CN111685110A

CN111685110A - Application of N, N-dimethylformamide in anticoagulant rodenticide penetrant

Info

Publication number: CN111685110A
Application number: CN202010603812.0A
Authority: CN
Inventors: 姜洪雪; 姚丹丹; 冯志勇
Original assignee: Plant Protection Research Institute Guangdong Academy of Agricultural Sciences
Current assignee: Plant Protection Research Institute Guangdong Academy of Agricultural Sciences
Priority date: 2020-06-29
Filing date: 2020-06-29
Publication date: 2020-09-22

Abstract

The invention discloses application of N, N-dimethylformamide in an anticoagulant rodenticide penetrant. The N, N-dimethylformamide can be used as a penetrant to improve the water solubility of the anticoagulant rodenticide, increase the content of rice grains entering the rice husks of the medicine, improve the utilization rate of the medicine, namely, the anticoagulant rodenticide has a synergistic effect, the rodenticide effect can be ensured not to be reduced under the condition of reducing the use concentration of the anticoagulant rodenticide, and the palatability of the anticoagulant rodenticide can be improved by using the penetrant. Therefore, the use of the penetrant in the invention can reduce the deratization cost, reduce the risk of environmental pollution, reduce the probability of poisoning events of people and livestock, ensure the safety of people and livestock, prolong the service life of the anticoagulant rodenticide and delay the resistance development of the rodenticide.

Description

Application of N, N-dimethylformamide in anticoagulant rodenticide penetrant

Technical Field

The invention belongs to the technical field of deratization, and particularly relates to application of N, N-dimethylformamide in an anticoagulant rodenticide penetrant.

Background

Rodents are the most diverse, widespread, and numerous groups of mammals, some of which pose significant hazards to agricultural production, human life safety, and public safety. In order to control the harm of the pest rats, comprehensive treatment technology based on ecological regulation is generally adopted, wherein chemical control is an extremely important control measure.

The use of chemical rodenticides is still the main prevention and control method at present worldwide, and the method has low cost, quick response, good effect and easy popularization. The anticoagulant raticide is a raticide which is relatively safe, good in palatability and high in deratization efficiency, is the most important chronic chemical agent for preventing and controlling rat damage at present, and is widely used in rural and pastoral areas and cities in China since the last 80 years. However, the occurrence of the drug resistance of the rats, the occurrence of cross resistance and resistant species groups are reported in succession in areas continuously used for more than 6 years, so that the rat killing effect is greatly reduced, and the rat killing difficulty and cost are improved. The new medicine is difficult to create, and the characteristics of good palatability, high efficiency, safety and economy must be simultaneously met. Therefore, exploring and researching the synergistic effect of some chemical components on the anticoagulant rodenticide, and prolonging the service life of the rodenticide become research hotspots in recent years, and substances such as aspirin, diclofenac sodium, salicylic acid and the like have a synergistic anticoagulant effect with the anticoagulant rodenticide, but the synergistic effect is limited.

In the south of China, the climate is humid and rainy, the paddy is the most suitable bait for killing rats in agricultural areas, and the bait has the advantages of better palatability, long fresh-keeping period and wide sources. But the anticoagulant rodenticide is insoluble in water, the rice hulls have a blocking effect on the drugs, about 90% of the rodenticide is adhered to the surfaces of the rice hulls, the rice contains very little content, the rats are husked to eat the rice, the utilization rate of the drugs is low, and the risk of environmental pollution and non-target animal poisoning caused by the low utilization rate of the drugs is also higher. The penetrant belongs to one of pesticide adjuvants, has the effects of improving the permeability of effective components of the pesticide, improving the pesticide effect and reducing the usage amount of the pesticide. The condition that the penetrant is used in rodenticide is very few, Chinese patent 201310316842.3, entitled anticoagulant rodenticide penetrant and preparation method and application thereof, discloses an anticoagulant penetrant compounded by sodium hydroxide, sodium chloride, ethanol and dimethyl sulfoxide, but the research has more compounded components, the preparation method is relatively complex, and the practical application is limited.

