Nicotinoyl aniline salt compound powder and preparation method thereof

Abstract

The invention provides nicotinazinyl aniline salt compound powder and a preparation method thereof, and is characterized in that the nicotinazinyl aniline salt compound powder comprises the following components in parts by weight: 50-80 parts of nicotinazinyl aniline salt compound microspheres, 3.8-6.0 parts of L-tartaric acid, 4-5 parts of sodium tartrate, 0.2-1 part of decyl glucoside, 0.2-1 part of sodium citrate, 0.2-1 part of ascorbic acid, 1-3 parts of ammonium sulfate and 1-3 parts of sodium chloride; the nicotinoyl aniline salt composite microspheres are prepared by a method comprising the following steps: S1, weighing tea saponin powder, sodium isethionate and deionized water, mixing, and uniformly mixing under an ultrasonic condition to form a first mixed solution; s2, weighing metacrylic acid ester, N, N-methylene bisacrylamide, polyethylene glycol, dibenzoyl peroxide and toluene, mixing in a beaker, and stirring uniformly to form a second mixed solution; s3, weighing nicotinoyl aniline salt, mixing the nicotinoyl aniline salt with deionized water, and uniformly stirring to form a nicotinoyl aniline salt solution; and S4, heating the first mixed solution to 45-50 DEG C, dropwise adding the second mixed solution under a stirring condition, carrying out a stirring reaction for 0.5 h, dropwise adding the nicotinoyl aniline salt solution, continuously carrying out heat preservation for 1-2 h, and carrying out pressure reduction to remove the solvent so as to obtain the nicotinoyl aniline salt / polyacrylate / tea saponin microspheres, namely the nicotinoyl aniline salt composite microspheres.

Description

Technical Field

[0001] The invention relates to the technical field of agriculture, and in particular to nicotinamide salt complex powder and a preparation method thereof. Background Art

[0002] In the field of aquaculture, the golden apple snail is native to South America and is one of the most dangerous invasive alien species. It has strong adaptability and reproduces rapidly. It is distributed in various water environments such as rivers, lakes, and rice fields. It feeds on the stems and leaves of crops such as rice and lotus roots, which will lead to varying degrees of crop yield reduction and eutrophication of water bodies, seriously threatening the aquatic biodiversity and ecosystem stability of the invaded areas. As a common benthic mollusk, it has become one of the main pests in aquaculture waters due to its extremely strong reproductive capacity and adaptability. The large-scale breeding of golden apple snails will compete with aquaculture economic species for bait and dissolved oxygen, and its metabolites can easily lead to water quality deterioration. It is also the intermediate host of a variety of parasites (such as liver fluke), which seriously threatens the healthy growth of aquatic animals. At present, the prevention and control of river snails in aquaculture waters mainly relies on chemical synthetic drugs, such as niclosamide and metaldehyde. However, long-term use has the following significant defects: (1) They are highly toxic to non-target organisms (such as fish, shrimp, crab, etc.) and can easily cause acute poisoning of farmed species; (2) Drug residues are easily enriched in organisms, affecting the safety of aquatic products; (3) Long-term single use causes river snails to develop drug resistance, and the prevention and control efficiency decreases year by year.

[0003] In recent years, botanical pesticides have attracted attention due to their high environmental compatibility and strong target specificity. For example, rotenone is neurotoxic to mollusks, but it requires a high concentration (>50 mg / L) when used alone, which can easily cause damage to fish gill tissue; although azadirachtin can inhibit the activity of acetylcholinesterase in field snails, it has a slow action rate and a short duration; tea saponin works by destroying the cell membrane structure, but high doses can cause foam pollution in water bodies. The existing technology attempts to compound plant ingredients, but it focuses more on expanding the insecticidal spectrum, and the permeability enhancement mechanism for field snails has not been studied enough, and the contradiction between rapidity and safety has not been resolved.

[0004] In addition, the current chemical snail-killing agent nicotinamide salt has shown high efficiency in agricultural pest control. How to improve the killing efficiency of field snails while reducing the dosage of each single component through the synergistic effect of multiple components and ensure the safety of non-target organisms has become a technical difficulty that needs to be solved in this field. Traditional carriers (such as polylactic acid) are expensive and difficult to control the degradation rate. In addition, the choice of excipients directly affects the dispersibility and environmental safety of the drug. Therefore, there is an urgent need for a snail growth inhibitor that is both efficient, slow-release and environmentally friendly. Summary of the invention

[0005] In view of the problems existing in the prior art, the object of the present invention is to provide a nicotinamide salt complex powder and a preparation method thereof.

[0006] In order to solve the above technical problems, the present invention provides the following technical solutions:

[0007] A nicotinamide salt composite powder and a preparation method thereof, comprising, by weight, 50-80 parts of nicotinamide salt composite microspheres, 3.8-6.0 parts of L-tartaric acid, 4-5 parts of sodium tartrate, 0.2-1 parts of decyl glucoside, 0.2-1 parts of sodium citrate, 0.2-1 parts of ascorbic acid, 1-3 parts of ammonium sulfate, and 1-3 parts of sodium chloride; the nicotinamide salt composite microspheres are prepared by a method comprising the following steps:

[0008] S1, weighing tea saponin powder, sodium isethionate and deionized water, mixing them evenly under ultrasonic conditions to form a first mixed solution;

[0009] S2, weighing methacrylate, N,N-methylenebisacrylamide, polyethylene glycol, dibenzoyl peroxide and toluene, mixing them in a beaker, and stirring until uniform to form a second mixed solution;

[0010] S3, weighing nicotinamide salt and deionized water, mixing, and stirring evenly to form a nicotinamide salt solution;

[0011] S4, heating the first mixed solution to 45-50° C., adding the second mixed solution dropwise under stirring, stirring and reacting for 1 hour, then adding nicotinamide salt solution dropwise, and keeping the temperature for 1-2 hours. After removing the solvent under reduced pressure, nicotinamide salt / polyacrylate / tea saponin microspheres, i.e., nicotinamide salt composite microspheres, are obtained.

[0012] Preferably, the ultrasonic conditions in step S1 are a frequency of 40 kHz and a time of 30 min, and the dropping speed in step S4 is 1-2 mL / min.

