A compound fumigation-type mildew inhibitor, its preparation method and application

Abstract

This invention discloses a compound fumigation-type mold inhibitor, its preparation method, and its application. The compound fumigation-type mold inhibitor comprises the following raw materials: trans-anestinol; carvacrol; linalool; terpineol; eugenol; terpineol; and auxiliary reagents. This mold inhibitor is made from natural plant essential oils, is stable, safe, green, highly efficient, and pollution-free, and has an aromatic odor. It has a strong inhibitory effect on Aspergillus flavus and Penicillium in grains, and also inhibits their toxin synthesis. It is a relatively ideal mold inhibitor for grain storage and has good application prospects in grain storage.

Description

Technical Field

[0001] This application relates to the field of grain storage, and more particularly to a compound fumigation-type antifungal agent, its preparation method, and its application in this field. Background Technology

[0002] my country is a major grain-producing country, and its total grain output is increasing year by year. However, grain is highly susceptible to factors such as temperature, humidity, moisture content, and oxygen levels during storage. After grain is stored, it generates heat through stacking and respiration, promoting the growth and reproduction of microorganisms and leading to mold or toxic contamination. This not only causes huge economic losses but also threatens the health of humans and livestock. Therefore, preventing mold has become an indispensable part of grain storage.

[0003] In recent years, countries worldwide have placed increasing emphasis on grain storage, and advanced methods such as controlled atmosphere storage, low-temperature storage, circulating fumigation, and biological mold and insect control have been applied in practical production. Among these, biological mold and insect control methods overcome the high requirements for hardware equipment, offering safety, non-toxicity, and high efficiency. Therefore, while ensuring the accuracy of stored grain quantity, they also guarantee good grain quality, playing a crucial role in preventing grain mold. The most effective way to prevent grain from molding during storage is to add mold inhibitors. Recent research both domestically and internationally indicates that mold inhibitors have evolved from contact-type to aerosol-type, and from single-type to compound-type. Compound mold inhibitors combine different antibacterial spectrum inhibitors with synergistic effects in specific proportions, expanding their applicability and enhancing their anti-mold effect. Summary of the Invention

[0004] The purpose of this invention is to provide a compound fumigation-type antifungal agent. This antifungal agent is made from natural plant essential oils, is stable, safe, green, efficient, and pollution-free, and has an aromatic odor. It has a strong inhibitory effect on Aspergillus flavus and Penicillium in grains, and also inhibits their toxin synthesis. It is a relatively ideal antifungal agent for grain storage and has good application prospects in grain storage.

[0005] To achieve the above objectives, the present invention adopts the following technical solution:

[0006] A compound fumigation-type antifungal agent includes the following raw materials: trans-anestinol; carvacrol; linalool; terpineol; eugenol; terpineol; and auxiliary reagents.

[0007] The auxiliary reagents include hexanal, heptanal, 2-heptenal, 2-hexenal, nonanol, and octanol.

[0008] Preferably, the above-mentioned compound fumigation-type antifungal agent comprises the following raw materials in parts by weight: 16-17 parts trans-anetinoside; 25-27 parts carvacrol; 12-14 parts linalool; 12-14 parts terpineol; 16-18 parts eugenol; 8-9 parts terpineol; 0.1-0.4 parts hexanal; 0.5-2 parts heptanal; 1-3 parts 2-heptenal; 0.5-2 parts 2-hexenal; 0.3-1 part nonanol; and 0.3-1 part octanol.

[0009] Preferably, the above-mentioned compound fumigation-type antifungal agent comprises the following raw materials in parts by weight: 17 parts trans-anetinoside; 26 parts carvacrol; 13 parts linalool; 13 parts terpineol; 17 parts eugenol; 9 parts terpineol; 0.3 parts hexanal; 1 part heptanal; 1.5 parts 2-heptenal; 1 part 2-hexenal; 0.5 parts nonanol; and 0.7 parts octanol.

