Trichoderma, Rhizopus cerealis, Rhizopus, Trichoderma, Staphylococcus aureus, Escherichia coli, Bacillus megaterium, Bacillus subtilis, Pseudomonas fluorescens, weevil, Chrysomyiame gacephala, Chlamydomonas, Mylophaga, tobacco beetle, cockroach, Indian meal moth, etc
Fumigant: fumigant 24(CAS number: 677-25-8)
Firstly, loading a fumigant on filter paper, then placing the filter paper in a hollow box body with meshes on the surface and self-provided with functions of fan speed regulation and self-heating temperature regulation, then placing the box body at the bottom of a glass cylinder, placing a grain sample above the box body (which can be realized by arranging a fixed frame in the glass cylinder), sealing the glass cylinder, and regulating the temperature of the box body to be 40 ℃ for fumigation; the pest death was monitored by periodic sampling and detailed results are shown in the following table:
The detection and analysis of the gas chromatograph-mass spectrometer show that: no fumigant residue exists on the grain sample after the fumigation treatment; in addition, the color of the grain sample after the fumigation treatment is observed by a color difference meter and is not obviously changed.
The grain sample treated by the fumigation of the embodiment is placed in a room temperature environment, the growth conditions of mold, bacteria and pests are tracked periodically, and the detection results are shown in the following table:
Storage time 0 month 1 month 3 months old 6 months old
Survival and growth of pests Without any pest Without any pest Without any pest Without any pest
mildew,Growth of bacteria No any mildew or fungus No any mildew or fungus No any mildew or fungus No any mildew or fungus
The invention can realize one-time treatment of various grains and various pests, mildews and bacteria in the same fumigation environment.
Examples 14 to 6: experiment of grain fumigation
Grain variety: corn, rice, wheat, soybean, broad bean, potato, sweet potato, etc
disease: aspergillus, Penicillium, Trichoderma, Rhizopus cerealis, Rhizopus, Trichoderma, Staphylococcus aureus, Escherichia coli, Bacillus megaterium, Bacillus subtilis, Pseudomonas fluorescens, weevil, Chrysomyiame gacephala, Chlamydomonas, Mylophaga, tobacco beetle, cockroach, Indian meal moth, etc
Fumigant: fumigant 24(CAS number: 677-25-8)
Firstly, loading a fumigant on filter paper, then placing the filter paper in a hollow box body with meshes on the surface and a self-contained fan and a temperature regulation function, then placing the box body at the bottom of a glass jar, placing a grain sample above the box body, sealing the glass jar, regulating the temperature of the box body to be 30 ℃, and simultaneously opening the fan (setting the wind speed to be low) for fumigation; the pest death was monitored by periodic sampling and detailed results are shown in the following table:
The detection and analysis of the gas chromatograph-mass spectrometer show that: no fumigant residue exists on the grain sample after the fumigation treatment; in addition, the color of the grain sample after the fumigation treatment is observed by a color difference meter and is not obviously changed.
The grain sample treated by the fumigation of the embodiment is placed in a room temperature environment, the growth conditions of mold, bacteria and pests are tracked periodically, and the detection results are shown in the following table:
Storage time 0 month 1 month 3 months old 6 months old
survival and growth of pests Without any pest Without any pest Without any pest without any pest
Growth of mold and bacteria No any mildew or fungus No any mildew or fungus No any mildew or fungus No any mildew or fungus
The invention can realize one-time treatment of various grains and various pests, mildews and bacteria in the same fumigation environment.
From the experimental results of examples 14-1 to 14-6, it can be seen that: the closed environment, the wind power of the fan and the proper heating are favorable for the fumigation effect, and the fumigation time can be obviously shortened under the same fumigation effect.
Example 15: experiment of grain fumigation
Grain variety: corn, rice, wheat, soybean, broad bean, potato, sweet potato, etc
Disease: aspergillus, Penicillium, Trichoderma, Rhizopus cerealis, Rhizopus, Trichoderma, Staphylococcus aureus, Escherichia coli, Bacillus megaterium, Bacillus subtilis, Pseudomonas fluorescens, weevil, Chrysomyiame gacephala, Chlamydomonas, Mylophaga, tobacco beetle, cockroach, Indian meal moth, etc
Fumigant:
Fumigant 16Fumigant 17
Fumigant 18Fumigant: fumigant 19
Fumigant 20Fumigant 21
Fumigant 22
Fumigant 23
Directly placing any fumigant in a culture dish, placing a grain sample above the culture dish, and fumigating at room temperature; the death condition of pests in the soil is monitored by sampling regularly, and the following monitoring results are obtained:
The detection and analysis of the gas chromatograph and mass spectrometer (GC-Ms) show that: no fumigant residue exists on the grain sample fumigated by any fumigant; in addition, the color of the grain sample fumigated by any one of the fumigants is not obviously changed through observation of a color difference meter.
