Process method for reducing toxin content in corn soaking water by adopting complex enzyme synergistic surfactant

Abstract

The invention relates to the technical field of corn soaking water treatment, in particular to a process method for reducing the toxin content in corn soaking water by adopting a complex enzyme and a surfactant, which comprises the following steps: collecting the corn soaking water adsorbing phytic acid, filtering by a nanofiltration membrane, adjusting the pH value and temperature of the collected filtrate, entering a resin column, and collecting the toxin content in the corn soaking water. The method comprises the following steps of: collecting effluent, effectively removing a small amount of toxins, concentrating the collected effluent, adding a compound enzyme and a surfactant into the obtained concentrated solution, adjusting the temperature and the pH value, carrying out microwave treatment on enzymatic hydrolysis reaction feed liquid obtained by reaction for several minutes, adding activated carbon, adsorbing by the activated carbon, filtering, concentrating and drying the collected filtrate, and thus obtaining the toxin-containing enzymatic hydrolysate. The content of vomitoxin in each kilogram of protein does not exceed 930 micrograms, and the content of fumonisins in each kilogram of protein does not exceed 9250 micrograms. According to the process method, the reaction is mild, and the yield and purity of the protein are improved while the content of vomitoxin and fumonisins is effectively reduced.

Description

Technical Field

[0001] The invention relates to the technical field of corn soaking water treatment, in particular to a process method for reducing the toxin content in corn soaking water by using a composite enzyme in coordination with a surfactant. 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 prone to mildew and produce toxins during storage, so corn soaking water also contains vomitoxin and fumonisin; the current research direction is to recover phytic acid, lactic acid, calcium and magnesium ions in corn soaking water. Although protein is also recovered, the corn soaking water contains a large amount of vomitoxin and fumonisin, resulting in a large amount of toxins in the recovered protein. If it is directly used as an animal feed ingredient, it has a safety hazard; therefore, in response to the above problems, it is necessary to develop a process method that uses a composite enzyme to cooperate with a surfactant to reduce the toxin content in corn soaking water. Summary of the invention

[0005] The technical problem to be solved by the present invention is: in view of the shortcomings of the prior art, a process method for reducing the toxin content in corn soaking water by using a composite enzyme in coordination with a surfactant is provided, and the content of vomitoxin and fumonisin can be reduced by using the process method.

[0006] In order to solve the above technical problems, the technical solution of the present invention is: A process for reducing the toxin content in corn soaking water by using a composite enzyme in coordination with a surfactant, the process comprising the following steps: (1) Take the corn soaking water after phytic acid adsorption, filter and collect the filtrate for later use; (2) taking the filtrate in step (1), passing it through a resin column after controlling the temperature and pH, and concentrating the collected effluent to obtain a concentrated solution for later use; (3) taking the concentrated solution in step (2), adding the complex enzyme and the surfactant, stirring and mixing, controlling the pH, temperature and reaction time, and setting the enzymatic hydrolysis solution after the reaction for later use; (4) taking the enzymatic hydrolysis solution in step (3), treating it with microwaves, adding activated carbon, and continuing to stir and mix, and the obtained solution is set aside; (5) The feed liquid in step (4) is concentrated and filtered, and the collected filtrate is dried to obtain a protein product having a vomitoxin content of no more than 930 μg and a fumonisin content of no more than 9250 μg per kilogram of protein.

[0007] As an improved technical solution, the filtrate in step (2) is controlled at a temperature of 35-40°C and a pH of 3.8-4.2, and the filtrate enters the resin column at a flow rate of 1-2BV / h; the filler in the resin column is a macroporous adsorption resin, and the model of the resin is Lanxiao Technology--LSA-900B.

[0008] As an improved technical solution, the complex enzyme in step (3) includes glucose oxidase, amylase and Aspergillus niger amine oxidase, the activity of the glucose oxidase is 5000 U / g, the activity of the amylase is 1000 U / g, and the activity of the Aspergillus niger amine oxidase is 1000 U / g.

