Process method for reducing toxin content in water-soluble protein from corn soaking water

Abstract

The invention relates to the technical field of corn soaking water treatment, in particular to a process method for reducing toxin content in water-soluble protein from corn soaking water, which comprises the following steps: collecting the corn soaking water adsorbing phytic acid, filtering by a nanofiltration membrane, and treating by an ultraviolet sterilization filter to obtain the toxin content in the water-soluble protein. The collected filtrate enters equipment filled with a zeolite layer, a resin layer and an activated aluminum oxide layer, ozone is introduced at the same time, a large amount of toxin can be effectively removed through oxidation of the ozone and adsorption of a composite adsorbent layer, the collected feed liquid is concentrated and filtered, and the collected filtrate is dried to obtain the toxin. The content of vomitoxin in each kilogram of protein does not exceed 890 micrograms, and the content of fumonisins in each kilogram of protein does not exceed 9210 micrograms. According to the process method, the content of vomitoxin and fumonisins in the protein is greatly reduced, and meanwhile, the yield, the yield and the purity of the protein are improved.

Description

Technical Field

[0001] The invention relates to the technical field of corn soaking water treatment, in particular to a process for reducing the toxin content in water-soluble protein derived from 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 leftovers after wet starch production, which contains effective ingredients such as dry matter, phytic acid, protein, lactic acid, calcium, and magnesium; corn is prone to mildew 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, and 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 potential safety hazards; although the prior art discloses a method of using an oxidant oxidation treatment and an adsorbent adsorption treatment, the above method has poor treatment effect and high toxin content. Therefore, in view of the above problems, it is necessary to develop a process method for reducing the toxin content in water-soluble protein from 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 existing technology, a process method for reducing the toxin content in water-soluble protein derived from corn soaking water is provided, and the process method can effectively reduce the content of vomitoxin and fumonisin in the water-soluble protein derived from corn soaking water.

[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 water-soluble protein derived from corn soaking water, the process comprising the following steps: (1) taking the corn soaking water after phytic acid adsorption, filtering it and then passing it through an ultraviolet sterilization filter to obtain a filtrate for use; (2) taking the filtrate in step (1), passing it through an adsorption device filled with a composite adsorbent layer and ozone treatment at the same time, and collecting the liquid for use; (3) The feed liquid in step (2) is concentrated, filtered, and the collected filtrate is then dried to obtain a protein product having a vomitoxin content of no more than 890 μg and a fumonisin content of no more than 9210 μg per kilogram of protein.

[0007] As an improved technical solution, a ceramic membrane with a pore size of 50 nm is used for filtration in step (1).

[0008] As an improved technical solution, when the ultraviolet sterilization filter is used in step (1), the wavelength is 253.7nm and the ultraviolet radiation dose is 1000-2000μw / cm 2 , and the clear liquid after filtering through the nanofiltration membrane enters the ultraviolet sterilization filter at a flow rate of 8-10L / h.

[0009] As an improved technical solution, the composite adsorbent layer in step (2) includes a zeolite layer, a resin layer and an activated alumina layer, the particle size of the zeolite in the zeolite layer is 300-500 microns, the particle size of the resin in the resin layer is 200-300 microns, the resin is a macroporous adsorption resin, and the model of the resin is Suqing DA201-E; the particle size of the activated alumina in the activated alumina layer is 200-300 microns, and the pore volume is 0.38-0.4cm 3 / g.

[0010] As an improved technical solution, in step (2), the zeolite layer is located at the upper part of the adsorption device, the resin layer is located in the middle part of the adsorption device, and the activated alumina layer is located at the lower part of the adsorption device, and the thickness ratio of the zeolite layer, the resin layer and the activated alumina layer is 3:4-5:2-3.

[0011] As an improved technical solution, in step (2), the filtrate enters from the upper side of the adsorption device at a flow rate of 3-5 L / h; the ozone enters from the lower side of the adsorption device, and the concentration of the ozone is 50-100 ml / L and the pressure is 0.2-0.3 MPa.