[0013] Preferably, the nicotinoanilide salt complex powder comprises, calculated by weight, 70 parts of nicotinoanilide salt composite microspheres, 4 parts of L-tartaric acid, 4 parts of sodium tartrate, 0.2 parts of decyl glucoside, 0.2 parts of sodium citrate, 0.2 parts of ascorbic acid, 1 part of ammonium sulfate, and 1 part of sodium chloride.

[0014] Preferably, in S1, the mass ratio of tea saponin powder, sodium isethionate and deionized water is 1:0.01-0.06:10-50.

[0015] Preferably, in S2, the mass ratio of methacrylate, N,N-methylenebisacrylamide, polyethylene glycol, dibenzoyl peroxide and toluene is 1.5-2.2:0.5-0.7:0.1-0.2:0.03-0.07:20-50.

[0016] Preferably, in S3, the nicotinamide salt is nicotinamide sulfate or nicotinamide hydrochloride.

[0017] Preferably, in S3, the mass ratio of nicotinamide salt to deionized water is 1:4-10.

[0018] Preferably, in S4, the mass ratio of the first mixed solution, the second mixed solution and the nicotinamide salt solution is 0.3-0.8:1.3-1.7:1.

[0019] The present invention provides a nicotinamide salt composite powder and a preparation method thereof, comprising:

[0020] (1) Weigh the nicotinamide salt composite microspheres according to weight, grind and mix in a mortar.

[0021] 3-8min, forming the first mixed material;

[0022] (2) weighing decyl glucoside, ammonium sulfate, sodium citrate, ascorbic acid, sodium chloride, and sodium tartrate according to weight, grinding and mixing in a mortar for 2-5 minutes to form a second mixture;

[0023] (3) Grinding and mixing the first mixed material and the second mixed material in a mortar for 4-10 minutes to form nicotinamide salt complex powder.

[0024] Preferably, a method for preparing a nicotinamide salt complex powder is as follows:

[0025] (1) Weighing nicotinamide salt composite microspheres according to weight, grinding and mixing in a mortar for 5 minutes to form a first mixture;

[0026] (2) weighing decyl glucoside, sodium citrate, ascorbic acid, ammonium sulfate, sodium chloride, and sodium tartrate according to weight, grinding and mixing in a mortar for 4 minutes to form a second mixture;

[0027] (3) Grinding and mixing the first mixed material and the second mixed material in a mortar for 6 minutes to form nicotinamide salt complex powder.

[0028] It has the following advantages:

[0029] 1. The present invention discloses a nicotinamide salt composite powder and a preparation method thereof. The composite powder comprises nicotinamide salt composite microspheres, L-tartaric acid and additives. Compared with traditional nicotinamide salt composite microspheres, the product obtained by the present invention has better dispersibility and a faster sustained release rate, so that the snails will not be killed quickly due to too slow sustained release. The most important reference factor in the breeding process is the continuous mortality rate of field snails. The nicotinamide salt composite microspheres play the characteristics of continuous release of drugs and also improve the stability of drugs.

[0030] 2. Nicotinoylanilide salt composite microspheres are self-made sustained-release microspheres of the present invention, with tea saponin as a natural porogen, and a porous network composite material formed by combining polymethacrylate and tea saponin as the microsphere wall, and nicotinoylanilide salt as the microsphere sustained-release agent. The microspheres are porous, not only have a faster and stronger sustained-release effect, can ensure the content of nicotinoylanilide salt, but also have strong hydrophilicity, can have a good dispersion effect in water, and realize drug gradient release.

[0031] 3. Sodium isethionate is added during the synthesis of the nicotinoylanilide salt composite microspheres of the present invention. The addition of sodium isethionate as a surfactant enhances the synthesis between the raw materials of the microspheres.

[0032] 4. The process of preparing nicotinamide salt composite microspheres of the present invention is different from the conventional process in that nicotinamide sulfate is added during the semi-molding process of the microspheres. In this process, the consumption of nicotinamide salt in the polymerization process of methacrylate is avoided and the nicotinamide salt can be more conveniently introduced into the pores of the microspheres without being wrapped by the polymer and affecting the precipitation of nicotinamide salt.

[0033] 5. In addition, due to the compounding of tea saponin powder, tea saponin powder itself has a strong snail-killing effect, so the snail-killing effect of the nicotinamide salt complex powder prepared by the present invention is also more excellent.

[0034] 6. In addition, due to the compound of ammonium sulfate and sodium chloride, during the snail killing process, the growth of aquatic plants, algae and microorganisms in the breeding environment is regulated, thereby achieving an inhibitory effect on snail production.

[0035] 7. Use sustained-release technology to control the release rate, prolong the efficacy, reduce the frequency of application, reduce the risk of exposure to non-target organisms, and reflect environmental protection.

[0036] 8. L-tartaric acid and sodium tartrate are used to form a buffer system to ensure that nicotinamide salt works within the appropriate pH range. Tartaric acid chelates metal ions in the water, preventing the precipitation or decomposition of ingredients and enhancing effectiveness.

[0037] 9. Reduce the surface tension of water to promote the wetting and penetration of the drug solution on the surface of the snail body, improve the contact efficiency of the active ingredients, and select low-concentration and biodegradable anionic surfactants to reduce environmental residues.

[0038] 10. Nicotinamide salt composite microspheres slowly release the main ingredient, and surfactants ensure its uniform dispersion, prolonging the effective action time. At the same time, it improves the drug penetration performance and improves the survival rate of the golden apple snail.

[0039] 11. The process parameters in the preparation process of the nicotinamide salt composite microspheres provided by the present invention, such as the stirring reaction for 1 hour, the ultrasonic frequency of 40KHZ, and the ultrasonic time of 30 minutes in step S4, indicate that under specific process parameters, the effect of inhibiting the survival rate of Pomacea canaliculata snails is better.