The grain sample fumigated by any one of the fumigants in this embodiment is placed in a room temperature environment, and the growth conditions of mold, bacteria and pests are regularly tracked, so that the following detection results are obtained:
Storage time 0 month 1 month 3 months old 6 months old
Survival and growth of pests Without any pest without any pest Without any pest Without any pest
Growth of mold and bacteria No any mildew or fungus No any mildew or fungus No any mildew or fungus No any mildew or fungus
The invention can realize one-time treatment of various grains and various pests, mildews and bacteria in the same fumigation environment.
Example 16: experiment of grain fumigation
Grain variety: corn, rice, wheat, soybean, broad bean, potato, sweet potato, etc
Disease: aspergillus, Penicillium, Trichoderma, Rhizopus cerealis, Rhizopus, Trichoderma, Staphylococcus aureus, Escherichia coli, Bacillus megaterium, Bacillus subtilis, Pseudomonas fluorescens, weevil, Chrysomyiame gacephala, Chlamydomonas, Mylophaga, tobacco beetle, cockroach, Indian meal moth, etc
Fumigant: fumigant 13(CAS:1536468-56-0)
Firstly, loading a fumigant on filter paper, then placing the filter paper in a hollow box body with meshes on the surface and self-provided with functions of fan speed regulation and self-heating temperature regulation, then placing the box body at the bottom of a glass cylinder, placing a grain sample above the box body (which can be realized by arranging a fixed frame in the glass cylinder), sealing the glass cylinder, and regulating the temperature of the box body to be 40 ℃ for fumigation; the pest death was monitored by periodic sampling and detailed results are shown in the following table:
The detection and analysis of the gas chromatograph-mass spectrometer show that: no fumigant residue exists on the grain sample after the fumigation treatment; in addition, the color of the grain sample after the fumigation treatment is observed by a color difference meter and is not obviously changed.
The grain sample treated by the fumigation of the embodiment is placed in a room temperature environment, the growth conditions of mold, bacteria and pests are tracked periodically, and the detection results are shown in the following table:
Storage time 0 month 1 month 3 months old 6 months old
Survival and growth of pests Without any pest Without any pest Without any pest Without any pest
Growth of mold and bacteria No any mildew or fungus Without anything elseMold and fungus No any mildew or fungus No any mildew or fungus
The invention can realize one-time treatment of various grains and various pests, mildews and bacteria in the same fumigation environment.
Example 17: experiment of grain fumigation
grain variety: corn, rice, wheat, soybean, broad bean, potato, sweet potato, etc
Disease: aspergillus, Penicillium, Trichoderma, Rhizopus cerealis, Rhizopus, Trichoderma, Staphylococcus aureus, Escherichia coli, Bacillus megaterium, Bacillus subtilis, Pseudomonas fluorescens, weevil, Chrysomyiame gacephala, Chlamydomonas, Mylophaga, tobacco beetle, cockroach, Indian meal moth, etc
Fumigant: fumigant 14(CAS number: 1536468-56-0)
Firstly, loading a fumigant on filter paper, then placing the filter paper in a hollow box body with meshes on the surface and self-heating and temperature-adjusting functions, then placing the box body at the bottom of a glass jar, placing a grain sample above the box body (which can be realized by arranging a fixed frame in the glass jar), sealing the glass jar, and adjusting the temperature of the box body to 30 ℃ for fumigation; the pest death was monitored by periodic sampling and detailed results are shown in the following table:
The detection and analysis of the gas chromatograph-mass spectrometer show that: no fumigant residue exists on the grain sample after the fumigation treatment; in addition, the color of the grain sample after the fumigation treatment is observed by a color difference meter and is not obviously changed.
The grain sample treated by the fumigation of the embodiment is placed in a room temperature environment, the growth conditions of mold, bacteria and pests are tracked periodically, and the detection results are shown in the following table:
Storage time 0 month 1 month 3 months old 6 months old
Survival and growth of pests Without any pest Without any pest Without any pest Without any pest
Growth of mold and bacteria No any mildew or fungus No any mildew or fungus No any mildew or fungus No any mildew or fungus
The invention can realize one-time treatment of various grains and various pests, mildews and bacteria in the same fumigation environment.