[0010] Preferably, the above-mentioned compound fumigation-type antifungal agent comprises the following raw materials in parts by weight: 16.7 parts trans-anetinoside; 25 parts carvacrol; 12.6 parts linalool; 12.6 parts terpineol; 16.7 parts eugenol; 8.4 parts terpineol; 0.4 parts hexanal; 1.6 parts heptanal; 2.8 parts 2-heptenal; 1.6 parts 2-hexenal; 0.8 parts nonanol; and 0.8 parts octanol.

[0011] Preferably, the above-mentioned compound fumigation-type antifungal agent comprises the following raw materials in parts by weight: 16.5 parts trans-anetinoside; 26.5 parts carvacrol; 13.9 parts linalool; 13.6 parts terpineol; 17.6 parts eugenol; 8.8 parts terpineol; 0.2 parts hexanal; 0.6 parts heptanal; 1.1 parts 2-heptenal; 0.6 parts 2-hexenal; 0.3 parts nonanol; and 0.3 parts octanol.

[0012] Preferably, the above-mentioned compound fumigation-type antifungal agent comprises the following raw materials in parts by weight: 16.3 parts trans-anetinoside; 26.6 parts carvacrol; 12.9 parts linalool; 13 parts terpineol; 17.3 parts eugenol; 9 parts terpineol; 0.4 parts hexanal; 1 part heptanal; 1.5 parts 2-heptenal; 1 part 2-hexenal; 0.5 parts nonanol; and 0.5 parts octanol.

[0013] The present invention also discloses a method for preparing the above-mentioned compound fumigation type antifungal agent, comprising the following steps: taking trans-anestochrome, carvacrol, camphor alcohol, terpineol, eugenol and terpineol according to the weight parts, mixing them thoroughly, and then adding hexanal, heptanal, 2-heptenal, 2-hexenal, nonanol and octanol according to the weight parts ratio.

[0014] The beneficial effects of this invention are:

[0015] The antifungal agent of this invention achieves its antibacterial and antifungal effects through steam fumigation, with a minimum inhibitory concentration (MIC) of 0.159 μL / mL. The main components of this antifungal agent—trans-anisole, linalool, terpineol, and terpineol—have MICs of 0.286 μL / mL, 0.571 μL / mL, 0.51 μL / mL, and 0.735 μL / mL, respectively. This indicates that each single component or different components in the above-mentioned ratio can achieve a synergistic effect, significantly inhibiting Aspergillus and Penicillium, which are common in grain storage, exhibiting broad-spectrum antibacterial activity and good antifungal effect. This compound fumigation-type antifungal agent can be used directly, dissolved in other liquid solvents, adsorbed onto other solid carriers, or formulated into a slow-release product for use. Since each component of this antifungal agent is a major component of natural plant essential oils, it is widely available, green, and pollution-free, leaving no toxic residues on grains and their processed products, thus enhancing its sustainability. Furthermore, it can be used at any time; applying it before grain becomes moldy can achieve a preventative effect, and applying it promptly after mold has appeared can also inhibit its growth. In addition, the mold inhibitor of this invention can also be added to grain storage insect repellents, achieving a dual effect of insect and mold prevention. Attached Figure Description

[0016] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on the provided drawings without creative effort.

[0017] Figure 1 The colony morphology of Aspergillus flavus after 7 days of treatment with the antifungal agent in Example 4 is shown. Detailed Implementation

[0018] The technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0019] The composite collector of the present invention has strong water solubility and good efficacy. Compared with conventional hydrocarbon oil collectors, the composite collector prepared by the present invention has better collection performance, stronger anti-mudification ability, more stable properties, and the foam is non-sticky, easy to dissipate, highly adaptable, fast flotation speed, and convenient to use.

[0020] Example 1:

[0021] A compound fumigation-type antifungal agent is prepared by weighing the following raw materials in the indicated weight ratios: 16.3 parts trans-anetinoside; 26.6 parts carvacrol; 12.9 parts linalool; 13 parts terpineol; 17.3 parts eugenol; 9 parts terpineol; 0.4 parts hexanal; 1 part heptanal; 1.5 parts 2-heptenal; 1 part 2-hexenal; 0.5 parts nonanol; and 0.5 parts octanol. The materials are thoroughly mixed to prepare the compound fumigation-type antifungal agent.

