Process method for reducing vomitoxin content and fumonisins content in corn soaking water

Abstract

The invention relates to the technical field of corn soaking water treatment, in particular to a process method for reducing the content of vomitoxin and fumonisins in corn soaking water, which comprises the following steps: collecting the corn soaking water adsorbed by phytic acid, adding diatomite, stirring, adsorbing and settling for a period of time, and filtering to remove a small amount of toxins; the method comprises the following steps: collecting a filtrate, carrying out hot concentration on the collected filtrate, adding an organic solvent formed by mixing acetone and ethyl acetate according to a volume ratio of 3: 1 into the collected concentrated solution, controlling the pH value to be 6-6.5 and the temperature to be 50-55 DEG C, standing for layering after extraction is finished, concentrating and drying the collected heavy-phase feed liquid, thereby obtaining the vomitoxin protein with the vomitoxin content of not more than 1832 [mu] g in each kilogram of protein and the vomitoxin content of not more than 1832 [mu] g in each kilogram of protein. And the fumonisins content of the protein product does not exceed 25669 [mu] g. The method is simple to operate, the content of vomitoxin and fumonisins in the protein can be greatly reduced, and the application safety of the protein is ensured.

Description

Technical Field

[0001] The invention relates to the technical field of corn soaking water treatment, in particular to a process for reducing the contents of vomitoxin and fumonisin in corn soaking water. Background Art

[0002] Deoxynivalenol (DON), also known as deoxynivalenol (DON), is a monothene compound. It is a toxic secondary metabolite produced by Fusarium fungi during their growth and is a common toxin in grains. It can cause animal poisoning, reduce animal production performance, and can remain in agricultural products such as meat, eggs, and milk, thus causing food safety problems and causing serious harm to human health.

[0003] Fumonisin is a diester compound of polyhydric alcohol and tricarbamic acid. It is mainly a secondary metabolite produced by the reproduction of Fusarium moniliforme and Fusarium prolificum under certain temperature and humidity conditions. It is not only a cancer promoter for humans and livestock, but also a carcinogen. Animal experiments have shown that fumonisin mainly damages liver and kidney functions and can cause diseases such as pulmonary edema in pigs.

[0004] Corn soaking water is the waste after wet starch production, which contains dry matter, phytic acid, protein, lactic acid, calcium, magnesium and other effective ingredients; corn is easy to mold and produce toxins when stored, so corn soaking water also contains vomitoxin and fumonisin; the current existing research direction is to recover phytic acid, lactic acid, calcium and magnesium ions in corn soaking water. Although there is also protein recovery, due to the large amount of vomitoxin and fumonisin in corn soaking water, the recovered protein contains a large amount of toxins. If it is directly used as an animal feed ingredient, it has safety hazards; although the prior art discloses a method for extracting fumonisin using n-butanol, the extraction efficiency is low, the toxin content is still high, and the vomitoxin cannot be removed. Therefore, in view of the above problems, it is necessary to develop a process for reducing the content of vomitoxin and fumonisin in corn soaking water. Summary of the invention

[0005] The technical problem to be solved by the present invention is: in view of the deficiencies of the prior art, a process method for reducing the content of vomitoxin and fumonisin in corn soaking water is provided. The process method can reduce the content of vomitoxin and fumonisin, thereby ensuring the safety of the protein.

[0006] In order to solve the above technical problems, the technical solution of the present invention is: A process for reducing the content of vomitoxin and fumonisin in corn soaking water, the process comprising the following steps: (1) Take the corn soaking water after phytic acid adsorption, add diatomaceous earth, stir, adsorb and settle, filter, and collect the filtrate for use; (2) taking the filtrate in step (1), concentrating it, and using the obtained concentrated solution for later use; (3) The concentrated solution in step (2) is added with a mixed organic solvent, stirred and mixed, and the pH and temperature are adjusted. The heavy phase solution collected after the extraction is concentrated and dried to obtain a protein product having a vomitoxin content of no more than 1350 μg and a fumonisin content of no more than 11400 μg per kilogram of protein.