[0040] The present invention is a highly practical substance for inhibiting harmful snails such as golden apple snails, and at the same time, it has almost no harm to farmed animals in water bodies, which complies with the needs of aquaculture. In addition to the technical problems solved by the present invention, the technical features constituting the technical solutions, and the beneficial effects brought by the technical features of these technical solutions described above, the present invention provides a nicotinamide salt complex powder and a preparation method thereof, which can solve other technical problems, other technical features included in the technical solutions, and the beneficial effects brought by these technical features, which will be further described in detail in the specific implementation manner. DETAILED DESCRIPTION

[0041] In order to more clearly illustrate the present invention and have a clearer understanding of the technical features, purposes and beneficial effects of the present invention, the technical solution of the present invention is now described in detail below, but it should not be construed as limiting the applicable scope of the present invention.

[0042] The present invention will be further described below in conjunction with the following examples.

[0043] Example 1

[0044] A nicotinamide salt complex powder and a preparation method thereof, comprising, by weight, 50 parts of nicotinamide sulfate microspheres, 4 parts of L-tartaric acid, 4 parts of sodium tartrate, 0.6 parts of decyl glucoside, 2.2 parts of ammonium sulfate, 2.2 parts of sodium chloride, 0.2 parts of sodium citrate and 0.2 parts of ascorbic acid.

[0045] The preparation method of the nicotinamide sulfate microspheres is as follows:

[0046] S1. Weigh tea saponin, sodium isethionate and deionized water, mix them in a beaker, and mix them evenly under ultrasonic conditions of a frequency of 40 kHz and a time of 30 min to form a first mixed solution; the mass ratio of tea saponin, sodium isethionate and deionized water is 1:0.04:25.

[0047] S2. Weigh methacrylate, N,N-methylenebisacrylamide, polyethylene glycol, dibenzoyl peroxide and toluene, mix them in a beaker, and stir until uniform to form a second mixed solution; the mass ratio of methacrylate, N,N-methylenebisacrylamide, polyethylene glycol, dibenzoyl peroxide and toluene is 2.8:0.5:0.2:0.06:38.

[0048] S3. Weigh nicotinamide sulfate and deionized water, mix them in a beaker, and stir them evenly to form a nicotinamide sulfate solution. The mass ratio of nicotinamide sulfate to deionized water is 1:8.

[0049] S4, heating the first mixed solution to 45° C., adding the second mixed solution dropwise under stirring, stirring and reacting for 1 hour, then adding nicotinamide sulfate solution dropwise, and keeping the temperature for 1.5 hours. After removing the solvent under reduced pressure, nicotinamide sulfate / polyacrylate / tea saponin microspheres, i.e. nicotinamide sulfate microspheres, are obtained; the mass ratio of the first mixed solution, the second mixed solution and the nicotinamide sulfate solution is 0.6:1.3:1.

[0050] The method for preparing the nicotinamide salt complex powder comprises:

[0051] (1) Weighing nicotinamide sulfate microspheres according to weight, grinding and mixing in a mortar for 5 minutes to form a first mixture;

[0052] (2) weighing decyl glucoside, sodium chloride, and sodium tartrate according to weight and grinding and mixing in a mortar for 3 minutes to form a second mixture;

[0053] (3) Grinding and mixing the first mixed material and the second mixed material in a mortar for 7 minutes to form nicotinamide sulfate complex powder.

[0054] Example 2

[0055] A nicotinamide salt complex powder and a preparation method thereof, calculated by weight, comprising:

[0056] 70 parts of nicotinamide salt composite microspheres, 4 parts of L-tartaric acid, 4 parts of sodium tartrate, 0.2 parts of decyl glucoside and 2.5 parts of sodium chloride, 1 part of ammonium sulfate, 1 part of sodium chloride, 0.2 parts of sodium citrate and 0.2 parts of ascorbic acid.

[0057] The preparation method of the nicotinamide sulfate microspheres is as follows:

[0058] S1. Weigh tea saponin, sodium isethionate and deionized water, mix them in a beaker, and mix them evenly under ultrasonic conditions of a frequency of 40 kHz and a time of 30 min to form a first mixed solution; the mass ratio of tea saponin, sodium isethionate and deionized water is 1:0.04:25.

[0059] S2. Weigh methacrylate, N,N-methylenebisacrylamide, polyethylene glycol, dibenzoyl peroxide and toluene, mix them in a beaker, and stir until uniform to form a second mixed solution; the mass ratio of methacrylate, N,N-methylenebisacrylamide, polyethylene glycol, dibenzoyl peroxide and toluene is 2.8:0.5:0.2:0.05:35.

[0060] S3. Weigh nicotinamide sulfate and deionized water, mix them in a beaker, and stir evenly to form a nicotinamide sulfate solution; the mass ratio of nicotinamide sulfate to deionized water is 1:7.

[0061] S4, heating the first mixed solution to 50° C., adding the second mixed solution dropwise under stirring, stirring and reacting for 1 hour, then dropping nicotinamide sulfate solution, and continuing to keep warm for 1 hour. After removing the solvent under reduced pressure, nicotinamide sulfate / polyacrylate / tea saponin microspheres, i.e. nicotinamide sulfate microspheres, are obtained; the mass ratio of the first mixed solution, the second mixed solution and the nicotinamide sulfate solution is 0.6:1.2:1.

[0062] The method for preparing the above-mentioned nicotinamide salt complex powder comprises:

[0063] (1) Weighing nicotinamide sulfate microspheres and sodium isethionate in parts by weight, grinding and mixing in a mortar for 6 minutes to form a first mixture;

[0064] (2) weighing decyl glucoside, ammonium sulfate, sodium chloride, and sodium tartrate according to weight, grinding and mixing in a mortar for 4 minutes to form a second mixture;

[0065] (3) Grinding and mixing the first mixed material and the second mixed material in a mortar for 7 minutes to form nicotinamide salt complex powder.

[0066] Example 3

[0067] A nicotinamide salt complex powder and a preparation method thereof, comprising, by weight, 80 parts of nicotinamide hydrochloride microspheres, 6 parts of L-tartaric acid, 5 parts of sodium tartrate, 1 part of decyl glucoside, 3 parts of ammonium sulfate, 3 parts of sodium chloride, 1 part of sodium citrate and 1 part of ascorbic acid.