[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, and then filters it through a nanofiltration membrane, treats it with an ultraviolet sterilization filter, and the collected filtrate enters an adsorption device filled with a zeolite layer, a resin layer, and an activated alumina layer, and then introduces ozone. After oxidation by ozone and adsorption by the composite adsorbent layer, a large amount of toxins can be effectively removed. The collected feed liquid is then concentrated and filtered, and the collected filtrate is then dried to obtain a protein product with a vomitoxin content of no more than 890 μg and a fumonisin content of no more than 9210 μg per kilogram of protein. The above process method greatly reduces the content of vomitoxin and fumonisin in the protein, while improving the yield, yield and purity of the protein. 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 toxin content in water-soluble protein derived from 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, filter the collected clear liquid through a ceramic membrane with a pore size of 50nm, and enter the ultraviolet sterilization filter at a flow rate of 8L / h (wavelength 253.7nm, ultraviolet radiation dose 1000μw / cm 2 ), the obtained filtrate 91L is reserved; (2) 91 L of the filtrate in step (1) was taken and fed from the upper feed port at a flow rate of 3 L / h into a composite adsorbent layer filled with a total volume of 10 L (including a zeolite layer, a resin layer and an activated alumina layer arranged in order from top to bottom inside the adsorption device, the thickness ratio of the zeolite layer, the resin layer and the activated alumina layer being 3:4:2; the particle size of the zeolite in the zeolite layer being 300-500 μm; the particle size of the resin in the resin layer being 200-300 μm, and the resin being a macroporous adsorption resin - Suqing DA201-E; the particle size of the activated alumina in the activated alumina layer being 200-300 μm, and the pore volume being 0.38-0.4 cm 3 / g) inside the adsorption device, ozone with a concentration of 50ml / L and a pressure of 0.2MPa enters the adsorption device from the lower air inlet, and after the feeding is completed, the composite adsorbent layer is rinsed with purified water, and 100L of the collected feed liquid is used for standby; (3) 100 L of the feed solution in step (2) was taken and concentrated by heating to obtain a concentrated solution with a solid content of 45 wt%. The filtrate was collected after filtering through a plate and frame filter and then dried to obtain 6.3 kg of a protein product with a vomitoxin content of 883 μg and a fumonisin content of 9210 μg per kilogram of protein, a yield of 87.3%, and a purity of 73.2%. Example 2

[0015] A process for reducing the toxin content in water-soluble protein derived from 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, filter the collected clear liquid through a ceramic membrane with a pore size of 50nm, and enter the ultraviolet sterilization filter at a flow rate of 8.5L / h (wavelength 253.7nm, ultraviolet radiation dose 1200μw / cm 2 ), the obtained filtrate 92L is reserved; (2) 92 L of the filtrate in step (1) was taken and fed from the upper feed port at a flow rate of 3.5 L / h into a composite adsorbent layer filled with a total volume of 10 L (including a zeolite layer, a resin layer and an activated alumina layer arranged in order from top to bottom inside the adsorption device, the thickness ratio of the zeolite layer, the resin layer and the activated alumina layer being 3:4.5:2.5; the particle size of the zeolite in the zeolite layer being 300-500 μm; the particle size of the resin in the resin layer being 200-300 μm, and the resin being a macroporous adsorption resin---Suqing DA201-E; the particle size of the activated alumina in the activated alumina layer being 200-300 μm, and the pore volume being 0.38-0.4 cm 3 / g) inside the adsorption device, ozone with a concentration of 65ml / L and a pressure of 0.25MPa enters the adsorption device from the lower air inlet, and after the feeding is completed, the composite adsorbent layer is rinsed with purified water, and 100L of the collected feed liquid is used for standby; (3) 100 L of the feed solution in step (2) was taken and concentrated by heating to obtain a concentrated solution with a solid content of 47 wt%. The filtrate was collected after filtering through a plate and frame filter and then dried to obtain 6.29 kg of a protein product with a vomitoxin content of 801 μg and a fumonisin content of 7909 μg per kilogram of protein, a yield of 87.9%, and a purity of 73.8%. Example 3