[0007] As an improved technical solution, the corn soaking water in step (1) contains 2000 ppb of vomitoxin and 12000 ppb of fumonisin.

[0008] As an improved technical solution, the amount of diatomaceous earth added in step (1) is 1-3‰ of the weight of the corn soaking water, and the time for stirring, adsorption and sedimentation treatment after adding the diatomaceous earth is 4-6 hours.

[0009] As an improved technical solution, the solid content of the concentrated solution in step (2) is 30-35wt%.

[0010] As an improved technical solution, the concentrated solution and the mixed organic solvent in step (3) are added in a weight-volume ratio of 1:2-3; the mixed organic solvent is formed by mixing water-saturated acetone and water-saturated ethyl acetate in a volume ratio of 6:4, 7:3 or 8:2.

[0011] As an improved technical solution, in step (3), the pH is adjusted to 6-6.5 and the temperature is adjusted to 50-55°C.

[0012] After adopting the above technical solution, the beneficial effects of the present invention are: The present invention collects corn soaking water after phytic acid adsorption, adds diatomaceous earth, stirs adsorption sedimentation for a period of time and then filters to remove a small amount of toxins; then the collected filtrate is heat concentrated, and an organic solvent mixed with acetone and ethyl acetate in a volume ratio of 3:1 is added to the collected concentrated solution, and the pH is controlled to be 6-6.5, and the temperature is 50-55°C. After the extraction is completed, the heavy phase liquid is allowed to stand for stratification, and the collected heavy phase liquid is concentrated and dried to obtain a protein product with a content of no more than 1350μg of vomitoxin and a content of no more than 11400μg of fumonisin per kilogram of protein. The method is simple to operate, can greatly reduce the content of vomitoxin and fumonisin in the protein, and ensures the safety of protein application. DETAILED DESCRIPTION

[0013] 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. Example 1

[0014] A process for reducing the content of vomitoxin and fumonisin in corn soaking water comprises the following steps: (1) Take 100L corn soaking water (solid content 11%, vomitoxin 2000ppb, fumonisin 12000ppb, protein content 5.28%) after adsorption of phytic acid, add 1‰ of diatomaceous earth by weight of corn soaking water, stir, adsorb and settle for 4h, filter with plate and frame filter, and collect 99L of filtrate for use; (2) 99 L of the filtrate from step (1) was taken and concentrated by heating to obtain 36.24 kg of a concentrated solution having a solid content of 30 wt % for standby use; (3) 36.24 kg of the concentrated solution with a solid content of 30 wt% in step (2) was added to a mixed organic solvent (water-saturated acetone and water-saturated ethyl acetate mixed in a volume ratio of 6:4) in a weight-to-volume ratio of 1:2 (kg / L), and the mixture was stirred and mixed. The pH was adjusted to 6 and the temperature was 50°C. The heavy phase liquid collected after the extraction was concentrated by heating and dried to obtain 6.77 kg of a protein product with a vomitoxin content of 1332 μg and a fumonisin content of 11354 μg per kilogram of protein, with a yield of 83.3% and a purity of 65%. Example 2

[0015] A process for reducing the content of vomitoxin and fumonisin in corn soaking water comprises the following steps: (1) Take 100L corn soaking water after phytic acid adsorption (solid content 11%, vomitoxin 2000ppb, fumonisin 12000ppb, protein content 5.28%), add 1.5‰ of diatomaceous earth by weight of corn soaking water, stir, adsorb and settle for 4.5h, filter with plate and frame filter, and collect 98.4L of filtrate for use; (2) 98.4 L of the filtrate from step (1) was taken and concentrated by heating to obtain 33.85 kg of a concentrated solution having a solid content of 32 wt % for standby use; (3) 33.85 kg of the concentrated solution with a solid content of 32 wt% in step (2) was added to a mixed organic solvent (water-saturated acetone and water-saturated ethyl acetate mixed in a volume ratio of 6:4) in a weight-to-volume ratio of 1:2.5 (kg / L), and the mixture was stirred and mixed. The pH was adjusted to 6.2 and the temperature was 52°C. The heavy phase liquid collected after the extraction was completed was heated, concentrated and dried to obtain 6.6 kg of a protein product with a vomitoxin content of 1164 μg and a fumonisin content of 10843 μg per kilogram of protein, with a yield of 84.1% and a purity of 67.3%. Example 3