Example 18: experiment of grain fumigation
Grain variety: corn, rice, wheat, soybean, broad bean, potato, sweet potato, etc
Disease: aspergillus, Penicillium, Trichoderma, Rhizopus cerealis, Rhizopus, Trichoderma, Staphylococcus aureus, Escherichia coli, Bacillus megaterium, Bacillus subtilis, Pseudomonas fluorescens, weevil, Chrysomyiame gacephala, Chlamydomonas, Mylophaga, tobacco beetle, cockroach, Indian meal moth, etc
Fumigant: fumigant 4: (CAS number: 756-21-8)
Firstly, loading a fumigant on filter paper, then placing the filter paper in a hollow box body with meshes on the surface and a fan and a speed regulation function, then placing the box body at the bottom of a glass cylinder, placing a grain sample above the box body (which can be realized by arranging a fixed frame in the glass cylinder), sealing the glass cylinder, and opening the fan at room temperature (the wind speed is set to be medium speed) for fumigation; the pest death was monitored by periodic sampling and detailed results are shown in the following table:
The detection and analysis of the gas chromatograph-mass spectrometer show that: no fumigant residue exists on the grain sample after the fumigation treatment; in addition, the color of the grain sample after the fumigation treatment is observed by a color difference meter and is not obviously changed.
The grain sample treated by the fumigation of the embodiment is placed in a room temperature environment, the growth conditions of mold, bacteria and pests are tracked periodically, and the detection results are shown in the following table:
Storage time 0 month 1 month 3 months old 6 months old
Survival and growth of pests Without any pest Without any pest Without any pest Without any pest
Growth of mold and bacteria No any mildew or fungus No any mildew or fungus No any mildew or fungus No any mildew or fungus
The invention can realize one-time treatment of various grains and various pests, mildews and bacteria in the same fumigation environment.
Example 19: experiment of grain fumigation
Grain variety: corn, rice, wheat, soybean, broad bean, potato, sweet potato, etc
Disease: aspergillus, Penicillium, Trichoderma, Rhizopus cerealis, Rhizopus, Trichoderma, Staphylococcus aureus, Escherichia coli, Bacillus megaterium, Bacillus subtilis, Pseudomonas fluorescens, weevil, Chrysomyiame gacephala, Chlamydomonas, Mylophaga, tobacco beetle, cockroach, Indian meal moth, etc
Fumigant:
Fumigant 2(CAS number: 815-36-1);
fumigant 8(CAS number: 2927-22-2);
Fumigant 26(CAS number: 154264-08-1);
Fumigant 45(CAS number: 2674-37-5);
Loading any one of the fumigants on filter paper, placing the filter paper at the bottom of a glass jar, placing a grain sample above the filter paper (which can be realized by arranging a fixed frame in the glass jar), sealing the glass jar, and fumigating at room temperature; the death condition of pests in the soil is monitored by sampling regularly, and the following detection results are obtained:
The detection and analysis of the gas chromatograph and mass spectrometer (GC-Ms) show that: no fumigant residue exists on the grain sample fumigated by any fumigant; in addition, the color of the grain sample fumigated by any one of the fumigants is not obviously changed through observation of a color difference meter.
The grain sample fumigated by any one of the fumigants in this embodiment is placed in a room temperature environment, and the growth conditions of mold, bacteria and pests are regularly tracked, so that the following detection results are obtained:
Storage time 0 month 1 month 3 months old 6 months old
Survival and growth of pests Without any pest Without any pest Without any pest Without any pest
Growth of mold and bacteria No any mildew or fungus No any mildew or fungus No any mildew or fungus No any mildew or fungus
The invention can realize one-time treatment of various grains and various pests, mildews and bacteria in the same fumigation environment.