At present, N, N-dimethylformamide which is an organic solvent is not applied in rat killing practice, and has important research value and application prospect.

Disclosure of Invention

In order to overcome the defects of the prior art, the invention mainly aims to provide the application of the N, N-dimethylformamide in the preparation of the anticoagulant rodenticide penetrant so as to improve the utilization rate and the prevention and control effect of the rodenticide, reduce the using amount of the rodenticide and reduce the ecological risk of the rodenticide.

The invention also aims to provide application of the N, N-dimethylformamide as the anticoagulant rodenticide penetrant in preparation of the synergistic anticoagulant rodenticide poison bait.

The invention further aims to provide the synergistic anticoagulant rodenticide poison bait.

The purpose of the invention is realized by the following technical scheme:

application of N, N-dimethylformamide in preparation of anticoagulant rodenticide penetrant.

The anticoagulant rodenticide penetrant can also contain other solvents.

The solvent is preferably water.

The volume ratio of the N, N-dimethylformamide to the water is 1-3: 1-3.

The application of N, N-dimethyl formamide as anticoagulant rodenticide penetrant.

The application of N, N-dimethylformamide as an anticoagulant rodenticide penetrant in preparation of synergistic anticoagulant rodenticide poison bait.

The synergistic anticoagulant rodenticide poison bait also contains grains (namely anticoagulant rodenticide bait), bromadiolone and the like.

The grain is at least one of common grains such as rice, wheat, corn and the like; preferably rice.

The dosage of the N, N-dimethylformamide is calculated according to the proportion of adding 20-60 mL of N, N-dimethylformamide per 1000g of grains; preferably, the amount of N, N-dimethylformamide added is 40mL per 1000g of grain.

The bromadiolone is preferably a bromadiolone mother solution with the effective component content of 0.5 percent.

The content of the effective components in the bromadiolone accounts for 0.0025 to 0.01 percent of the weight of the grains; preferably 0.0025% by weight of the cereal.

A synergistic anticoagulant rodenticide poison bait is prepared from N, N-dimethyl formamide, grains and bromadiolone.

The synergistic anticoagulant rodenticide poison bait can also contain other solvents.

The solvent is preferably water.

The preparation method of the synergistic anticoagulant rodenticide poison bait comprises the following steps: adding N, N-dimethylformamide into water, adding bromadiolone, uniformly mixing with grains, and airing after the liquid medicine is sucked dry to obtain the synergistic anticoagulant rodenticide poison bait.

Compared with the prior art, the invention has the following advantages and effects:

(1) most anticoagulant rodenticides are insoluble in water, the southern regions have humid climate and abundant rainfall, the rice poison bait is commonly used for killing rats, about 90 percent of drugs are adhered to the surfaces of rice hulls, the drugs are easily washed by rainwater or naturally fall off to reduce the prevention and control effect, and the poisonous rice hulls left behind after rats eat the ratchets to pollute the environment. Therefore, the invention provides the penetrant which improves the solubility and permeability of the anticoagulant rodenticide, increases the content of the rice grains entering the rice husks of the medicament, thereby improving the utilization rate of the medicament, reducing the use concentration of the rodenticide, ensuring the deratization effect under the frequent rainfall condition, lightening the environmental pollution and reducing the probability of toxic events of people and livestock; meanwhile, the service life of the anticoagulant rodenticide is prolonged, and the resistance development of the rodenticide is delayed.

(2) The anticoagulant rodenticide provided by the invention can ensure that the deratization effect is not reduced under the condition of reducing the use concentration of the anticoagulant rodenticide, and the effect is that the penetrant can improve the water solubility of the anticoagulant rodenticide, increase the content of rice grains entering the rice husks of drugs and improve the utilization rate of the drugs.

(3) The infiltration agent can improve the water solubility of the anticoagulant rodenticide, increase the content of rice grains entering the hulls of the drugs and improve the utilization rate of the drugs.

(4) The use of the penetrating agent in the invention reduces the deratization cost, lightens the risk of environmental pollution and ensures the safety of people and livestock, and the effect is that the penetrating agent causes more medicine to permeate into rice, thereby reducing the use concentration of the medicine.