[0009] As an improved technical solution, the solid content of the concentrated solution in step (3) is 35-40wt%, the amount of the glucose oxidase used is 0.5-1.5‰ of the solid content of the concentrated solution, the amount of the amylase used is 0.15-0.2‰ of the solid content of the concentrated solution, and the amount of the Aspergillus niger amine oxidase used is 0.3-0.5‰ of the solid content of the concentrated solution.

[0010] As an improved technical solution, the surfactant in step (3) is sodium dodecyl sulfate, and the amount of the surfactant used is 0.8-1.0‰ of the volume of the concentrated solution.

[0011] As an improved technical solution, in step (3), the temperature is controlled at 50-60°C, the pH is 6.5-7, and the reaction time is 4-6h.

[0012] As an improved technical solution, the power of the microwave treatment in step (4) is 200-300 W, and the microwave treatment time is 3-5 min.

[0013] As an improved technical solution, the amount of activated carbon added in step (4) is 0.5-1.0‰ of the solid content of the concentrated liquid.

[0014] 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, first filters it through a nanofiltration membrane, adjusts the pH and temperature of the collected filtrate, and enters a resin column to effectively remove a small amount of toxins, and then concentrates the collected effluent, adds a composite enzyme and a surfactant to the obtained concentrated solution, adjusts the temperature and pH, and then microwaves the enzymatic hydrolysis reaction liquid obtained by the reaction for a few minutes, adds activated carbon, and then filters it after adsorption by the activated carbon. The collected filtrate is concentrated and dried to obtain a protein product with a content of no more than 930 μg of vomitoxin and a content of no more than 9250 μg of fumonisin per kilogram of protein. The above process method has a mild reaction, effectively reduces the content of vomitoxin and fumonisin, and also improves the yield and purity of the protein. DETAILED DESCRIPTION

[0015] 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

[0016] A process for reducing the toxin content in corn soaking water by using a composite enzyme in coordination with a surfactant comprises the following steps: (1) Take 100 L of corn soaking water (solid content 11%, vomitoxin 2000 ppb, fumonisin 12000 ppb, protein content 5.28%) after phytic acid adsorption, filter through a 50 nm ceramic membrane, and collect 91 L of the filtrate for later use; (2) 91 L of the filtrate from step (1) was taken, the temperature was controlled at 35°C, the pH was 3.8, and the filtrate was introduced into a 20 L resin column (filler was macroporous adsorption resin, model: Lanxiao Technology--LSA-900B) at a flow rate of 1 BV / h. The collected 91 L of effluent was thermally concentrated to obtain 23.66 L of a concentrate with a solid content of 35 wt% for standby use; (3) Take 23.66 L of the concentrated solution with a solid content of 35 wt% in step (2), add a composite enzyme (including glucose oxidase with an activity of 5000 U / g and an amount of 0.5‰ of the solid content of the concentrated solution, amylase with an activity of 1000 U / g and an amount of 0.15‰ of the solid content of the concentrated solution, and Aspergillus niger amine oxidase with an activity of 1000 U / g and an amount of 0.3‰ of the solid content of the concentrated solution) and a surfactant (sodium dodecyl sulfate, an amount of 0.8‰ of the volume of the concentrated solution), stir and mix, control the pH to 6.5 and the temperature to 50°C, react for 4 h, and collect 23.66 L of the enzymatic hydrolysis solution for use; (4) Take 23.66 L of the enzymatic hydrolysis solution in step (3), treat it with microwave (power is 200 W, treatment time is 3 min), then add activated carbon (the amount is 0.5‰ of the solid content of the concentrate), continue to stir and mix, and the obtained solution is set aside; (5) The feed liquid in step (4) was heated and concentrated to a solid content of 50 wt %, filtered, and the collected filtered clear liquid was dried to obtain 5.75 kg of a protein product having a vomitoxin content of 921 μg and a fumonisin content of 9041 μg per kilogram of protein, a yield of 85%, and a purity of 71%. Example 2