[0016] A process for reducing the content of vomitoxin and fumonisin in corn soaking water comprises the following steps: (1) Take 100L corn soaking water (solid content 11%, vomitoxin 2000ppb, fumonisin 12000ppb, protein content 5.28%) after phytic acid adsorption, add 2‰ of diatomaceous earth by weight of corn soaking water, stir, adsorb and settle for 5h, filter with plate and frame filter, and collect 97.8L of filtrate for use; (2) 97.8 L of the filtrate from step (1) was taken and concentrated by heating to obtain 30.7 kg of a concentrated solution having a solid content of 35 wt % for standby use; (3) 30.7 kg of the concentrated solution with a solid content of 35 wt% in step (2) was taken, and a mixed organic solvent (water-saturated acetone and water-saturated ethyl acetate mixed in a volume ratio of 6:4) was added in a weight-to-volume ratio of 1:3 (kg / L), and the mixture was stirred and mixed. The pH was adjusted to 6.5 and the temperature was 55°C. The heavy phase liquid collected after the extraction was completed was heated, concentrated and dried to obtain 6.53 kg of a protein product with a vomitoxin content of 981 μg and a fumonisin content of 7816 μg per kilogram of protein, with a yield of 84.8% and a purity of 68.6%. Example 4

[0017] A process for reducing the content of vomitoxin and fumonisin in corn soaking water comprises the following steps: (1) Take 100L corn soaking water (solid content 11%, vomitoxin 2000ppb, fumonisin 12000ppb, protein content 5.28%) after adsorption of phytic acid, add 2.5‰ of diatomaceous earth by weight of corn soaking water, stir, adsorb and settle for 5.5h, filter with a plate and frame filter, and collect 97.1L of filtrate for use; (2) 97.1 L of the filtrate from step (1) was taken and concentrated by heating to obtain 30.5 kg of a concentrated solution having a solid content of 35 wt % for standby use; (3) 30.5 kg of the concentrated solution with a solid content of 35 wt% in step (2) was added to a mixed organic solvent (water-saturated acetone and water-saturated ethyl acetate mixed in a volume ratio of 7:3) at a weight-to-volume ratio of 1:3 (kg / L), and the mixture was stirred and mixed. The pH was adjusted to 6.5 and the temperature was 55°C. The heavy phase liquid collected after the extraction was completed was heated, concentrated and dried to obtain 6.48 kg of a protein product with a vomitoxin content of 1098 μg and a fumonisin content of 8634 μg per kilogram of protein, with a yield of 83.8% and a purity of 68.2%. Example 5

[0018] A process for reducing the content of vomitoxin and fumonisin in corn soaking water comprises the following steps: (1) Take 100L corn soaking water (solid content 11%, vomitoxin 2000ppb, fumonisin 12000ppb, protein content 5.28%) after adsorption of phytic acid, add 3‰ of diatomaceous earth by weight of corn soaking water, stir, adsorb and settle for 6h, filter with plate and frame filter, and collect 96% of filtrate for use; (2) 96 L of the filtrate from step (1) was taken and concentrated by heating to obtain 30.14 kg of a concentrated solution having a solid content of 35 wt % for standby use; (3) 30.14 kg of the concentrated solution with a solid content of 35 wt% in step (2) was taken, and a mixed organic solvent (water-saturated acetone and water-saturated ethyl acetate mixed in a volume ratio of 8:2) was added in a weight-to-volume ratio of 1:3 (kg / L), and the mixture was stirred and mixed. The pH was adjusted to 6.5 and the temperature was 55°C. The heavy phase liquid collected after the extraction was completed was heated, concentrated and dried to obtain 6.63 kg of a protein product with a vomitoxin content of 1070 μg and a fumonisin content of 9606 μg per kilogram of protein, with a yield of 83% and a purity of 66.1%.