[0016] A process for reducing the toxin content in water-soluble protein derived from 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, filter the collected clear liquid through a ceramic membrane with a pore size of 50nm, and enter the ultraviolet sterilization filter at a flow rate of 9L / h (wavelength 253.7nm, ultraviolet radiation dose 1500μw / cm 2 ), the obtained filtrate 91.5L is reserved; (2) 91.5 L of the filtrate in step (1) was taken and fed from the upper feed port at a flow rate of 4 L / h into a composite adsorbent layer filled with a total volume of 10 L (including a zeolite layer, a resin layer and an activated alumina layer arranged in order from top to bottom inside the adsorption device, the thickness ratio of the zeolite layer, the resin layer and the activated alumina layer being 3:5:3; the particle size of the zeolite in the zeolite layer being 300-500 μm; the particle size of the resin in the resin layer being 200-300 μm, and the resin being a macroporous adsorption resin---Suqing DA201-E; the particle size of the activated alumina in the activated alumina layer being 200-300 μm, and the pore volume being 0.38-0.4 cm 3 / g) inside the adsorption device, ozone with a concentration of 75ml / L and a pressure of 0.3MPa enters the adsorption device from the lower air inlet, and after the feeding is completed, the composite adsorbent layer is rinsed with purified water, and 100L of the collected feed liquid is used for standby; (3) 100 L of the feed solution in step (2) was taken and concentrated by heating to obtain a concentrated solution with a solid content of 48 wt%. The filtrate was filtered through a plate and frame filter and then dried to obtain 6.23 kg of a protein product with a vomitoxin content of 612 μg and a fumonisin content of 6501 μg per kilogram of protein, a yield of 88.6%, and a purity of 75.1%. Example 4

[0017] A process for reducing the toxin content in water-soluble protein derived from 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, filter the collected clear liquid through a ceramic membrane with a pore size of 50nm, and enter the ultraviolet sterilization filter at a flow rate of 9.5L / h (wavelength 253.7nm, ultraviolet radiation dose 1800μw / cm 2 ), the obtained filtrate 91.3L is reserved; (2) 91.3 L of the filtrate in step (1) was taken and fed from the upper feed port at a flow rate of 4.5 L / h into a composite adsorbent layer filled with a total volume of 10 L (including a zeolite layer, a resin layer and an activated alumina layer arranged in order from top to bottom inside the adsorption device, the thickness ratio of the zeolite layer, the resin layer and the activated alumina layer being 3:5:3; the particle size of the zeolite in the zeolite layer being 300-500 μm; the particle size of the resin in the resin layer being 200-300 μm, and the resin being a macroporous adsorption resin---Suqing DA201-E; the particle size of the activated alumina in the activated alumina layer being 200-300 μm, and the pore volume being 0.38-0.4 cm 3 / g) inside the adsorption device, ozone with a concentration of 85ml / L and a pressure of 0.3MPa enters the adsorption device from the lower air inlet, and after the feeding is completed, the composite adsorbent layer is rinsed with purified water, and 100L of the collected feed liquid is used for standby; (3) 100 L of the feed solution in step (2) was taken and concentrated by heating to obtain a concentrated solution with a solid content of 49 wt%. The filtrate was collected after plate and frame filtration and then dried to obtain 6.07 kg of a protein product with a vomitoxin content of 711 μg and a fumonisin content of 7334 μg per kilogram of protein, a yield of 85.4%, and a purity of 74.3%. Example 5