[0017] A process for reducing the toxin content in corn soaking water by using a composite enzyme in coordination with a surfactant comprises the following steps: (1) Take 100 L of corn soaking water (solid content 11%, vomitoxin 2000 ppb, fumonisin 12000 ppb, protein content 5.28%) after phytic acid adsorption, filter through a 50 nm ceramic membrane, and collect 91.5 L of the filtrate for later use; (2) 91.5 L of the filtrate in step (1) was taken, the temperature was controlled at 38°C, the pH was 4.0, and it was fed into a 20 L resin column (filler was macroporous adsorption resin, model: Lanxiao Technology--LSA-900B) at a flow rate of 1.2 BV / h. The collected 91.5 L of effluent was thermally concentrated to obtain 22 L of concentrated solution with a solid content of 38 wt% for standby use; (3) Take 22L of the concentrated solution with a solid content of 38wt% in step (2), add a composite enzyme (including glucose oxidase with an activity of 5000U / g and an amount of 0.8‰ of the solid content of the concentrated solution, amylase with an activity of 1000U / g and an amount of 0.18‰ of the solid content of the concentrated solution, and Aspergillus niger amine oxidase with an activity of 1000U / g and an amount of 0.4‰ of the solid content of the concentrated solution) and a surfactant (sodium dodecyl sulfate, an amount of 0.9‰ of the volume of the concentrated solution), stir and mix, control the pH to 6.8 and the temperature to 52°C, react for 4.5h, and collect 22L of the enzymatic hydrolysis solution for use; (4) Take 22 L of the enzymatic hydrolysis solution in step (3), treat it with microwave (power is 230 W, treatment time is 3.5 min), then add activated carbon (the amount is 0.8‰ of the solid content of the concentrate), continue stirring and mixing, and the obtained solution is set aside; (5) The feed liquid in step (4) was heated and concentrated to a solid content of 52%, filtered, and the filtered clear liquid was collected and dried to obtain 5.89 kg of a protein product having a vomitoxin content of 886 μg and a fumonisin content of 9230 μg per kilogram of protein, a yield of 85.6%, and a purity of 70.2%. Example 3

[0018] A process for reducing the toxin content in corn soaking water by using a composite enzyme in coordination with a surfactant comprises the following steps: (1) Take 100 L of corn soaking water (solid content 11%, vomitoxin 2000 ppb, fumonisin 12000 ppb, protein content 5.28%) after phytic acid adsorption, filter through a 50 nm ceramic membrane, and collect 91.1 L of the filtrate for later use; (2) Take 91.1 L of the filtrate in step (1), control the temperature to 40°C and the pH to 4.2, and enter a 20 L resin column (filler is macroporous adsorption resin, model: Lanxiao Technology--LSA-900B) at a flow rate of 1.5 BV / h. The collected 91.1 L of effluent is thermally concentrated to obtain 21 L of concentrated solution with a solid content of 40 wt% for standby use; (3) Take 21L of the concentrated solution with a solid content of 40wt% in step (2), add composite enzyme (including glucose oxidase with an activity of 5000U / g and an amount of 1.0‰ of the solid content of the concentrated solution, amylase with an activity of 1000U / g and an amount of 0.18‰ of the solid content of the concentrated solution, Aspergillus niger amine oxidase with an activity of 1000U / g and an amount of 0.5‰ of the solid content of the concentrated solution) and surfactant (sodium dodecyl sulfate, an amount of 1.0‰ of the volume of the concentrated solution), stir and mix, control the pH to 6.8 and the temperature to 55°C, react for 5h, and collect 21L of enzymatic hydrolysis solution for use; (4) Take 21 L of the enzymatic hydrolysis solution in step (3), treat it with microwave (power is 250 W, treatment time is 5 min), then add activated carbon (0.8‰ of the solid content of the concentrate), continue stirring and mixing, and the obtained solution is ready for use; (5) The feed liquid in step (4) was heated and concentrated to a solid content of 55%, filtered, and the filtered clear liquid was collected and dried to obtain 5.78 kg of a protein product having a vomitoxin content of 805 μg and a fumonisin content of 7603 μg per kilogram of protein, a yield of 87.1%, and a purity of 72.5%. Example 4