[0019] In order to better demonstrate that the process of the present invention can reduce the content of vomitoxin and fumonisin, and at the same time can obtain a protein product with high yield, high yield and high purity, the following 13 comparative examples are given with reference to Example 3.

[0020] Comparative Example 1 The difference from the operation of Example 3 is that in step (1), diatomaceous earth adsorption treatment is not added, and ceramic membrane filtration is directly used. In step (3), 7.44 kg of protein product with a vomitoxin content of 3210 μg and a fumonisin content of 21000 μg per kilogram of protein is obtained, with a yield of 86% and a purity of 61%.

[0021] Comparative Example 2 The difference from the operation in Example 3 is that the diatomaceous earth adsorption and sedimentation treatment time in step (1) is 7 hours, and the other operations are the same. In step (3), 6.3 kg of protein product with a vomitoxin content of 1120 μg and a fumonisin content of 9055 μg per kilogram of protein is obtained, with a yield of 79% and a purity of 66.2%.

[0022] Comparative Example 3 The difference from the operation in Example 3 is that the diatomaceous earth adsorption and sedimentation treatment time in step (1) is 3 hours, and the other operations are the same. In step (3), 6.85 kg of protein product with a vomitoxin content of 2140 μg and a fumonisin content of 18366 μg per kilogram of protein is obtained, with a yield of 83% and a purity of 64%.

[0023] Comparative Example 4 The difference from the operation in Example 3 is that the pH is adjusted to 5.5 in step (3), and the other operations are the same. In step (3), 6.5 kg of protein product with a DON content of 3788 μg and a fumonisin content of 32011 μg per kg of protein is obtained, with a yield of 83% and a purity of 67.4%.

[0024] Comparative Example 5 The difference from the operation in Example 3 is that the pH in step (3) is adjusted to 7, and the other operations are the same. In step (3), 6.88 kg of protein product with a DON content of 1437 μg and a fumonisin content of 13200 μg per kg of protein is obtained, with a yield of 73% and a purity of 56%.

[0025] Comparative Example 6 The difference from the operation in Example 3 is that the temperature in step (3) is adjusted to 45° C., and the other operations are the same. In step (3), 6.75 kg of protein product with a DON content of 2651 μg and a fumonisin content of 27033 μg per kg of protein is obtained, with a yield of 78% and a purity of 61%.

[0026] Comparative Example 7 The operation is different from that in Example 3, in step (3), the mixed organic solvent is water-saturated acetonitrile and water-saturated ethyl acetate mixed in a volume ratio of 6:4, and the remaining operations are the same. In step (3), 7.37 kg of protein product with a DON content of 4270 μg and a fumonisin content of 31988 μg per kg of protein is obtained, with a yield of 81% and a purity of 58%.

[0027] Comparative Example 8 The difference from the operation in Example 3 is that the mixed organic solvent in step (3) is water-saturated acetone and water-saturated acetonitrile mixed in a volume ratio of 6:4, and the other operations are the same. In step (3), 7.38 kg of protein product with a vomitoxin content of 3974 μg and a fumonisin content of 28100 μg per kilogram of protein was obtained, with a yield of 80.2% and a purity of 57.4%.