[0022] The inhibitory effect of this compound fumigation-type mold inhibitor on Aspergillus flavus during grain storage:

[0023] Select plump wheat kernels free from mold contamination, disinfect their surface with a 1% sodium hypochlorite solution, rinse 3-5 times with sterile distilled water, dry under sterile conditions, and then adjust the moisture content to 20%. Use a 10% sodium hypochlorite solution for surface disinfection. 7 A suspension of Aspergillus flavus spores (spores / g) was inoculated into wheat grains, and the surface moisture was blotted dry with sterile filter paper. For each fumigation concentration, 300g of the treated wheat grains were evenly placed in a sterile glass bottle, and 0μL, 100μL, 200μL, 300μL, 400μL, and 500μL of the corresponding antifungal agent were added to the sterile filter paper on the inner wall of the bottle cap. The bottle was then sealed with the cap and placed in a constant temperature incubator at 28±1℃ for 6 weeks to simulate storage. The fungal count of each grain sample was then measured. First, 25g of wheat grains were immersed in a 500ml flask containing 225ml of sterile distilled water and shaken on a plate shaker for 30 minutes to completely wash away the mold on the surface of the wheat grains. Each sample solution was diluted 10% with sterile distilled water. 2 -10 6 Dilute 10 times, take the diluted product 3 -10 5 The sample solutions were then used for subsequent experiments. Next, 1 mL of each dilution was inoculated into a modified Czapek's medium prepared with reagents including sodium nitrate, dipotassium hydrogen phosphate, magnesium sulfate, potassium chloride, ferrous sulfate, sucrose, and sodium chloride, and incubated at 28°C for 5 days. Aspergillus flavus was then counted. Each experiment was repeated three times.

[0024] When the sample solution is diluted by a factor of 10... 3 When 0 μL, 100 μL, 200 μL, 300 μL, 400 μL, and 500 μL of antifungal agent were added, the mean colony counts of Aspergillus flavus in the petri dishes were 131.25, 127.75, 1225, 11.25, 8.25, and 8.25, respectively; when the sample solution was diluted 10... 4 When the antifungal agents of different dilution levels were added, the average colony counts in the petri dishes were 33.75, 26.75, 4.25, 3, 2.25, and 0.5, respectively; when the sample solution was diluted 10 times... 5 At that time, the average colony counts in each petri dish were 12.75, 8, 0.75, 0.25, 0, and 0, respectively.

[0025] Experimental results showed that the amount of Aspergillus flavus in the petri dish was negatively correlated with the amount of antifungal agent added and the dilution factor of the sample solution. When the amount of antifungal agent added was 400 μL and the dilution factor of the sample solution was 10... 5 At this time, the growth of Aspergillus flavus in the petri dish can be completely inhibited.

[0026] The results show that for 300g of wheat, using 400μL of the liquid antifungal agent at this ratio can completely inhibit Aspergillus flavus contamination of wheat grains, while other concentrations show varying degrees of inhibitory effects on Aspergillus flavus. The results indicate that this compound antifungal agent, under steam fumigation, has a significant inhibitory effect on Aspergillus flavus in wheat grains, and the number of moldy wheat grains decreases in a dose-dependent manner. This demonstrates its promising application prospects.

[0027] Example 2:

[0028] A compound fumigation-type antifungal agent is prepared by weighing the following raw materials in the indicated weight ratios: 16.5 parts trans-anetinoside; 26.5 parts carvacrol; 13.9 parts linalool; 13.6 parts terpineol; 17.6 parts eugenol; 8.8 parts terpineol; 0.2 parts hexanal; 0.6 parts heptanal; 1.1 parts 2-heptenal; 0.6 parts 2-hexenal; 0.3 parts nonanol; and 0.3 parts octanol. These are thoroughly mixed to prepare a compound liquid antifungal agent for grain storage.

