Method for removing aflatoxin in feed
Through the use of thermally modified concave and convex rods, the problem of poor impurity content in the prior art when removing aflatoxins in feed is solved, and efficient and economical detoxification effect is achieved, ensuring the improvement of adsorption effect and cost. reduce.
Patent Information
- Application Number
- CN202411539209.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-10-31
- Publication Date
- 2025-01-10
AI Technical Summary
In the prior art, when using concave and convex rods to remove aflatoxins in the feed, poor impurities content leads to poor detoxification effect, and commonly used modification methods are cumbersome and costly.
The thermally modified concave and convex rod is used as a detoxifier to obtain concave and convex rods by modification at 200°C to 700°C, and the dosage is accurately determined based on the content of aflatoxin in the feed, and the aflatoxin is efficiently adsorbed and removed.
It improves the removal efficiency and selective adsorption effect of aflatoxin, reduces the amount of detoxicant, avoids sintering caused by excessive temperature, and achieves a good detoxication effect under a small amount.
Smart Images
Figure CN119279080A_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of feed detoxification treatment, and specifically to a method for removing aflatoxin in feed. Background Art
[0002] Soybean meal is usually used in livestock and poultry feed to improve feed utilization and promote growth. Peanut meal is a byproduct of peanut kernel oil pressing and refining. Its metabolic energy is the highest among meal feeds. Its crude protein content is close to that of soybean meal, reaching more than 48%. Its arginine content is 4.8%, the highest among all animal and plant feeds. Therefore, peanut meal can be widely used in feed as a substitute for soybean meal. However, feeds added with peanut meal are susceptible to infection with Aspergillus flavus and the production of aflatoxin, which has become the main factor restricting the use of peanut meal as feed.
[0003] At present, the main method for detoxification of aflatoxin produced by peanut meal is to mix feed containing peanut meal with biological detoxification and physical detoxification to remove aflatoxin. Commonly used biological detoxification agents include mannan, glucose oxidase, glucan, mycotoxin decomposing enzyme, Bacillus subtilis, etc.; commonly used physical detoxification agents include sodium aluminosilicate and montmorillonite. Attapulgite, also known as attapulgite, is a hydrated magnesium aluminum silicate with a unique chain layered structure, good colloidal properties and high adsorption and decolorization ability. The existing technology also uses attapulgite to remove aflatoxin from feed. However, due to the difference in the terrain conditions in which attapulgite is formed, its impurity content varies greatly, making the detoxification effect of aflatoxin in feed not very ideal. Summary of the invention
[0004] In order to solve the above technical problems, the present invention provides a method for removing aflatoxin in feed, which can effectively remove aflatoxin in feed.
[0005] To achieve the above object, the present invention adopts the following technical solution:
[0006] A method for removing aflatoxin in feed comprises the following steps:
[0007] Adding a detoxifying agent to the feed containing aflatoxin and mixing the mixture, and using the detoxifying agent to adsorb and remove the aflatoxin;
[0008] The detoxifying agent is heat-modified attapulgite, which is obtained by modifying attapulgite at 200° C. to 700° C.;
[0009] The mass ratio of the heat-modified attapulgite to the feed containing aflatoxin is 1:1500-8000.
[0010] After the detoxification treatment is performed by using the heat-modified attapulgite, aflatoxin can be quickly removed from the feed, and the removal efficiency of aflatoxin can be effectively improved. By controlling the temperature of the heat modification, the phenomenon of internal sintering and the like caused by excessively high temperature can be effectively avoided, thereby affecting the adsorption effect. The entire detoxification treatment process can not only effectively improve the detoxification effect, but also achieve a good detoxification effect with a small amount of detoxification agent, and will not cause waste.
[0011] In another preferred embodiment, the particle size of the attapulgite is 200-600 mesh.
[0012] In another preferred embodiment, the heat treatment process is as follows:
[0013] The attapulgite is kept at a temperature of 200° C. to 700° C. for 2 h to 4 h to obtain a heat-modified attapulgite.
[0014] In another preferred embodiment, the amount of heat-modified attapulgite added is determined according to the content of aflatoxin in the feed;
[0015] When the content of aflatoxin in the feed is ≤10 μg / kg, the mass ratio of the feed to the heat-modified attapulgite is 5000-8000:1;
[0016] When the aflatoxin content in the feed is 10 μg / kg to 50 μg / kg, the mass ratio of the feed to the heat-modified attapulgite is 3000 to 5000:1;
[0017] When the aflatoxin content in the feed is ≥50 μg / kg yellow, the mass ratio of the feed to the heat-modified attapulgite is 1500-3000:1.