Example 20: experiment of grain fumigation
Grain variety: corn, rice, wheat, soybean, broad bean, potato, sweet potato, etc
Disease: aspergillus, Penicillium, Trichoderma, Rhizopus cerealis, Rhizopus, Trichoderma, Staphylococcus aureus, Escherichia coli, Bacillus megaterium, Bacillus subtilis, Pseudomonas fluorescens, weevil, Chrysomyiame gacephala, Chlamydomonas, Mylophaga, tobacco beetle, cockroach, Indian meal moth, etc
Fumigant: fumigant 3(CAS number: 18225-68-8)
Firstly, loading a fumigant on filter paper, then placing the filter paper in a hollow box body with meshes on the surface and a self-contained fan and a temperature regulation function, then placing the box body at the bottom of a glass jar, placing a grain sample above the box body, sealing the glass jar, regulating the temperature of the box body to be 30 ℃, and simultaneously opening the fan (setting the wind speed to be low) for fumigation; the pest death was monitored by periodic sampling and detailed results are shown in the following table:
The detection and analysis of the gas chromatograph-mass spectrometer show that: no fumigant residue exists on the grain sample after the fumigation treatment; in addition, the color of the grain sample after the fumigation treatment is observed by a color difference meter and is not obviously changed.
The grain sample treated by the fumigation of the embodiment is placed in a room temperature environment, the growth conditions of mold, bacteria and pests are tracked periodically, and the detection results are shown in the following table:
Storage time 0 month 1 month 3 months old 6 months old
Survival and growth of pests Without any pest Without any pest Without any pest Without any pest
Growth of mold and bacteria No any mildew or fungus No any mildew or fungus No any mildew or fungus No any mildew or fungus
the invention can realize one-time treatment of various grains and various pests, mildews and bacteria in the same fumigation environment.
It should be noted that the above-mentioned embodiments are only preferred embodiments of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily made by those skilled in the art within the technical scope of the present invention should be covered by the scope of the present invention.

Claims (10)

1. A fumigation method for preventing and controlling entomophthora in grain is characterized by comprising the following operations: placing the fumigant below or/and around the grain heap at room temperature to 40 ℃; the fumigant is of the general formula I:Or formula II:The chemistry shownA compound of structure (la), wherein, in the general formula I: x is halogen or hydroxy; y is1And Y2Each is independently selected from H or F; r1Is R3Substituted C1-C10Alkyl radical, R3Substituted C2-C10Alkylene radical, R3Substituted phenyl, R3Substituted benzyl, R3Substituted C3-C8Cycloalkyl radical, R3Substituted C3-C8Cycloalkenyl radical or R3substituted adamantyl; the R is3Selected from hydrogen, hydroxy, halogen, C1-C3Alkyl radical, C2-C3At least one of alkylene groups; in the general formula II: x is halogen or hydroxy; r2Is R4Substituted C1-C4Alkyl radical, R4Substituted C2-C4Alkylene radical, R4Substituted phenyl, R4Substituted benzyl, R4Substituted C3-C8Cycloalkyl radical, R4Substituted C3-C8Cycloalkenyl radical or R4Substituted adamantyl; the R is4Selected from hydrogen, hydroxy, halogen, C1-C3Alkyl radical, C2-C3at least one olefin group.
2. The fumigation method of claim 1, wherein in formula I: x is F, Cl, Br or OH; y is1And Y2Simultaneously being F or Y1、Y2One of them is F; r1Is R3Substituted C1-C10Alkyl radical, R3substituted C2-C10Alkylene radical, R3substituted phenyl, R3Substituted benzyl, R3Substituted C3-C6Cycloalkyl radical, R3Substituted C3-C6Cycloalkenyl radical or R3substituted adamantyl; the R is3at least one selected from hydrogen, hydroxyl, fluorine, chlorine, bromine, methyl, ethyl, isopropyl and allyl.
3. According to the claimsThe fumigation method according to claim 2, characterized in that in the general formula I: x is F or Cl; y is1And Y2And is simultaneously F; r1Is R3substituted C1-C4Alkyl radical, R3Substituted C2-C4Alkylene radical, R3Substituted phenyl or R3Substituted C3-C6A cycloalkyl group; the R is3At least one selected from hydrogen, hydroxyl, fluorine and chlorine.
4. The fumigation method of claim 1, wherein in formula II: x is F, Cl, Br or OH; r2is R4Substituted C1-C4Alkyl radical, R4Substituted C2-C4Alkylene radical, R4substituted phenyl, R4Substituted benzyl, R4Substituted C3-C7Cycloalkyl radical, R4Substituted C3-C7Cycloalkenyl radical or R4Substituted adamantyl; the R is4At least one selected from hydrogen, hydroxyl, fluorine, chlorine, bromine, methyl, ethyl, isopropyl and allyl.