[0029] The inhibitory effect of this compound fumigation-type mold inhibitor on Aspergillus flavus in feed storage:

[0030] Take 200 kg of wheat grains with a moisture content of 20% (the wheat treatment method is the same as in Example 1), of which 100 kg is placed in a container with a volume of 0.3 m³. 3 The container was subjected to high-concentration fumigation for 24 hours at 28°C using a circulating fumigation device, with a fumigation concentration of 15 mL / m³. 3 Another 100 kg was used as a blank control, and both groups were stored under the same conditions. Mold growth was checked after 30 days. The control group, which did not use this invention, had a noticeable musty smell, a mold rate of 6.62%, and a mold loss of 6.62 kg. The treatment group using this invention had a 0% mold rate and a 0 kg mold loss. Therefore, the compound fumigation-type mold inhibitor of this invention shows good promise for specific applications in grain storage.

[0031] Example 3:

[0032] A compound fumigation-type antifungal agent is made from the following raw materials in parts by weight: 16.7 parts trans-anetinoside; 25 parts carvacrol; 12.6 parts linalool; 12.6 parts terpineol; 16.7 parts eugenol; 8.4 parts terpineol; 0.4 parts hexanal; 1.6 parts heptanal; 2.8 parts 2-heptenal; 1.6 parts 2-hexenal; 0.8 parts nonanol; and 0.8 parts octanol. These are thoroughly mixed to prepare a compound liquid antifungal agent for feed.

[0033] The inhibitory effect of this compound fumigation-type mold inhibitor on Aspergillus flavus in feed storage:

[0034] Take 200 kg of grain feed (wheat treatment method is the same as in Example 1), of which 100 kg is placed in a container with a volume of 0.3 m³. 3 The container was subjected to high-concentration fumigation for 24 hours at 28°C through a circulating fumigation pipe, with a fumigation concentration of 15 mL / m³. 3 Another 100 kg was used as a blank control, and both groups were stored under the same conditions. Mold growth was checked after 30 days. The control group, which did not use this invention, had a noticeable musty odor, a mold rate of 6.62%, and a mold loss of 6.62 kg. The treatment group using this invention had a 0% mold rate and a 0 kg mold loss. Therefore, the compound fumigation-type mold inhibitor of this invention also shows good application prospects in feed storage.

[0035] Example 4

[0036] A compound fumigation-type antifungal agent is made from the following raw materials in parts by weight: 17 parts trans-anetinoside; 26 parts carvacrol; 13 parts linalool; 13 parts terpineol; 17 parts eugenol; 9 parts terpineol; 0.3 parts hexanal; 1 part heptanal; 1.5 parts 2-heptenal; 1 part 2-hexenal; 0.5 parts nonanol; and 0.7 parts octanol. These are thoroughly mixed to prepare a compound liquid antifungal agent for feed. At this compound ratio, the liquid antifungal agent achieves good antifungal effects and has a more acceptable aromatic odor with minimal residual odor.

[0037] Different ratios of antifungal agents were mixed and their sensory characteristics were analyzed. A sensory evaluation panel of 10 sensory evaluators (5 men and 5 women, aged 20-30) was formed. The sensory characteristics were examined by the panel members. The panel members used a nine-point scale (9 = very much liked, 8 = very much liked, 7 = generally liked, 6 = slightly liked, 5 = neither liked nor disliked, 4 = slightly disliked, 3 = generally disliked, 2 = very disliked, 1 = very disliked) to comprehensively score each antifungal agent sample, testing the color, odor, and texture of the antifungal agent samples. The sensory test results showed that the ratio in Example 4 was the optimal ratio.

[0038] The inhibitory effect of this compound fumigation-type mold inhibitor on Aspergillus flavus in feed storage:

[0039] A plate fumigation experiment was conducted using this concentration of antifungal agent against Aspergillus flavus. 1 μL of the agent at a concentration of 10... 7 A suspension of Aspergillus flavus spores (spores / g) was spotted in the center of the culture medium. The medium was then fumigated with 0 μL, 5 μL, 10 μL, 15 μL, and 20 μL of antifungal agent for 5-7 days, respectively. It was found that adding 10 μL of antifungal agent completely inhibited Aspergillus flavus growth, resulting in an airborne concentration of 0.159 μL / mL in the sealed culture dish. Therefore, this concentration of antifungal agent (0.159 μL / mL) completely inhibits Aspergillus flavus growth, thus achieving the purpose of mold prevention.