[0018] In another preferred embodiment, the aflatoxin content is determined according to the GB / T36858-2018 method.
[0019] In another preferred embodiment, the adsorption removal time is 24h to 48h.
[0020] In another preferred embodiment, the feed is peanut meal.
[0021] Compared with the prior art, the present invention has the following beneficial effects:
[0022] (1) The removal method of the present invention can effectively improve the removal effect of aflatoxin in feed. The thermally modified attapulgite can effectively increase the specific surface area of the attapulgite, as well as the increase of active centers and adsorption sites, thereby improving the selective adsorption and adsorption effect of aflatoxin. The entire treatment process is simple and the removal effect is good. By controlling the temperature of thermal modification to 200°C to 700°C, it is possible to effectively avoid the occurrence of internal sintering due to excessive temperature, thereby affecting the adsorption effect. During use, by controlling the dosage ratio with feed to 1:1500 to 8000, the removal effect of aflatoxin can be improved while reducing the dosage.
[0023] (2) The present invention can not only improve the removal effect of aflatoxin by accurately determining the amount of detoxifying agent added according to the content of aflatoxin in the feed, but also effectively improve the use efficiency of the detoxifying agent and reduce costs. BRIEF DESCRIPTION OF THE DRAWINGS
[0024] Figure 1 This is a graph showing the adsorption results of aflatoxin by attapulgite with different mesh sizes after thermal modification in an embodiment of the present invention.
[0025] Figure 2 : is a scanning electron microscope image of ATP in an example of the present invention, wherein ATP refers to attapulgite without thermal modification.
[0026] Figure 3 It is a scanning electron microscope image of TATP-500℃, wherein TATP-500℃ refers to the attapulgite heat-treated at 500℃, and TATP refers to the heat-treated attapulgite.
[0027] Figure 4 It is a scanning electron microscope image of TATP-800℃, where TATP-800℃ refers to the attapulgite heat-treated at 800℃.
[0028] Figure 5 These are the X-ray diffraction patterns of ATP, TTAP-500°C, and TTAP-800°C.
[0029] Figure 6 These are infrared spectrum analysis diagrams of ATP, TTAP-500℃, and TTAP-800℃.
[0030] Figure 7 Specific surface area diagrams of ATP, TTAP-500℃, and TTAP-800℃, A is the specific surface area diagram, and B is the porosity diagram.
[0031] Figure 8 This is a diagram showing the adsorption effect of aflatoxin after the heat-modified attapulgite was mixed with the aflatoxin working solution in a ratio of 1:1 (m / v). DETAILED DESCRIPTION
[0032] In order to make the purpose, technical solution and advantages of the present invention more clearly understood, the present invention is further described in detail below in conjunction with the embodiments. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not used to limit the present invention.
[0033] Unless otherwise specified, the experimental methods described in the following examples are all conventional methods; the reagents and materials described are all commercially available unless otherwise specified.
[0034] Attapulgite, also known as attapulgite, is a hydrated magnesium aluminum silicate with a unique chain layered structure, good colloidal properties and high adsorption and decolorization capabilities. Due to the differences in the terrain conditions in which it is formed, the impurity content of attapulgite varies greatly, so using it directly will seriously affect its adsorption effect. In the prior art, physical modification or chemical modification is usually used to obtain modified attapulgite. The use of acid-modified attapulgite can improve the adsorption and removal effect of heavy metals, and the use of organically modified attapulgite can improve the dispersibility of attapulgite in water, but the above method is relatively cumbersome to modify the attapulgite, and hydrochloric acid or sulfuric acid will be used in the chemical modification. Therefore, the above-mentioned modified attapulgite is used for the removal of aflatoxin in feed, and its effect is not ideal.
[0035] The embodiment of the present invention provides a method for removing aflatoxin in feed, wherein thermally modified attapulgite is selected as a detoxifying agent, thereby improving the selective adsorption and adsorption effect of aflatoxin, the whole treatment process is simple, and the removal effect is good. Furthermore, according to the content of aflatoxin in the feed, the amount of the detoxifying agent is accurately added, thereby effectively improving the removal effect of aflatoxin, and at the same time, the amount of the detoxifying agent can be reduced.
[0036] The following is a detailed description of a method for removing aflatoxin from feed, wherein the feed in the following embodiment is peanut meal.
[0037] Example 1
[0038] A method for removing aflatoxin in feed comprises the following steps:
[0039] S1. Weigh 5 g of attapulgite with a particle size of 200 mesh into a crucible, put it into a muffle furnace, start timing when the temperature rises to 500°C, close the muffle furnace after calcining for 2 hours, take it out after the temperature naturally cools to room temperature, and obtain thermally modified attapulgite, i.e., a detoxifying agent.