(5) The use of the penetrants in the present invention enhances the palatability of the anticoagulant rodenticide, which may be due to the special odor of the penetrants.

Drawings

FIG. 1 is a graph of the amount of rodenticide in the kernels of hazel rice formulated with different adjuvants.

Detailed Description

The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto. Except where expressly indicated, the medicaments, methods and apparatus employed in the present invention are conventional in the art. The following examples are given without reference to specific experimental conditions, and are generally in accordance with conventional experimental conditions. Unless otherwise specified, all agents, reagents and raw materials used in the present invention are commercially available.

The bromadiolone mother liquor with the effective component content of 0.5 percent (namely, 2.5g of bromadiolone is contained in every 500ml of mother liquor) related in the examples is purchased from the large sanitation chemical industry Co., Ltd, Shanghai Shangqiu.

Example 1 0.0025% bromadiolone valley with 2% osmotic agent added

The compounding method of the 2% penetrant and the rodenticide is as follows:

taking 1000g of bromadiolone rice with the concentration of 0.0025 percent as an example, 20ml of N, N-dimethylformamide is accurately weighed and mixed with 60ml of water, 5ml of bromadiolone mother liquor with the content of 0.5 percent of active ingredients is added, the mixture is uniformly mixed and then is uniformly stirred with 1000g of rice, and the mixture is dried after the liquid medicine is sucked dry.

Example 2 0.0025% bromadiolone valley with 4% osmotic agent added

The compounding method of the 4% penetrant and the rodenticide is as follows:

taking 1000g of bromadiolone rice with the concentration of 0.0025 percent as an example, accurately weighing 40ml of N, N-dimethylformamide, mixing with 40ml of water, adding 5ml of bromadiolone mother liquor with the effective component content of 0.5 percent, uniformly mixing, stirring and uniformly mixing with 1000g of rice, and airing after the liquid medicine is sucked dry.

Example 3 0.0025% bromadiolone valley with 6% osmotic agent added

The compounding method of the 6 percent penetrant and the rodenticide is as follows:

taking 1000g of bromadiolone rice with the concentration of 0.0025 percent as an example, 60ml of N, N-dimethylformamide is accurately weighed and mixed with 20ml of water, 5ml of bromadiolone mother liquor with the content of 0.5 percent of active ingredients is added, the mixture is uniformly mixed and then is uniformly stirred with 1000g of rice, and the drying is carried out after the liquid medicine is sucked dry.

Example 4 comparison of rodenticide content in differently formulated kernels of cereals

(1) The test auxiliary agents are: polyethylene glycol, propylene glycol, glycerol and N, N-dimethylformamide.

(2) The preparation method comprises the following steps:

accurately weighing 20ml of N, N-dimethylformamide, mixing with 20ml of water, adding 10ml of bromadiolone mother liquor with the effective component content of 0.5%, uniformly mixing, stirring and uniformly mixing with 500g of rice, airing after the liquid medicine is sucked dry, and preparing 0.01% bromadiolone valley added with 4% of N, N-dimethylformamide; the preparation method of other adjuvants (polyethylene glycol, propylene glycol, and glycerol) is the same as above;

② a preparation method of bromadiolone valley with conventional concentration of 0.01 percent is as follows: adding 50ml of bromadiolone mother liquor with the content of 0.5 percent of active ingredients into 200ml of water, fully stirring and pouring the mixture into 2.5kg of rice, airing the mixture after the liquid medicine is sucked dry, and preparing the bromadiolone toxic rice with the concentration of 0.01 percent.