[0040] For individual samples of the antifungal agents, in the plate fumigation experiment, the minimum inhibitory concentration (MIC) of terpineol against Aspergillus flavus was 0.51 μL / mL, linalool completely inhibited the growth of Aspergillus flavus in the petri dish at a concentration of 0.571 μL / mL, and anethole also completely inhibited Aspergillus flavus at a concentration of 0.286 μL / mL. In this formulation, each component can inhibit the growth of Aspergillus flavus, but overall, the combined inhibitory effect is better, the aromatic odor is more acceptable than that of single samples or other raw material formulations, and the odor residue is less.

[0041] The various embodiments in this specification are described in a progressive manner, with each embodiment focusing on the differences from other embodiments. The same or similar parts between the various embodiments can be referred to each other.

[0042] The above description of the disclosed embodiments enables those skilled in the art to make or use the invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the invention. Therefore, the invention is not to be limited to the embodiments shown herein, but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. A compound fumigation-type mildew inhibitor, characterized in that, It is composed of the following raw materials in parts by weight: 16-17 parts trans-anescenol; 25-27 parts carvacrol; 12-14 parts linalool; 12-14 parts terpineol; 16-18 parts eugenol; 8-9 parts terpineol; 0.1-0.4 parts hexanal; 0.5-2 parts heptanal; 1-3 parts 2-heptenal; 0.5-2 parts 2-hexenal; 0.3-1 part nonanol; 0.3-1 part octanol.

2. The compound fumigation-type mildew inhibitor according to claim 1, characterized in that, It is composed of the following raw materials in parts by weight: 17 parts trans-anescenol; 26 parts carvacrol; 13 parts linalool; 13 parts terpineol; 17 parts eugenol; 9 parts terpineol; 0.3 parts hexanal; 1 part heptanal; 1.5 parts 2-heptenal; 1 part 2-hexenal; 0.5 parts nonanol; and 0.7 parts octanol.

3. The compound fumigation-type mildew inhibitor according to claim 1, characterized in that, It is composed of the following raw materials in parts by weight: 16.7 parts trans-anescenol; 25 parts carvacrol; 12.6 parts linalool; 12.6 parts terpineol; 16.7 parts eugenol; 8.4 parts terpineol; 0.4 parts hexanal; 1.6 parts heptanal; 2.8 parts 2-heptenal; 1.6 parts 2-hexenal; 0.8 parts nonanol; and 0.8 parts octanol.

4. The compound fumigation-type mildew inhibitor according to claim 1, characterized in that, It is composed of the following raw materials in parts by weight: 16.5 parts trans-anescenol; 26.5 parts carvacrol; 13.9 parts linalool; 13.6 parts terpineol; 17.6 parts eugenol; 8.8 parts terpineol; 0.2 parts hexanal; 0.6 parts heptanal; 1.1 parts 2-heptenal; 0.6 parts 2-hexenal; 0.3 parts nonanol; and 0.3 parts octanol.

5. The compound fumigation-type mildew inhibitor according to claim 1, characterized in that, It is composed of the following raw materials in parts by weight: 16.3 parts trans-anescenol; 26.6 parts carvacrol; 12.9 parts linalool; 13 parts terpineol; 17.3 parts eugenol; 9 parts terpineol; 0.4 parts hexanal; 1 part heptanal; 1.5 parts 2-heptenal; 1 part 2-hexenal; 0.5 parts nonanol; 0.5 parts octanol.

6. A method for preparing a compound fumigation-type mildew inhibitor according to any one of claims 1-5, characterized in that, Includes the following steps: Take trans-anesitol, carvacrol, linalool, terpineol, eugenol, and terpineol according to the weight ratio, mix them thoroughly, and then add hexanal, heptanal, 2-heptenal, 2-hexenal, nonanol, and octanol according to the weight ratio.

7. The application of a compound fumigation-type antifungal agent according to any one of claims 1-5 in inhibiting aflatoxin in grain storage.

8. The application according to claim 7, characterized in that, Inhibition is achieved through fumigation at a concentration of 0.1-0.2 g / m³. 3 .

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