[0019] A process for reducing the toxin content in corn soaking water by using a composite enzyme in coordination with a surfactant comprises the following steps: (1) Take 100 L of corn soaking water after phytic acid adsorption (solid content 11%, vomitoxin 1800 ppb, fumonisin 8800 ppb, protein content 5.28%), filter through a 50 nm ceramic membrane, and collect 91.2 L of the filtrate for later use; (2) 91.2 L of the filtrate in step (1) was taken, the temperature was controlled at 40°C, the pH was 4.2, and it was fed into a 20 L resin column (filler was macroporous adsorption resin, model: Lanxiao Technology--LSA-900B) at a flow rate of 1.8 BV / h. The collected 91.2 L of effluent was thermally concentrated to obtain 21 L of concentrated solution with a solid content of 40 wt% for standby use; (3) Take 21L of the concentrated solution with a solid content of 40wt% in step (2), add composite enzyme (including glucose oxidase with an activity of 5000U / g and an amount of 1.2‰ of the solid content of the concentrated solution, amylase with an activity of 1000U / g and an amount of 0.18‰ of the solid content of the concentrated solution, Aspergillus niger amine oxidase with an activity of 1000U / g and an amount of 0.5‰ of the solid content of the concentrated solution) and surfactant (sodium dodecyl sulfate, an amount of 1.0‰ of the volume of the concentrated solution), stir and mix, control the pH to 7 and the temperature to 58°C, react for 5.5h to complete the reaction, and collect 21L of enzymatic hydrolysis solution for use; (4) Take 21 L of the enzymatic hydrolysis solution in step (3), treat it with microwaves (power of 280 W, treatment time of 5 min), then add activated carbon (1.0‰ of the solid content of the concentrate), continue stirring and mixing, and the resulting solution is ready for use; (5) The feed liquid in step (4) was heated and concentrated to a solid content of 50%, filtered, and the filtered clear liquid was collected and dried to obtain 5.71 kg of a protein product having a vomitoxin content of 890 μg and a fumonisin content of 8823 μg per kilogram of protein, a yield of 84.6%, and a purity of 71.3%. Example 5

[0020] A process for reducing the toxin content in corn soaking water by using a composite enzyme in coordination with a surfactant comprises the following steps: (1) Take 100 L of corn soaking water (solid content 11%, vomitoxin 2000 ppb, fumonisin 9000 ppb, protein content 5.28%) after phytic acid adsorption, filter through a 50 nm ceramic membrane, and collect 91 L of the filtrate for later use; (2) Take 91L of the filtrate in step (1), control the temperature to 40°C and the pH to 4.2, and enter a 20L resin column (filler is macroporous adsorption resin, model: Lanxiao Technology--LSA-900B) at a flow rate of 2BV / h. The collected 91L of effluent is thermally concentrated to obtain 21L of concentrated solution with a solid content of 40wt% for standby use; (3) Take 21L of the concentrated solution with a solid content of 40wt% in step (2), add composite enzyme (including glucose oxidase with an activity of 5000U / g and an amount of 1.5‰ of the solid content of the concentrated solution, amylase with an activity of 1000U / g and an amount of 0.2‰ of the solid content of the concentrated solution, Aspergillus niger amine oxidase with an activity of 1000U / g and an amount of 0.5‰ of the solid content of the concentrated solution) and surfactant (sodium dodecyl sulfate, an amount of 1.0‰ of the volume of the concentrated solution), stir and mix, control the pH to 7 and the temperature to 60°C, react for 6h, and collect 21L of enzymatic hydrolysis solution for use; (4) Take 21 L of the enzymatic hydrolysis solution in step (3), treat it with microwaves (power of 300 W, treatment time of 5 min), then add activated carbon (1.0‰ of the solid content of the concentrate), continue stirring and mixing, and the resulting solution is ready for use; (5) The feed liquid in step (4) was heated and concentrated to a solid content of 52%, filtered, and the filtered clear liquid was collected and dried to obtain 5.67 kg of a protein product having a vomitoxin content of 907 μg and a fumonisin content of 9020 μg per kilogram of protein, a yield of 83.5%, and a purity of 70.8%.