[0018] A process for reducing the toxin content in water-soluble protein derived from 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, filter the collected clear liquid through a ceramic membrane with a pore size of 50nm, and enter the ultraviolet sterilization filter at a flow rate of 10L / h (wavelength 253.7nm, ultraviolet radiation dose 2000μw / cm 2 ), the obtained filtrate 91.8L is reserved; (2) 91.8 L of the filtrate in step (1) was taken and fed from the upper feed port at a flow rate of 5 L / h into a composite adsorbent layer filled with a total volume of 10 L (including a zeolite layer, a resin layer and an activated alumina layer arranged in order from top to bottom inside the adsorption device, the thickness ratio of the zeolite layer, the resin layer and the activated alumina layer being 3:5:3; the particle size of the zeolite in the zeolite layer being 300-500 μm; the particle size of the resin in the resin layer being 200-300 μm, and the resin being a macroporous adsorption resin---Suqing DA201-E; the particle size of the activated alumina in the activated alumina layer being 200-300 μm, and the pore volume being 0.38-0.4 cm 3 / g) inside the adsorption device, ozone with a concentration of 100ml / L and a pressure of 0.3MPa enters the adsorption device from the lower air inlet, and after the feeding is completed, the composite adsorbent layer is rinsed with purified water, and 100L of the collected feed liquid is reserved for use; (3) 100 L of the feed solution in step (2) was taken and concentrated by heating to obtain a concentrated solution with a solid content of 50 wt%. The filtrate was filtered through a plate and frame filter and then dried to obtain 6.16 kg of a protein product with a vomitoxin content of 820 μg and a fumonisin content of 7920 μg per kilogram of protein, a yield of 84%, and a purity of 72%.

[0019] In order to better prove that the process method of the present invention has a good technical effect, 9 comparative examples are given with reference to Example 3, and the details are shown in the following content.

[0020] Comparative Example 1 The difference from Example 3 is that in step (1), the corn soaking water is only filtered by a nanofiltration membrane and is not treated by an ultraviolet sterilization filter, and the remaining operations are the same. In step (3), 5.72 kg of a protein product with a vomitoxin content of 2802 μg and a fumonisin content of 34005 μg per kilogram of protein is obtained, with a yield of 86% and a purity of 72.7%.

[0021] Comparative Example 2 The difference from Example 3 is that the composite adsorbent layer in step (2) does not contain a resin layer, the thickness ratio of the zeolite layer to the activated alumina layer is 1:1, and the other operations are the same. In step (3), 5.71 g of protein product with a DON content of 2104 μg and a fumonisin content of 24000 μg per kilogram of protein was obtained, with a yield of 82.1% and a purity of 69.4%.

[0022] Comparative Example 3 The difference from Example 3 is that the composite adsorbent layer in step (2) does not contain an activated alumina layer, the thickness ratio of the zeolite layer to the resin layer is 3:5, and the other operations are the same. In step (3), 5.8 kg of protein product with a vomitoxin content of 1990 μg and a fumonisin content of 23055 μg per kilogram of protein was obtained, with a yield of 83% and a purity of 69%.

[0023] Comparative Example 4 The difference from Example 3 is that the resin in the resin layer in step (2) is a macroporous adsorption resin--LX-T83, and the other operations are the same. In step (3), 5.6 kg of protein product with a DON content of 2247 μg and a fumonisin content of 23780 μg per kg of protein is obtained, with a yield of 79.1% and a purity of 68.2%.

[0024] Comparative Example 5 The difference from Example 3 is that the thickness ratio of the zeolite layer, the resin layer and the activated alumina layer in step (2) is 2:3:2, and the other operations are the same. In step (3), 5.57 kg of protein product with a vomitoxin content of 1690 μg and a fumonisin content of 18440 μg per kilogram of protein is obtained, with a yield of 81% and a purity of 70.3%.

[0025] Comparative Example 6 The difference from Example 3 is that the thickness ratio of the zeolite layer, the resin layer and the activated alumina layer in step (2) is 3:7:3, and the other operations are the same. In step (3), 5.58 kg of protein product with a DON content of 2089 μg and a fumonisin content of 16004 μg per kg of protein is obtained, with a yield of 82% and a purity of 71%.