5. the fumigation method of claim 4, wherein in formula II: x is F or Cl; r2Is R4Substituted C1-C4Alkyl radical, R4Substituted C2-C4Alkylene radical, R4Substituted C3-C7Cycloalkyl or R4substituted phenyl; the R is4At least one selected from hydrogen, hydroxyl, fluorine and chlorine.
6. The fumigation method as defined in claim 1, wherein: at room temperature, the fumigant is placed under or/and around the grain heap in a closed environment.
7. The fumigation method as defined in claim 1, wherein: the fumigant is loaded on a carrier material with adsorption effect, wherein the carrier material comprises but is not limited to filter paper, silica gel, a filter membrane, cotton, sponge or cloth.
8. The fumigation method of claim 7, wherein: the fumigant-loaded carrier material is placed in a hollow device having an outwardly diffusing mouth or mesh surface, including but not limited to a box structure, cage structure or bag.
9. The fumigation method of claim 8, wherein: the hollow device has the functions of a fan and speed regulation.
10. The fumigation method as defined in claim 8 or 9, wherein: the hollow device has the functions of self-heating and temperature regulation.
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CN106343013A (en) * 2015-07-19 2017-01-25 中国科学院上海有机化学研究所 Grain storage method
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CN111084186B (en) * 2018-10-23 2021-09-03 中国科学院上海有机化学研究所 Method for preventing and controlling entomophthora in grains

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1075057A (en) * 1992-01-15 1993-08-11 联邦科学及工业研究组织 Carbonyl sulphide fumigant
CN1138948A (en) * 1995-06-29 1997-01-01 叶中良 Mildew preventing method of grains
CN1156952A (en) * 1994-07-05 1997-08-13 联邦科学及工业研究组织 Cyanogen fumigants and method of fumigation using cyanogen
CN1681387A (en) * 2002-09-19 2005-10-12 阿肯马公司 Pesticide treatment for stored produce, enclosures, structures and works of art comprises applying a volatile sulfur compound
CN101102670A (en) * 2004-12-24 2008-01-09 联邦科学技术研究组织 Pesticide compositions and methods
CN101558760A (en) * 2009-05-20 2009-10-21 武汉乐立基生物科技有限责任公司 Compound agent of ethyl isothiocyanate and allyl isothiocyanate and application thereof
CN102464592A (en) * 2010-11-03 2012-05-23 中国中化股份有限公司 Acyl benzylamine compound and use thereof
CN104286168A (en) * 2014-11-10 2015-01-21 陕西大统投资股份有限公司 Method for preserving fresh walnut fruit

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
ES2326717B1 (en) * 2007-07-12 2010-07-26 Dmc Research Center, S.L. UNTILIZATION OF ANTIMICROBIAL AGENTS DERIVED FROM ALIACEAS FOR THE PREVENTION AND CONTROL OF CULTURE DISEASES, POST-DUTY POWERS AND AS ENVIRONMENTAL DISINFECTION PRODUCTS.
CN103997897B (en) * 2011-09-23 2018-11-30 戴弗西公司 Make the method for grain kernels decontamination with chlorine dioxide

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1075057A (en) * 1992-01-15 1993-08-11 联邦科学及工业研究组织 Carbonyl sulphide fumigant
CN1156952A (en) * 1994-07-05 1997-08-13 联邦科学及工业研究组织 Cyanogen fumigants and method of fumigation using cyanogen
CN1138948A (en) * 1995-06-29 1997-01-01 叶中良 Mildew preventing method of grains
CN1681387A (en) * 2002-09-19 2005-10-12 阿肯马公司 Pesticide treatment for stored produce, enclosures, structures and works of art comprises applying a volatile sulfur compound
CN101102670A (en) * 2004-12-24 2008-01-09 联邦科学技术研究组织 Pesticide compositions and methods
CN101558760A (en) * 2009-05-20 2009-10-21 武汉乐立基生物科技有限责任公司 Compound agent of ethyl isothiocyanate and allyl isothiocyanate and application thereof
CN102464592A (en) * 2010-11-03 2012-05-23 中国中化股份有限公司 Acyl benzylamine compound and use thereof
CN104286168A (en) * 2014-11-10 2015-01-21 陕西大统投资股份有限公司 Method for preserving fresh walnut fruit

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
《蒜素类化合物的合成以及生物活性研究》;张琛等;《中国化学会全国第十一届有机合成化学学术研讨会》;20141016;第47页 *

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