[0040] S2. The GB / T36858-2018 method was used to determine the aflatoxin in the peanut meal to be tested. The result showed that the concentration of aflatoxin in 15g of peanut meal was 60ng / g, that is, the total amount of aflatoxin was 900ng. The peanut meal was mixed with the detoxification agent in a ratio of 5000:1, and the detoxification was completed after 24 hours.
[0041] Example 2
[0042] A method for removing aflatoxin in feed comprises the following steps:
[0043] S1. Weigh 5 g of attapulgite with a particle size of 200 mesh into a crucible, put it into a muffle furnace, start timing when the temperature rises to 500°C, close the muffle furnace after calcining for 2 hours, take it out after the temperature naturally cools to room temperature, and obtain thermally modified attapulgite, i.e., a detoxifying agent.
[0044] S2. The GB / T36858-2018 method was used to determine the aflatoxin in the peanut meal to be tested. The result showed that the concentration of aflatoxin in 15g of peanut meal was 60ng / g, that is, the total amount of aflatoxin was 900ng. The peanut meal was mixed with the detoxification agent in a ratio of 3000:1, and the detoxification was completed after 24 hours.
[0045] Example 3
[0046] A method for removing aflatoxin in feed comprises the following steps:
[0047] S1. Weigh 5 g of attapulgite with a particle size of 200 mesh into a crucible, put it into a muffle furnace, start timing when the temperature rises to 500°C, close the muffle furnace after calcining for 2 hours, take it out after the temperature naturally cools to room temperature, and obtain thermally modified attapulgite, i.e., a detoxifying agent.
[0048] S2. The GB / T36858-2018 method was used to determine the aflatoxin in the peanut meal to be tested. The result showed that the concentration of aflatoxin in 15g of peanut meal was 60ng / g, that is, the total amount of aflatoxin was 900ng. The peanut meal was mixed with the detoxification agent in a ratio of 1500:1, and the detoxification was completed after 24 hours.
[0049] In order to study the effects of attapulgite particle size and heat treatment temperature on aflatoxin removal, the following experiments were conducted.
[0050] 1. Adsorption effect of thermally modified attapulgite prepared under different conditions
[0051] Attapulgite with mesh sizes of 200, 400 and 600 were selected and modified at 200, 300, 400, 500, 600, 700 and 800 °C, respectively. The holding time was 2 h to obtain heat-modified attapulgite with different mesh sizes. Attapulgite with mesh sizes of 200, 400 and 600 that were not heat-modified were used as controls and mixed with 5 mL of a standard solution of 300 ng / mL aflatoxin, respectively. After 24 h, the adsorption amount of aflatoxin was measured. The results are shown in FIG. Figure 1 As shown. Among them, ATP is an attapulgite of different meshes without thermal modification, TATP-1 is an attapulgite of different meshes thermally modified at 200°C, TATP-2 is an attapulgite of different meshes thermally modified at 300°C, TATP-3 is an attapulgite of different meshes thermally modified at 400°C, TATP-4 is an attapulgite of different meshes thermally modified at 500°C, TATP-5 is an attapulgite of different meshes thermally modified at 600°C, TATP-6 is an attapulgite of different meshes thermally modified at 700°C, and TATP-7 is an attapulgite of different meshes thermally modified at 800°C.
[0052] from Figure 1 It can be seen from the results that when the heat treatment temperature is between 200℃ and 700℃, the heat-treated attapulgite with mesh sizes of 200 to 600 has a comparable removal effect on aflatoxin, and the content of aflatoxin after detoxification is between 0.2 and 0.5 ng. According to Part 8 of GB13078-2017 Feed Hygiene Standard, the aflatoxin content of peanut meal is less than or equal to 50 μg / kg. When the temperature is 500℃, the detoxification effect of 200-mesh attapulgite is the best. At TATP-7, i.e., 800℃, the thermally modified attapulgite with different mesh sizes has the worst adsorption effect on aflatoxin, among which the attapulgite with a mesh size of 400 has the worst adsorption effect.
[0053] 2. Structural characterization of thermally modified attapulgite
[0054] Investigate the effect of different heating temperatures on the surface structure and crystal structure of attapulgite
[0055] Figure 2 is a scanning electron microscope image of the unmodified attapulgite. Figure 3 This is a scanning electron microscope image of the attapulgite heat-modified at 500°C. Figure 4 This is a scanning electron microscope image of the attapulgite heat-modified at 800°C. Figure 2 to Figure 4 It can be seen that after thermal modification, when the heating temperature is 500°C, the surface structure of the attapulgite does not change significantly. When the temperature is 800°C, the structure of the attapulgite changes significantly, the agglomeration phenomenon of its rod-like structure is enhanced, and the diameter becomes larger.