[0068] The preparation method of the nicotinamide sulfate microspheres is as follows:

[0069] S1. Weigh tea saponin, sodium isethionate and deionized water, mix them in a beaker, and mix them evenly under ultrasonic conditions of a frequency of 40 kHz and a time of 30 min to form a first mixed solution; the mass ratio of tea saponin to deionized water is 1:0.04:35.

[0070] S2. Weigh methacrylate, N,N-methylenebisacrylamide, polyethylene glycol, dibenzoyl peroxide and toluene, mix them in a beaker, and stir until uniform to form a second mixed solution; the mass ratio of methacrylate, N,N-methylenebisacrylamide, polyethylene glycol, dibenzoyl peroxide and toluene is 2.2:0.6:0.2:0.05:40.

[0071] S3. Weigh nicotinamide sulfate and deionized water, mix them in a beaker, and stir evenly to form a nicotinamide sulfate solution; the mass ratio of nicotinamide sulfate to deionized water is 1:8.

[0072] S4, heating the first mixed solution to 45° C., adding the second mixed solution dropwise under stirring, stirring and reacting for 1 hour, then dropping the nicotinamide sulfate solution, and continuing to keep warm for 2 hours. After removing the solvent under reduced pressure, nicotinamide sulfate / polyacrylate / tea saponin microspheres, i.e., nicotinamide sulfate microspheres, are obtained; the mass ratio of the first mixed solution, the second mixed solution, and the nicotinamide sulfate solution is 0.7:1.3:1.

[0073] The preparation method of the nicotinoanilide salt complex powder comprises: (1) weighing nicotinoanilide sulfate microspheres and sodium isethionate in parts by weight, grinding and mixing them in a mortar for 7 minutes to form a first mixture; (2) weighing sodium chloride and sodium tartrate in parts by weight, grinding and mixing them in a mortar for 4 minutes to form a second mixture; (3) grinding and mixing the first mixture and the second mixture in a mortar for 8 minutes to form a nicotinoanilide salt complex powder.

[0074] Example 4

[0075] A nicotinamide salt complex powder and a preparation method thereof, comprising, by weight, 80 parts of nicotinamide sulfate microspheres, 5 parts of L-tartaric acid, 2 parts of sodium tartrate, 0.2 parts of decyl glucoside, 1 part of ammonium sulfate, 1 part of sodium chloride, 1 part of sodium citrate and 1 part of ascorbic acid.

[0076] The preparation method of the nicotinamide sulfate microspheres is as follows:

[0077] S1. Weigh tea saponin, sodium isethionate and deionized water, mix them in a beaker, and mix them evenly under ultrasonic conditions of a frequency of 40 kHz and a time of 30 min to form a first mixed solution; the mass ratio of tea saponin, sodium isethionate and deionized water is 1:0.04:20.

[0078] S2. Weigh methacrylate, N,N-methylenebisacrylamide, polyethylene glycol, dibenzoyl peroxide and toluene, mix them in a beaker, and stir until uniform to form a second mixed solution; the mass ratio of methacrylate, N,N-methylenebisacrylamide, polyethylene glycol, dibenzoyl peroxide and toluene is 1.8:0.4:0.1:0.04:30.

[0079] S3. Weigh nicotinamide sulfate and deionized water, mix them in a beaker, and stir evenly to form a hydrogen persulfate complex salt solution; the mass ratio of nicotinamide sulfate to deionized water is 1:5.

[0080] S4, heating the first mixed solution to 45° C., adding the second mixed solution dropwise under stirring, stirring and reacting for 1 hour, then adding nicotinamide sulfate solution dropwise, and continuing to keep warm for 1 hour. After removing the solvent under reduced pressure, nicotinamide sulfate / polyacrylate / tea saponin microspheres, i.e., nicotinamide sulfate microspheres, are obtained; the mass ratio of the first mixed solution, the second mixed solution, and the nicotinamide sulfate solution is 0.5:1.2:1.

[0081] The method for preparing the nicotinamide salt complex powder comprises:

[0082] (1) Weighing nicotinamide sulfate microspheres according to weight, grinding and mixing in a mortar for 3 minutes to form a first mixture;

[0083] (2) weighing decyl glucoside, sodium chloride, and sodium tartrate according to weight, grinding and mixing in a mortar for 2 minutes to form a second mixture;

[0084] (3) Grinding and mixing the first mixed material and the second mixed material in a mortar for 4 minutes to form nicotinamide salt complex powder.

[0085] Example 5

[0086] A nicotinamide salt complex powder and a preparation method thereof, comprising, by weight, 80 parts of nicotinamide sulfate microspheres, 6.0 parts of L-tartaric acid, 5 parts of sodium tartrate, 1 part of decyl glucoside, 3 parts of ammonium sulfate, 3 parts of sodium chloride, 1 part of sodium citrate and 1 part of ascorbic acid.

[0087] The preparation method of the nicotinamide sulfate microspheres is as follows:

[0088] S1. Weigh tea saponin and deionized water, mix them in a beaker, and mix them evenly under ultrasonic conditions of a frequency of 40 kHz and a time of 30 minutes to form a first mixed solution; the mass ratio of tea saponin to deionized water is 1:40.

[0089] S2. Weigh methacrylate, N,N-methylenebisacrylamide, polyethylene glycol, dibenzoyl peroxide and toluene, mix them in a beaker, and stir until uniform to form a second mixed solution; the mass ratio of methacrylate, N,N-methylenebisacrylamide, polyethylene glycol, dibenzoyl peroxide and toluene is 3.2:0.6:0.3:0.08:50.

[0090] S3. Weigh nicotinamide sulfate and deionized water, mix them in a beaker, and stir them evenly to form a nicotinamide sulfate solution; the mass ratio of nicotinamide sulfate to deionized water is 1:10.

[0091] S4. The first mixed solution is heated to 50°C, and the second mixed solution is added dropwise under stirring. After stirring for 1 hour, the nicotinamide sulfate solution is added dropwise, and the temperature is kept for 2 hours. After the solvent is removed under reduced pressure, nicotinamide sulfate microspheres are obtained.