(3) Respectively measuring the content of bromadiolone in the bromadiolone kernels after the addition of the auxiliary agent by adopting a high performance liquid chromatography, taking the content of bromadiolone in the bromadiolone kernels with the concentration of 0.01 percent commonly used in southern areas as a reference, and performing sample pretreatment and measurement by adopting the following steps:

methanol extraction: manually separating the poisonous grain rice hulls from the brown rice, grinding the separated poisonous grain rice hulls and the brown rice by using a grinder, and sieving the ground rice by using a 60-mesh sieve to obtain shell powder and rice flour; then accurately weighing 1g of shell powder and 4g of rice flour, placing into a 100ml centrifuge tube with a plug, adding 40ml of methanol, vibrating for 15min after the plug is added, extracting for 15min by ultrasonic (ultrasonic frequency 40KHZ), centrifuging for 5min at 3000r/min, and separating supernatant to obtain shell powder supernatant and rice flour supernatant;

② purifying by neutral alumina solid phase extraction column: activating a neutral Alumina column (AL5006-N, Alumina N SPE,500mg/6ml) with 5ml of methanol in advance, discarding effluent, respectively taking 4ml of shell powder supernatant and 5ml of rice flour supernatant, eluting with 10ml of methanol-acetic acid (95% + 5%, v/v) solution, collecting eluent, blowing nitrogen at 60 ℃ to dry, dissolving residues with 1ml of methanol, and passing through an organic filter head (0.2 mu m, 13mm) to be detected;

measuring by high performance liquid chromatography, wherein the working conditions of the instrument are as follows: c18 column (4.6 mm. times.250 mm, 5 μm); column temperature: 30 ℃; flow rate: 0.5 ml/min; sample introduction amount: 20 mu l of the mixture; a detector: detecting by a fluorescence detector, wherein the excitation wavelength is 310nm, and the emission wavelength is 390 nm; mobile phase A: water + 0.25% (v/v) acetic acid, mobile phase B: methanol + 0.25% (v/v) acetic acid, gradient elution is shown in Table 1.

TABLE 1 gradient elution protocol

Time (minutes)	(A)％	(B)％
			0	75	25
5	5	95
			20	0	100

The results are shown in FIG. 1: the results show that the content of bromadiolone in the 0.01% bromadiolone-containing rice grains prepared by adding 4% of dimethylformamide is obviously higher than that in the other auxiliary agents (F: 145.829, P: 0.000). Therefore, the invention selects N, N-dimethylformamide as the bromadiolone valley penetrant.

Example 5 palatability and poisoning effect of Poison Valley with osmotic agent addition

(1) Results of a selective test of a penetrant-added trough on mice

Selecting adult, healthy, non-pregnant and non-traumatic Kunming mice (purchased from Cambodia district Changsheng farm in Guangzhou city), identifying male and female, weighing, adopting a selective feeding test, and breeding in a single cage, wherein the weight is averagely more than 20g, 31 females and 29 males.

Experimental mice were divided into A, B, C three groups (20 per group), of which:

group A: 5g of 0.01% bromadiolone valley (same as example 4) and 5g of rice (i.e. non-toxic) were used as optional baits;

group B: 5g of 0.0025% bromadiolone (prepared in example 2) with 4% osmotic agent added and 5g of rice (non-toxic) were used as optional baits;

group C: 0.01% bromadiolone valley (same as example 4) and 5g of rice (no-poison grain) with 4% penetrant added are used as selectable baits;

the specific process is as follows: each group of mice is raised with rice for 2 days, then 5g of rice and 5g of bromadiolone valley diagonal lines are respectively placed in a raising cage, the mice freely select to eat, the consumption of the rice and the valley is weighed every day, and new baits are replaced and the positions are exchanged. After continuously selecting for ingestion for 3 days, removing the poisonous grains, normally feeding with conventional feed, and calculating the ingestion coefficient.

The results are shown in table 2, where the feeding coefficient of 0.0025% bromadiolone trough (group B) with 4% penetrant is higher than 0.01% bromadiolone trough (group a) (t-2.971, P-0.006) and 0.01% bromadiolone trough with 4% penetrant (group C) (t-2.459, P-0.019) with good palatability. After the test was completed, all mice in the 0.0025% bromadiolone valley-treated group to which 4% penetrant was added were sacrificed (mortality rate 100%), and the mortality rates in the other two groups were 95%.

Table 2 results of selective test of penetration agent-added trough on mice

(2) Results of non-selection test of penetration agent-added valleca on white mice

Selecting adult, healthy, non-pregnant and non-traumatic Kunming mice (purchased from Cambodia district Changsheng farm in Guangzhou city), identifying male and female, weighing, adopting a non-selection quantitative feeding test, and breeding in a single cage, wherein the weight is averagely more than 20g, 26 female mice and 28 male mice.