[0021] In order to better prove that the process of the present invention can reduce the content of vomitoxin and fumonisin, and obtain a protein product with high yield and high purity, 12 comparative examples are given with reference to Example 3, as shown in the following content.

[0022] Comparative Example 1 The difference from Example 3 is that the temperature in step (2) is controlled at 30°C, and the other operations are the same. In step (5), 5.9 kg of protein product with a DON content of 1950 μg and a fumonisin content of 22060 μg per kg of protein is obtained, with a yield of 83% and a purity of 68%.

[0023] Comparative Example 2 The difference from Example 3 is that the temperature in step (2) is controlled at 45°C, and the other operations are the same. In step (5), 6.2 kg of protein product with a DON content of 2404 μg and a fumonisin content of 33011 μg per kg of protein is obtained, with a yield of 84% and a purity of 65.2%.

[0024] Comparative Example 3 The difference from Example 3 is that the pH in step (2) is controlled to be 3.2, and the other operations are the same. In step (5), 5.8 kg of protein product with a DON content of 3201 μg and a fumonisin content of 37720 μg per kg of protein is obtained, with a yield of 84.5% and a purity of 70.1%.

[0025] Comparative Example 4 The difference from Example 3 is that the pH in step (2) is controlled to be 4.8, and the other operations are the same. In step (5), 5.62 kg of protein product with a DON content of 2800 μg and a fumonisin content of 31022 μg per kg of protein is obtained, with a yield of 83% and a purity of 71%.

[0026] Comparative Example 5 The difference from Example 3 is that the filler in the resin column in step (2) is a macroporous resin, LX-T28, and the other operations are the same. In step (5), 5.9 kg of protein product with a DON content of 4302 μg and a fumonisin content of 47800 μg per kg of protein is obtained, with a yield of 78.4% and a purity of 64%.

[0027] Comparative Example 6 The difference from Example 3 is that no surfactant is added in step (3), and the remaining operations are the same. In step (5), 5.76 kg of protein product with a DON content of 2603 μg and a fumonisin content of 34100 μg per kg of protein is obtained, with a yield of 85.4% and a purity of 71.3%.

[0028] Comparative Example 7 The difference from Example 3 is that in step (3), the pH is controlled to be 6, and the other operations are the same. In step (5), 5.75 kg of protein product with a DON content of 3511 μg and a fumonisin content of 46089 μg per kg of protein is obtained, with a yield of 86% and a purity of 72%.

[0029] Comparative Example 8 The difference from Example 3 is that in step (3), the pH is controlled to be 7.5, and the other operations are the same. In step (5), 5.77 kg of protein product with a DON content of 4701 μg and a fumonisin content of 49833 μg per kg of protein is obtained, with a yield of 85.9% and a purity of 71.6%.

[0030] Comparative Example 9 The difference from Example 3 is that the temperature in step (3) is controlled at 45°C, and the other operations are the same. In step (5), 5.77 kg of protein product with a DON content of 3012 μg and a fumonisin content of 24200 μg per kg of protein is obtained, with a yield of 86.5% and a purity of 72.1%.