[0092] The method for preparing the nicotinamide salt complex powder comprises:

[0093] (1) Weighing nicotinamide sulfate microspheres according to weight, grinding and mixing in a mortar for 3 minutes to form a first mixture;

[0094] (2) weighing decyl glucoside, sodium chloride, and sodium tartrate according to weight, grinding and mixing in a mortar for 2 minutes to form a second mixture;

[0095] (3) Grinding and mixing the first mixed material and the second mixed material in a mortar for 4 minutes to form nicotinamide salt complex powder.

[0096] Example 6

[0097] A nicotinamide salt complex powder and a preparation method thereof, comprising, by weight, 50 parts of nicotinamide sulfate microspheres, 3.8 parts of L-tartaric acid, 4 parts of sodium tartrate, 0.6 parts of decyl glucoside, 2.2 parts of ammonium sulfate, 2.2 parts of sodium chloride, 0.2 parts of sodium citrate and 0.2 parts of ascorbic acid.

[0098] The preparation method of the nicotinamide sulfate microspheres is as follows:

[0099] S1. Weigh tea saponin, sodium isethionate and deionized water, mix them in a beaker, and mix them evenly under ultrasonic conditions of a frequency of 40 kHz and a time of 30 min to form a first mixed solution; the mass ratio of tea saponin, sodium isethionate and deionized water is 1:30.

[0100] S2. Weigh methacrylate, N,N-methylenebisacrylamide, polyethylene glycol, dibenzoyl peroxide and toluene, mix them in a beaker, and stir until uniform to form a second mixed solution; the mass ratio of methacrylate, N,N-methylenebisacrylamide, polyethylene glycol, dibenzoyl peroxide and toluene is 2.8:0.5:0.2:0.06:38.

[0101] S3. Weigh nicotinamide sulfate and deionized water, mix them in a beaker, and stir them evenly to form a nicotinamide sulfate solution. The mass ratio of nicotinamide sulfate to deionized water is 1:8.

[0102] S4, heating the first mixed solution to 45° C., adding the second mixed solution dropwise under stirring, stirring and reacting for 1 hour, then adding nicotinamide sulfate solution dropwise, and keeping the temperature for 1.5 hours. After removing the solvent under reduced pressure, nicotinamide sulfate / polyacrylate / tea saponin microspheres, i.e. nicotinamide sulfate microspheres, are obtained; the mass ratio of the first mixed solution, the second mixed solution and the nicotinamide sulfate solution is 0.6:1.3:1.

[0103] The preparation method of the nicotinoanilide salt complex powder comprises: (1) weighing nicotinoanilide sulfate microspheres according to weight, grinding and mixing in a mortar for 5 minutes to form a first mixture; (2) weighing decyl glucoside, sodium chloride, and sodium tartrate according to weight, grinding and mixing in a mortar for 3 minutes to form a second mixture; (3) grinding and mixing the first mixture and the second mixture in a mortar for 7 minutes to form a nicotinoanilide sulfate complex powder.

[0104] Comparative Example 1

[0105] A nicotinamide salt composite powder and a preparation method thereof, compared with Example 1, the difference is that the preparation method of nicotinamide sulfate microspheres is different. Specifically:

[0106] A nicotinamide sulfate complex powder comprises, by weight, 50 parts of nicotinamide sulfate microspheres, 4 parts of L-tartaric acid, 4 parts of sodium tartrate, 0.6 parts of decyl glucoside, 2.2 parts of ammonium sulfate, 2.2 parts of sodium chloride, 0.2 parts of sodium citrate and 0.2 parts of ascorbic acid.

[0107] The preparation method of the nicotinamide sulfate microspheres is as follows:

[0108] S1. Weigh sodium hydroxyethyl sulfonate and deionized water, mix them in a beaker, and mix them evenly under ultrasonic conditions at a mixing frequency of 40 kHz for 30 minutes to form a first mixed solution; the mass ratio of sodium hydroxyethyl sulfonate to deionized water is 0.04:25.

[0109] S2. Weigh methacrylate, N,N-methylenebisacrylamide, polyethylene glycol, dibenzoyl peroxide and toluene, mix them in a beaker, and stir until uniform to form a second mixed solution; the mass ratio of methacrylate, N,N-methylenebisacrylamide, polyethylene glycol, dibenzoyl peroxide and toluene is 2.8:0.5:0.2:0.06:38.

[0110] S3. Weigh nicotinamide sulfate and deionized water, mix them in a beaker, and stir them evenly to form a nicotinamide sulfate solution; the mass ratio of nicotinamide sulfate to deionized water is 1:8.

[0111] S4, heating the first mixed solution to 45° C., adding the second mixed solution dropwise under stirring, stirring and reacting for 1 hour, then adding nicotinamide sulfate solution dropwise, and keeping the temperature for 1.5 hours. After removing the solvent under reduced pressure, nicotinamide sulfate / polyacrylate microspheres, i.e., potassium persulfate composite microspheres, are obtained; the mass ratio of the first mixed solution, the second mixed solution and the nicotinamide sulfate solution is 0.6:1.3:1.

[0112] The method for preparing the above-mentioned nicotinamide salt complex powder comprises:

[0113] (1) weighing nicotinamide sulfate microspheres according to weight, grinding and mixing in a mortar for 5 minutes to form a first mixture;

[0114] (2) weighing decyl glucoside, sodium chloride, and sodium tartrate according to weight, grinding and mixing in a mortar for 3 minutes to form a second mixture;

[0115] (3) Grinding and mixing the first mixed material and the second mixed material in a mortar for 7 minutes to form nicotinamide salt complex powder.

[0116] Comparative Example 2

[0117] A nicotinamide salt complex powder and a preparation method thereof, compared with Example 2, the difference is: the nicotinamide sulfate microspheres are replaced by nicotinamide sulfate complex salt and tea saponin converted in proportion. Specifically:

[0118] 65 parts of nicotinamide complex salt, 5 parts of tea saponin, 4 parts of L-tartaric acid, 4 parts of sodium tartrate, 0.2 parts of decyl glucoside and 2.5 parts of sodium chloride, 1 part of ammonium sulfate, 1 part of sodium chloride, 0.2 parts of sodium citrate and 0.2 parts of ascorbic acid.