[0026] Comparative Example 7 The difference from Example 3 is that in step (2), the filtrate enters the upper side of the adsorption device at a flow rate of 2.5 L / h, and the other operations are the same. In step (3), 5.7 kg of protein product with a vomitoxin content of 3735 μg and a fumonisin content of 29500 μg per kilogram of protein was obtained, with a yield of 84% and a purity of 71.2%.

[0027] Comparative Example 8 The difference from Example 3 is that in step (2), the filtrate enters the upper side of the adsorption device at a flow rate of 5.5 L / h, and the other operations are the same. In step (3), 5.59 kg of protein product with a DON content of 5460 μg and a fumonisin content of 48801 μg per kg of protein is obtained, with a yield of 83.3% and a purity of 72%.

[0028] Comparative Example 9 The difference from Example 3 is that in step (1), the clear liquid after the corn soaking water is filtered through the nanofiltration membrane enters the ultraviolet sterilization filter at a flow rate of 12 L / h, and the rest of the operations are the same. In step (3), 5.63 kg of protein product with a vomitoxin content of 3202 μg and a fumonisin content of 28901 μg per kilogram of protein is obtained, with a yield of 83% and a purity of 71.2%.

[0029] It should be noted that the adsorption device filled with a composite adsorbent layer (purchased from the manufacturer) has a specific structure: including a shell, a feed port is provided at the top of the shell, an ozone inlet is provided on one side of the lower part of the shell, and a discharge is provided at the bottom of the shell. A zeolite layer, a resin layer and an activated alumina layer are provided in sequence from top to bottom inside the shell. Since the specific structure of the adsorption device can be known from the description, the drawings of the adsorption device are not provided.

[0030] 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 water-soluble protein derived from corn soaking water, characterized in that: The process comprises the following steps: (1) taking the corn soaking water after phytic acid adsorption, filtering it and then passing it through an ultraviolet sterilization filter to obtain a filtrate for use; (2) The filtrate in step (1) is taken and treated simultaneously with ozone by an adsorption device filled with a composite adsorbent layer, and the collected liquid is set aside; the composite adsorbent layer comprises a zeolite layer, a resin layer and an activated alumina layer, the particle size of the zeolite in the zeolite layer is 300-500 microns, the particle size of the resin in the resin layer is 200-300 microns, the resin is a macroporous adsorption resin, and the model of the resin is DA201-E; the particle size of the activated alumina in the activated alumina layer is 200-300 microns, and the pore volume is 0.38-0.4cm 3 / g; the zeolite layer is located above the interior of the adsorption device, the resin layer is located in the middle of the interior of the adsorption device, the activated alumina layer is located below the interior of the adsorption device, and the thickness ratio of the zeolite layer, the resin layer and the activated alumina layer is 3:4-5:2-3; (3) The feed liquid in step (2) is concentrated, filtered, and the collected filtrate is then dried to obtain a protein product having a vomitoxin content of no more than 890 μg and a fumonisin content of no more than 9210 μg per kilogram of protein.

2. A process for reducing the toxin content in water-soluble protein derived from corn soaking water according to claim 1, characterized in that: In step (1), a ceramic membrane with a pore size of 50 nm is used for filtration.

3. A process for reducing the toxin content in water-soluble protein derived from corn soaking water according to claim 1, characterized in that: When the ultraviolet sterilization filter is used in step (1), the wavelength is 253.7nm and the ultraviolet radiation dose is 1000-2000μw / cm 2 , and the clear liquid after filtering through the nanofiltration membrane enters the ultraviolet sterilization filter at a flow rate of 8-10L / h.

4. The process for reducing the toxin content in water-soluble protein derived from corn soaking water according to claim 1, characterized in that: In step (2), the filtrate enters from the upper side of the adsorption device at a flow rate of 3-5 L / h; the ozone enters from the lower side of the adsorption device, and the concentration of the ozone is 50-100 ml / L and the pressure is 0.2-0.3 MPa.