[0028] Comparative Example 9 The difference from the operation in Example 3 is that the mixed organic solvent in step (3) is methanol and water-saturated ethyl acetate mixed in a volume ratio of 6:4, and the other operations are the same. In step (3), 6.15 kg of protein product with a vomitoxin content of 5830 μg and a fumonisin content of 56210 μg per kilogram of protein was obtained, with a yield of 71% and a purity of 61%.

[0029] Comparative Example 10 The difference from the operation in Example 3 is that the mixed organic solvent in step (3) is methanol and water-saturated acetonitrile mixed in a volume ratio of 6:4, and the other operations are the same. In step (3), 5.93 kg of protein product with a vomitoxin content of 4671 μg and a fumonisin content of 45000 μg per kilogram of protein was obtained, with a yield of 70% and a purity of 62.3%.

[0030] Comparative Example 11 The operation is different from that in Example 3, in step (3), the mixed organic solvent is water-saturated acetone and water-saturated ethyl acetate mixed in a volume ratio of 5:5, and the other operations are the same. In step (3), 6.42 kg of protein product with a vomitoxin content of 2906 μg and a fumonisin content of 23012 μg per kilogram of protein was obtained, with a yield of 79% and a purity of 65%.

[0031] Comparative Example 12 The operation is different from that in Example 3, in step (3), the mixed organic solvent is water-saturated acetone and water-saturated ethyl acetate mixed in a volume ratio of 3:7, and the other operations are the same. In step (3), 6.4 kg of protein product with a vomitoxin content of 3104 μg and a fumonisin content of 42122 μg per kilogram of protein was obtained, with a yield of 74% and a purity of 61%.

[0032] Comparative Example 13 The difference from the operation in Example 3 is that the mixed organic solvent in step (3) is water-saturated acetone and water-saturated ethyl acetate mixed in a volume ratio of 1:9, and the other operations are the same. In step (3), 7 kg of protein product with a vomitoxin content of 4051 μg and a fumonisin content of 56400 μg per kilogram of protein is obtained, with a yield of 78% and a purity of 59%.

[0033] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. A process for reducing the content of vomitoxin and fumonisin in corn soaking water, characterized in that: The process comprises the following steps: (1) Take the corn soaking water after phytic acid adsorption, add diatomaceous earth, stir, adsorb and settle, filter, and collect the filtrate for use; (2) taking the filtrate in step (1), concentrating it, and using the obtained concentrated solution for later use; (3) The concentrated solution in step (2) is added with a mixed organic solvent, stirred and mixed, and the pH and temperature are adjusted. The heavy phase solution collected after the extraction is concentrated and dried to obtain a protein product having a vomitoxin content of no more than 1350 μg and a fumonisin content of no more than 11400 μg per kilogram of protein.

2. The process for reducing the content of vomitoxin and fumonisin in corn soaking water according to claim 1, characterized in that: The corn soaking water in step (1) contains 2000 ppb of vomitoxin and 12000 ppb of fumonisin.

3. The process for reducing the content of vomitoxin and fumonisin in corn soaking water according to claim 1, characterized in that: In step (1), the amount of diatomaceous earth added is 1-3‰ of the weight of the corn soaking water, and the time for stirring, adsorption and sedimentation treatment after adding the diatomaceous earth is 4-6 hours.

4. The process for reducing the content of vomitoxin and fumonisin in corn soaking water according to claim 1, characterized in that: The solid content of the concentrated solution in step (2) is 30-35wt%.

5. The process for reducing the content of vomitoxin and fumonisin in corn soaking water according to claim 1, characterized in that: In step (3), the concentrated solution and the mixed organic solvent are added in a weight-volume ratio of 1:2-3; the mixed organic solvent is prepared by mixing water-saturated acetone and water-saturated ethyl acetate in a volume ratio of 6:4, 7:3 or 8:

2.

6. The process for reducing the content of vomitoxin and fumonisin in corn soaking water according to claim 1, characterized in that: In step (3), the pH is adjusted to 6-6.5 and the temperature is adjusted to 50-55°C.