[0119] The method for preparing the above-mentioned nicotinamide salt complex powder comprises:

[0120] (1) Weighing nicotinamide composite salt and tea saponin according to weight, grinding and mixing in a mortar for 6 minutes to form a first mixture;

[0121] (2) weighing decyl glucoside, ammonium sulfate, sodium chloride, and sodium tartrate according to weight, grinding and mixing in a mortar for 4 minutes to form a second mixture;

[0122] (3) Grinding and mixing the first mixed material and the second mixed material in a mortar for 7 minutes to form nicotinamide salt complex powder.

[0123] Comparative Example 3

[0124] A nicotinamide salt composite powder and a preparation method thereof, compared with Example 2, the difference is: potassium persulfate composite microspheres are replaced by nicotinamide sulfate composite salt converted according to a ratio.

[0125] Specifically: the nicotinamide salt complex powder, calculated by weight, includes: 70 parts of nicotinamide salt, 4 parts of L-tartaric acid, 4 parts of sodium tartrate, 0.2 parts of decyl glucoside, 1 part of ammonium sulfate, 1 part of sodium chloride, 0.2 parts of sodium citrate, and 0.2 parts of ascorbic acid.

[0126] The method for preparing the nicotinamide salt complex powder comprises:

[0127] (1) Weighing nicotinamide sulfate and sodium isethionate according to weight, grinding and mixing in a mortar for 6 minutes to form a first mixture;

[0128] (2) weighing decyl glucoside, ammonium sulfate, sodium chloride, and sodium tartrate according to weight, grinding and mixing in a mortar for 4 minutes to form a second mixture;

[0129] (3) Grinding and mixing the first mixed material and the second mixed material in a mortar for 7 minutes to form nicotinamide salt complex powder.

[0130] In order to more clearly illustrate the content of the present invention, the dispersibility, stability and disinfection performance of the nicotinamide salt complex powder obtained in Examples 1-3 and Comparative Examples 1-3 of the present invention were tested. The results are shown in Table 1 below:

[0131]

[0132] Among them, (1) water dispersibility is to mix the product with purified water at a mass ratio of 1:250 in a 500 mL flask, shake it at 50 rpm for 1 min, and then observe the dispersion state; water stability is to seal the product in a flask after the water dispersibility is carried out, and place the flask in a dark place at a temperature of 25±2°C and a humidity of 55±5% for 72 hours, and then observe the dispersion state again.

[0133] It can be seen from Table 1 that the nicotinamide salt composite powder prepared in Examples 1-3 of the present invention not only has good dispersibility in water but also has stable performance. The nicotinamide salt composite microspheres are self-made sustained-release microspheres of the present invention. Tea saponin is used as a natural porogen, and a porous network composite material is formed by combining polymethacrylate and tea saponin as the microsphere wall. Nicotinamide salt is used as a microsphere sustained-release agent. The microspheres are porous, and not only have a faster and stronger sustained-release effect, but also can ensure the content of nicotinamide salt, but also have strong hydrophilicity, can have a good dispersion effect in water, and realize drug gradient release. Tea saponin has a certain effect on the dispersibility in water.

[0134] Comparative Example 4

[0135] A nicotinamide salt complex powder and a preparation method thereof, compared with Example 2, the difference is: the nicotinamide sulfate microspheres are replaced by nicotinamide sulfate complex salt and tea saponin converted according to a ratio, and sodium citrate and ascorbic acid are not added. Specifically:

[0136] A nicotinamide salt complex powder and a preparation method thereof, comprising, by weight, 65 parts of nicotinamide sulfate complex salt, 5 parts of tea saponin, 4 parts of L-tartaric acid, 4 parts of sodium tartrate, 0.2 parts of decyl glucoside and 1 part of sodium chloride.

[0137] The preparation method of the above-mentioned nicotinamide salt complex powder and the preparation method thereof comprises:

[0138] (1) Weighing nicotinamide composite salt and tea saponin according to weight, grinding and mixing in a mortar for 5 minutes to form a first mixture;

[0139] (2) weighing decyl glucoside, ammonium sulfate, sodium chloride, and sodium tartrate according to weight, grinding and mixing in a mortar for 3 minutes to form a second mixture;

[0140] (3) Grinding and mixing the first mixed material and the second mixed material in a mortar for 7 minutes to form nicotinamide salt complex powder.

[0141] Comparative Example 5

[0142] A nicotinamide salt complex powder and a preparation method thereof, comprising, by weight: 70 parts of nicotinamide sulfate microspheres, 4 parts of L-tartaric acid, 4 parts of sodium tartrate, 0.2 parts of decyl glucoside, 1 part of sodium chloride, 1 part of ammonium sulfate, and 0.2 parts of sodium citrate. Compared with Example 2, no ascorbic acid is added.

[0143] The preparation method of the nicotinamide sulfate microspheres is as follows:

[0144] S1. Weigh tea saponin, sodium isethionate and deionized water, mix them in a beaker, and mix them evenly under ultrasonic conditions of a frequency of 40 kHz and a time of 30 min to form a first mixed solution; the mass ratio of tea saponin, sodium isethionate and deionized water is 1:0.04:25.

[0145] S2. Weigh methacrylate, N,N-methylenebisacrylamide, polyethylene glycol, dibenzoyl peroxide and toluene, mix them in a beaker, and stir until uniform to form a second mixed solution; the mass ratio of methacrylate, N,N-methylenebisacrylamide, polyethylene glycol, dibenzoyl peroxide and toluene is 2.8:0.5:0.2:0.05:35.

[0146] S3. Weigh nicotinamide sulfate and deionized water, mix them in a beaker, and stir them evenly to form a nicotinamide sulfate solution; the mass ratio of nicotinamide sulfate to deionized water is 1:7.

[0147] S4, heating the first mixed solution to 50° C., adding the second mixed solution dropwise under stirring, stirring and reacting for 1 hour, then dropping the nicotinamide sulfate solution, and continuing to keep the temperature for 1 hour. After removing the solvent under reduced pressure, nicotinamide sulfate / polyacrylate / tea saponin microspheres, i.e., nicotinamide sulfate microspheres, are obtained; the mass ratio of the first mixed solution, the second mixed solution, and the nicotinamide sulfate solution is 0.6:1.2:1.