[0031] Comparative Example 10 The difference from Example 3 is that the temperature in step (3) is controlled at 65°C, and the other operations are the same. In step (5), 5.74 kg of protein product with a DON content of 4361 μg and a fumonisin content of 45303 μg per kg of protein is obtained, with a yield of 85.8% and a purity of 71.9%.

[0032] Comparative Example 11 The difference from Example 3 is that microwave treatment is omitted in step (4), and the other operations are the same. In step (5), 5.8 kg of protein product with a DON content of 3500 μg and a fumonisin content of 32066 μg per kg of protein is obtained, with a yield of 86.1% and a purity of 71.5%.

[0033] Comparative Example 12 The difference from Example 3 is that the compound enzyme in step (3) does not contain amylase, and the other operations are the same. In step (5), 6.1 kg of protein product with a DON content of 4122 μg and a fumonisin content of 40193 μg / kg of protein was obtained, with a yield of 87% and a purity of 68.6%.

[0034] 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 toxin content in corn soaking water by using complex enzymes in coordination with surfactants, characterized in that: The process comprises the following steps: (1) Take the corn soaking water after phytic acid adsorption, filter and collect the filtrate for later use; (2) taking the filtrate in step (1), passing it through a resin column after controlling the temperature and pH, and concentrating the collected effluent to obtain a concentrated solution for later use; (3) taking the concentrated solution in step (2), adding a composite enzyme and a surfactant, stirring and mixing, controlling the pH, temperature and reaction time, and setting the enzymatic solution after the reaction aside; the composite enzyme comprises glucose oxidase, amylase and Aspergillus niger amine oxidase, the activity of the glucose oxidase is 5000U / g, the activity of the amylase is 1000U / g, and the activity of the Aspergillus niger amine oxidase is 1000U / g; the surfactant is sodium dodecyl sulfate, and the amount of the surfactant is 0.8-1.0‰ of the volume of the concentrated solution; (4) taking the enzymatic hydrolysis solution in step (3), treating it with microwaves, adding activated carbon, and continuing to stir and mix, and the obtained solution is set aside; (5) The feed liquid in step (4) is concentrated and filtered, and the collected filtrate is dried to obtain a protein product having a vomitoxin content of no more than 930 μg and a fumonisin content of no more than 9250 μg per kilogram of protein.

2. The process of reducing the toxin content in corn soaking water by using complex enzymes in coordination with surfactants according to claim 1, characterized in that: In step (2), the filtrate is controlled at a temperature of 35-40°C and a pH of 3.8-4.2, and the filtrate enters the resin column at a flow rate of 1-2 BV / h; the filler in the resin column is a macroporous adsorption resin, and the model of the resin is Lanxiao Technology--LSA-900B.

3. The process of reducing the toxin content in corn soaking water by using complex enzymes in coordination with surfactants according to claim 1, characterized in that: The solid content of the concentrated solution in step (3) is 35-40wt%, the amount of the glucose oxidase used is 0.5-1.5‰ of the solid content of the concentrated solution, the amount of the amylase used is 0.15-0.2‰ of the solid content of the concentrated solution, and the amount of the Aspergillus niger amine oxidase used is 0.3-0.5‰ of the solid content of the concentrated solution.

4. The process of claim 1 for reducing the toxin content in corn soaking water by using a composite enzyme in coordination with a surfactant, characterized in that: In step (3), the temperature is controlled at 50-60°C, the pH is 6.5-7, and the reaction time is 4-6h.

5. The process of reducing the toxin content in corn soaking water by using complex enzymes in coordination with surfactants according to claim 1, characterized in that: The power of the microwave treatment in step (4) is 200-300 W, and the microwave treatment time is 3-5 min.

6. The process of claim 1 for reducing the toxin content in corn soaking water by using complex enzymes in coordination with surfactants, characterized in that: The amount of activated carbon added in step (4) is 0.5-1.0‰ of the solid content of the concentrated solution.