[0056] Figure 5 These are the X-ray diffraction patterns of ATP, TTAP-500℃, and TTAP-800℃. It can be seen from the figure that heating causes the change of the shape of the attapulgite crystals, especially when the temperature is 800℃, the internal crystal structure of ATP collapses, resulting in a sharp decrease in its adsorption capacity.
[0057] The infrared spectroscopy analysis was performed on the thermally modified attapulgite with a mesh size of 200 mesh and the attapulgite with a heating temperature of 500°C and 800°C, and the results were as follows: Figure 6 As shown in the figure, ATP has a wavelength of 3460 cm -1 ~3630cm -1 , 1455cm -1 ~1660cm -1 The characteristic peak at disappeared, further verifying the change of ATP crystal structure.
[0058] The specific surface area of the heat-modified attapulgite with a mesh size of 200 mesh and the attapulgite without heat modification at the heating temperature of 500℃ and 800℃ was characterized. The results are as follows: Figure 7 As shown in the figure, it can be seen that the specific surface area of ATP is 107.1053m 2 / g, total porosity is 0.224641cm 3 / g, the specific surface area of TTAP-500c is 58.2400m 2 / g, total porosity is 0.007768cm 3 / g, the specific surface area of TTAP-800c is 9.5107m 2 / g, total porosity is 0.001129cm 3 / g.
[0059] In order to further illustrate the effect of the heat-modified attapulgite in the present invention, a kinetic study was conducted on the heat-modified attapulgite. The 200-mesh attapulgite heated at 500°C was reacted with aflatoxin in a simulated intestinal fluid environment, and after being protected from light, it was placed in a 37°C shaker for different periods of time. The residual aflatoxin was measured at different points at different times. The results are as follows: Figure 8 shown.
[0060] The following uses attapulgite with a heat treatment temperature of 500°C and a mesh size of 200 as an example to detoxify peanut meal with different contamination degrees, and uses it as the experimental group. The dosage of the detoxifying agent and the experimental results are shown in Table 1. Sodium aluminosilicate was selected as the control group, and detoxification was carried out according to different aflatoxin contents. The dosage of sodium aluminosilicate and the detoxification effect are shown in Table 2.
[0061] Table 1 Aflatoxin content in the experimental group after detoxification
[0062]
[0063] Table 2 Aflatoxin content of the control group after detoxification
[0064]
[0065]
[0066] It can be seen from the results in Table 1 and Table 2 that the detoxification of peanut meal with different contamination degrees using the thermally modified attapulgite of the present invention is significantly better than the prior art method for removing aflatoxin.
[0067] Obviously, the above embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.
Claims
1. A method for removing aflatoxin in feed, characterized in that: The following steps are involved: Adding a detoxifying agent to the feed containing aflatoxin and mixing the mixture, and using the detoxifying agent to adsorb and remove the aflatoxin; The detoxifying agent is heat-modified attapulgite, which is obtained by modifying attapulgite at 200° C. to 700° C.; The mass ratio of the heat-modified attapulgite to the feed is 1:1500-8000.
2. The method for removing aflatoxin in feed according to claim 1, characterized in that: The mesh number of the attapulgite is 200-600 meshes.
3. The method for removing aflatoxin in feed according to claim 1, characterized in that: The heat treatment process is specifically as follows: The attapulgite is kept at 200°C to 700°C for 2h to 4h to obtain a heat-modified attapulgite.
4. The method for removing aflatoxin in feed according to claim 1, characterized in that: The amount of heat-modified attapulgite added is determined according to the content of aflatoxin in the feed; When the content of aflatoxin in the feed is ≤10 μg / kg, the mass ratio of the feed to the heat-modified attapulgite is 5000-8000:1; When the aflatoxin content in the feed is 10 μg / kg to 50 μg / kg, the mass ratio of the feed to the heat-modified attapulgite is 3000 to 5000:1; When the aflatoxin content in the feed is ≥50 μg / kg, the mass ratio of the feed to the heat-modified attapulgite is 1500-3000:
1.
5. The method for removing aflatoxin in feed according to claim 4, characterized in that: The aflatoxin content is determined according to the GB / T36858-2018 method.
6. The method for removing aflatoxin in feed according to claim 1, characterized in that: The adsorption removal time is 24h to 48h.
7. The method for removing aflatoxin in feed according to claim 1, characterized in that: The feed includes peanut meal.