[0148] The method for preparing the above-mentioned nicotinamide salt complex powder comprises:

[0149] (1) Weighing nicotinamide sulfate microspheres and sodium isethionate in parts by weight, grinding and mixing in a mortar for 6 minutes to form a first mixture;

[0150] (2) weighing decyl glucoside, sodium chloride, sodium tartrate, and sodium citrate according to weight, grinding and mixing in a mortar for 4 minutes to form a second mixture;

[0151] (3) Grinding and mixing the first mixed material and the second mixed material in a mortar for 5 minutes to form nicotinamide salt complex powder.

[0152] Comparative Example 6

[0153] A nicotinamide salt complex powder and a preparation method thereof, comprising, by weight: 70 parts of nicotinamide sulfate microspheres, 4 parts of L-tartaric acid, 4 parts of sodium tartrate, 0.2 parts of decyl glucoside, 2.5 parts of sodium chloride, 0.2 parts of sodium citrate, and 0.2 parts of ascorbic acid. Compared with Example 2, no ammonium sulfate is added.

[0154] The preparation method of the nicotinamide sulfate microspheres is as follows:

[0155] S1. Weigh tea saponin, sodium isethionate and deionized water, mix them in a beaker, and mix them evenly under ultrasonic conditions of a frequency of 40 kHz and a time of 30 min to form a first mixed solution; the mass ratio of tea saponin, sodium isethionate and deionized water is 1:0.04:25.

[0156] S2. Weigh methacrylate, N,N-methylenebisacrylamide, polyethylene glycol, dibenzoyl peroxide and toluene, mix them in a beaker, and stir until uniform to form a second mixed solution; the mass ratio of methacrylate, N,N-methylenebisacrylamide, polyethylene glycol, dibenzoyl peroxide and toluene is 2.8:0.5:0.2:0.05:35.

[0157] S3. Weigh nicotinamide sulfate and deionized water, mix them in a beaker, and stir them evenly to form a nicotinamide sulfate solution; the mass ratio of nicotinamide sulfate to deionized water is 1:7.

[0158] S4, heating the first mixed solution to 50° C., adding the second mixed solution dropwise under stirring, stirring and reacting for 1 hour, then dropping the nicotinamide sulfate solution, and continuing to keep the temperature for 1 hour. After removing the solvent under reduced pressure, nicotinamide sulfate / polyacrylate / tea saponin microspheres, i.e., nicotinamide sulfate microspheres, are obtained; the mass ratio of the first mixed solution, the second mixed solution, and the nicotinamide sulfate solution is 0.6:1.2:1.

[0159] The method for preparing the above-mentioned nicotinamide salt complex powder comprises:

[0160] (1) Weighing nicotinamide sulfate microspheres and sodium isethionate in parts by weight, grinding and mixing in a mortar for 6 minutes to form a first mixture;

[0161] (2) weighing decyl glucoside, sodium chloride, and sodium tartrate according to weight, grinding and mixing in a mortar for 4 minutes to form a second mixture;

[0162] (3) Grinding and mixing the first mixed material and the second mixed material in a mortar for 5 minutes to form nicotinamide salt complex powder.

[0163] The survival rate of the snails inhibited by the preparations of Example 1, Example 2, Example 3 and Comparative Example 4, Comparative Example 5 and Comparative Example 6 was tested, and the field efficacy experiment on the rice field Pomacea canaliculata was carried out using the nicotinamide salt complex powder prepared in the above examples and comparative examples. The number of live and dead snails in each area was checked on the 1st, 3rd, 7th and 14th day after the application and after the rain, and the mortality rate of Pomacea canaliculata was calculated. Mortality rate = (number of live snails before treatment - number of live snails after treatment) / number of live snails before treatment × 100%.

[0164] The results are shown in Table 2 below:

[0165]

[0166]

[0167] The above data show that the mortality rate of field snails is stable and continuous, and the nicotinamide salt composite microspheres have exerted their characteristics of sustained drug release, while also improving the stability of the drug. The nicotinamide salt composite microspheres are self-made sustained-release microspheres of the present invention, with tea saponin as a natural porogen, and a porous network composite material formed by combining polymethacrylate and tea saponin as the microsphere wall, and nicotinamide salt as a microsphere sustained-release agent. The microspheres are porous, not only the sustained-release effect is faster and stronger, and the content of nicotinamide salt can be guaranteed, but also it has strong hydrophilicity, and can have a good dispersion effect in water, realizing drug gradient release, and its snail-killing persistence is higher than that of the nicotinamide composite preparation of Comparative Example 4 that does not use the microsphere process.

[0168] Sodium isethionate is added during the synthesis of the nicotinamide salt composite microspheres of the present invention, and the addition of a surfactant to the sodium isethionate enhances the synthesis of the various raw materials of the microspheres. In the process of preparing the nicotinamide salt composite microspheres of the present invention, unlike conventional methods, nicotinamide sulfate is added during the semi-molding process of the microspheres, which not only avoids the consumption of nicotinamide salt during the polymerization of methacrylate, but also allows it to be more conveniently introduced into the pores of the microspheres, without being wrapped by the polymer and affecting the precipitation of nicotinamide salt.

[0169] In addition, due to the compounding of tea saponin powder, tea saponin powder itself has a strong snail-killing effect, so the snail-killing effect of the nicotinamide salt complex powder prepared by the present invention is also more excellent. The sustained-release technology is used to control the release rate, prolong the efficacy, reduce the frequency of application, reduce the risk of exposure to non-target organisms, and reflect environmental protection.

[0170] From Comparative Examples 5-6, it can be seen that while ammonium sulfate and ascorbic acid improve the stability of the drug, they also have a certain effect in inhibiting the survival rate of Pomacea canaliculata. The combination of ammonium sulfate, ascorbic acid and sodium chloride can inhibit the production of snails by regulating the growth of aquatic plants, algae and microorganisms in the breeding environment during the snail killing process.