Experimental mice were divided into A, B, C three groups, of which:

group A: 0.01% bromadiolone valley (prepared as in example 4);

group B: 0.0025% bromadiolone valley, and the preparation method comprises the following steps: adding 5ml of bromadiolone mother liquor with the effective component content of 0.5 percent into 80ml of water, fully stirring and pouring into 1.0kg of rice, and airing after the liquid medicine is sucked dry to prepare 0.0025 percent of bromadiolone toxic rice;

group C: 0.0025% bromadiolone valley with 4% osmotic agent added (prepared in example 2);

the specific process is as follows: each group of mice is fed with paddy for 2 days, and then the mice are fed with the paddy with weight of 15% for 3 days, the consumption of the paddy is weighed every day, and the bait is replaced with new bait. After 3d, removing the poisonous grains, normally feeding with conventional feed, observing for 14 days, recording death time, and calculating mortality.

The test results are shown in table 3, the poisoning effect of 0.0025% bromadiolone valley (group C) added with 4% penetrant is consistent with that of 0.01% bromadiolone valley (group A), the poisoning rate reaches 100%, and is remarkably higher than that of 0.0025% bromadiolone valley (chi) without penetrant²19.259, P is 0.000), and the average death days of the 4% penetrant added to the valley is shorter than 0.0025% bromadiolone valley (group B), which indicates that the 4% penetrant added to the 0.0025% bromadiolone valley has significant synergy.

Table 3 results of non-selective test of penetration agent-added trough on mice

The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.

Claims

The application of N, N-dimethyl formamide in preparing anticoagulant rodenticide penetrant.
2. The use of N, N-dimethylformamide as claimed in claim 1 for the preparation of an anticoagulant rodenticide penetrant, characterized in that:

the anticoagulant rodenticide penetrant can also contain a solvent;

the solvent is water;

the volume ratio of the N, N-dimethylformamide to the water is 1-3: 1-3.
The application of N, N-dimethyl formamide as anticoagulant rodenticide penetrant.
Application of N, N-dimethylformamide as an anticoagulant rodenticide penetrant in preparation of synergistic anticoagulant rodenticide poison bait.
5. Use according to claim 4, characterized in that:

the synergistic anticoagulant rodenticide poison bait also contains grains and bromadiolone;

the dosage of the N, N-dimethylformamide is calculated according to the proportion of adding 20-60 mL of N, N-dimethylformamide per 1000g of grains;

the content of the effective components in the bromadiolone accounts for 0.0025-0.01 percent of the weight of the grains.
6. Use according to claim 5, characterized in that:

the grain is at least one of rice, wheat and corn;

the bromadiolone is a bromadiolone mother solution with the effective component content of 0.5 percent.
7. A synergistic anticoagulant rodenticide poison bait is characterized in that: including N, N-dimethylformamide, cereals and bromadiolone.
8. The synergistic anticoagulant rodenticide bait according to claim 7, wherein:

the dosage of the N, N-dimethylformamide is calculated according to the proportion of adding 20-60 mL of N, N-dimethylformamide per 1000g of grains;

the content of the effective components in the bromadiolone accounts for 0.0025 to 0.01 percent of the weight of the grains;

the grain is at least one of rice, wheat and corn;

the bromadiolone is a bromadiolone mother solution with the effective component content of 0.5 percent.
9. The synergistic anticoagulant rodenticide bait according to claim 8, wherein:

the dosage of the N, N-dimethylformamide is calculated according to the proportion that 40mL of N, N-dimethylformamide is added into every 1000g of grains;

the content of the effective components in the bromadiolone accounts for 0.0025 percent of the weight of the grains.
10. The method of preparing a synergistic anticoagulant rodenticide bait according to any one of claims 7 to 9, which comprises the steps of:

adding N, N-dimethylformamide into water, adding bromadiolone, uniformly mixing with grains, and airing after the liquid medicine is sucked dry to obtain the synergistic anticoagulant rodenticide poison bait.