[0171] L-tartaric acid and sodium tartrate are used to form a buffer system to ensure that nicotinamide salt works within an appropriate pH range. Tartaric acid chelates metal ions in water to prevent precipitation or decomposition of ingredients and enhance effectiveness. The surface tension of water is reduced to promote wetting and penetration of the drug solution on the surface of the snail body, improve the contact efficiency of the active ingredients, and select low-concentration and biodegradable anionic surfactants to reduce environmental residues. Nicotinamide salt composite microspheres slowly release the main ingredient, and the surfactant ensures its uniform dispersion, prolonging the effective action time. At the same time, it improves the drug penetration performance and improves the survival rate of the golden apple snail.

[0172] Comparative Example 7

[0173] Compared with Example 1, the difference is that in step S4, after stirring the reaction for 0.5h, nicotinamide sulfate solution is added dropwise, and the temperature is kept for 1.5h. After the solvent is removed under reduced pressure, nicotinamide sulfate / polyacrylate / tea saponin microspheres, i.e. nicotinamide sulfate microspheres, are obtained; and the mass ratio of the first mixed solution, the second mixed solution and the nicotinamide sulfate solution is 0.6:1.3:1.

[0174] Comparative Example 8

[0175] Compared with Example 1, the difference is that in step S4, after stirring the reaction for 1 hour, the ultrasonic conditions are mixed evenly at a frequency of 20 khz and a time of 30 minutes, and the other conditions remain unchanged.

[0176] The results are shown in Table 3:

[0177]

[0178]

[0179] It can be seen from Comparative Examples 7-8 of the present invention that the process parameters in the preparation process of the nicotinamide salt composite microspheres provided, such as the stirring reaction for 1h, the ultrasonic frequency of 40KHZ, and the ultrasonic time of 30min in step S4, indicate that under specific process parameters, the effect of inhibiting the survival rate of Pomacea canaliculata is better.

[0180] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit it. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the aforementioned embodiments, or replace some or all of the technical features therein with equivalents. However, these modifications or replacements do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present invention.

Claims

1. A nicotinamide salt complex powder and a preparation method thereof, characterized in that: Calculated by weight, including: Nicotinanilide salt composite microspheres 50-80 parts, 3.8-6.0 parts of L-tartaric acid, 4-5 parts of sodium tartrate, Decyl glucoside 0.2-1 part, Sodium citrate 0.2-1 part, Ascorbic acid 0.2-1 part, 1-3 parts of ammonium sulfate, 1-3 parts of sodium chloride; The nicotinamide salt composite microspheres are prepared by a method comprising the following steps: S1, weighing tea saponin powder, sodium isethionate and deionized water, mixing them evenly under ultrasonic conditions to form a first mixed solution; S2, weighing methacrylate, N,N-methylenebisacrylamide, polyethylene glycol, dibenzoyl peroxide and toluene, mixing them in a beaker, and stirring until uniform to form a second mixed solution; S3, weighing nicotinamide salt and deionized water, mixing, and stirring evenly to form a nicotinamide salt solution; S4, heating the first mixed solution to 45-50° C., adding the second mixed solution dropwise under stirring, stirring and reacting for 1 hour, then adding nicotinamide salt solution dropwise, and keeping the temperature for 1-2 hours. After removing the solvent under reduced pressure, nicotinamide salt / polyacrylate / tea saponin microspheres, i.e., nicotinamide salt composite microspheres, are obtained.

2. The nicotinamide salt composite powder and the preparation method thereof according to claim 1, characterized in that: The ultrasonic conditions in step S1 are a frequency of 40 kHz and a time of 30 min.

3. The nicotinamide salt composite powder and the preparation method thereof according to claim 1, characterized in that: The nicotinoanilide salt composite powder comprises, by weight, 70 parts of nicotinoanilide salt composite microspheres, 4 parts of L-tartaric acid, 4 parts of sodium tartrate, 0.2 parts of decyl glucoside, 0.2 parts of sodium citrate, 0.2 parts of ascorbic acid, 1 part of ammonium sulfate, and 1 part of sodium chloride.

4. The nicotinamide salt composite powder and the preparation method thereof according to claim 1, characterized in that: In the S1, the mass ratio of tea saponin powder, sodium isethionate and deionized water is 1:0.01-0.06:10-50.

5. The nicotinamide salt composite powder and the preparation method thereof according to claim 1, characterized in that: In S2, the mass ratio of methacrylate, N,N-methylenebisacrylamide, polyethylene glycol, dibenzoyl peroxide and toluene is 1.5-2.2:0.5-0.7:0.1-0.2:0.03-0.07:20-50.

6. The nicotinamide salt composite powder and the preparation method thereof according to claim 1, characterized in that: In S3, the nicotinamide salt is nicotinamide sulfate or nicotinamide hydrochloride.

7. The nicotinamide salt complex powder and the preparation method thereof according to claim 1, characterized in that: In S3, the mass ratio of nicotinamide salt to deionized water is 1:4-10.

8. The nicotinamide salt composite powder and the preparation method thereof according to claim 1, characterized in that: In S4, the mass ratio of the first mixed solution, the second mixed solution and the nicotinamide salt solution is 0.3-0.8:1.3-1.7:

1.

9. A method for preparing the nicotinamide salt composite powder and the preparation method thereof according to claim 1 or 2, characterized in that: include: (1) Weighing nicotinamide salt composite microspheres according to weight, grinding and mixing in a mortar for 3-8 minutes to form a first mixture; (2) Weighing decyl glucoside, ammonium sulfate, sodium citrate, ascorbic acid, sodium chloride, and sodium tartrate according to weight, grinding and mixing in a mortar for 2-5 minutes to form a second mixture; (3) Grinding and mixing the first mixture and the second mixture in a mortar for 4-10 minutes to form a nicotinamide salt composite powder.

10. A method for preparing the nicotinamide salt complex powder and the preparation method thereof according to claim 1 or 2, characterized in that: include: (1) Weighing nicotinamide salt composite microspheres according to weight, grinding and mixing in a mortar for 5 minutes to form a first mixture; (2) Weighing decyl glucoside, sodium citrate, ascorbic acid, ammonium sulfate, sodium chloride, and sodium tartrate according to weight, grinding and mixing in a mortar for 4 minutes to form a second mixture; (3) Grinding and mixing the first mixture and the second mixture in a mortar for 6 minutes to form a nicotinamide salt composite powder.

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