WO2024001031A1 - 一种高压交流脉冲电场辅助制备菜籽油的装置和方法 - Google Patents

一种高压交流脉冲电场辅助制备菜籽油的装置和方法 Download PDF

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WO2024001031A1
WO2024001031A1 PCT/CN2022/135462 CN2022135462W WO2024001031A1 WO 2024001031 A1 WO2024001031 A1 WO 2024001031A1 CN 2022135462 W CN2022135462 W CN 2022135462W WO 2024001031 A1 WO2024001031 A1 WO 2024001031A1
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main body
electric field
enzyme
layer
rapeseed oil
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French (fr)
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徐勇将
陈小颖
刘元法
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Future Food Nanjing Fuzhe Research Institute Co Ltd
Jiangnan University
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Future Food Nanjing Fuzhe Research Institute Co Ltd
Jiangnan University
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    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B1/00—Production of fats or fatty oils from raw materials
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B1/00—Production of fats or fatty oils from raw materials
    • C11B1/02—Pretreatment
    • C11B1/025—Pretreatment by enzymes or microorganisms, living or dead

Definitions

  • the invention relates to the technical field of oil processing, and in particular to a device and method for preparing rapeseed oil assisted by a high-voltage AC pulse electric field.
  • Rapeseed oil has a mellow smell and rich nutrition.
  • the human body's absorption rate of rapeseed oil is very high, up to 99%. It has the functions of replenishing deficiency, moisturizing the intestines, clearing the liver and promoting gallbladder, promoting brain development, helping the eyes to resist the stimulation of various bright lights, preventing senile eye diseases and amblyopia in children.
  • High-oleic acid rapeseed oil is rich in unsaturated fatty acids such as oleic acid and linoleic acid, as well as vitamin E, which can soften blood vessels and delay aging.
  • the sterol content is also higher than that of common vegetable oils such as soybean oil, and there are many types.
  • rapeseed oil Some sterols also have special physiological functions.
  • the phospholipids of rapeseed oil are beneficial to the development of blood vessels, nerves, and brain. Rapeseed oil has little or almost no cholesterol.
  • the saturated fatty acid content of low erucic acid rapeseed oil is very low, the oleic acid content reaches more than 60%, and there are reasonable contents of linoleic acid and linolenic acid. Therefore, low erucic acid rapeseed oil is called "the healthiest edible vegetable oil" .
  • Rapeseed polyphenols are an important secondary metabolite unique to rapeseed. They have biological activities such as anti-tumor, hypoglycemic, bacteriostatic, and scavenging free radicals. They are a potentially important natural antioxidant.
  • Aqueous enzymatic methods have been attempted for oil extraction from many oleaginous seeds/fruits at laboratory and pilot industrial scale levels. Compared to traditional techniques, the process is gentle and safe as organic solvents are completely avoided. Despite these advantages, the aqueous enzymatic method has significant disadvantages. First of all, the current price of enzyme preparations is still high, which increases production costs. As a result, aqueous enzyme methods have mostly stayed in the laboratory research and pilot stages for many years, and their industrial applications have been restricted. Secondly, in the process of extracting vegetable oils, due to the hard, thick and complex cell walls, the synergistic action of multiple enzymes is often required, which results in poor wall-breaking effect of some oils and low oil extraction rate. In addition, during the aqueous enzymatic oil extraction process, the residual oil rate in the emulsified layer and residue layer formed is high, resulting in a low oil extraction rate.
  • the purpose of the present invention is to overcome the shortcomings of the existing technology and provide a device and method for preparing strong-flavor rapeseed oil through high-voltage AC pulse electric field-assisted catalysis, which has the characteristics of low processing temperature, maximum retention of the flavor of rapeseed, and fertility.
  • bioactive substances such as phenols, polyphenols, antioxidants and phytosterols.
  • the AC pulsed electric field is used to change the permeability of plant seed cell membranes and increase the oil yield.
  • the AC pulse electric field can effectively increase the vibration and collision of droplets in the oil, improve the coalescence efficiency of the droplets, and have a good demulsification effect.
  • immobilized enzymes are used instead of traditional free forms of enzymes. Compared with the free form of enzyme, it not only has good temperature and pH adaptability, but can also be recycled and reused through simple methods with less loss of enzyme activity. And it is easier to separate and purify from the product.
  • the first object of the present invention is to provide a device for preparing aromatic rapeseed oil through high-voltage AC pulse electric field-assisted extraction, including a main body (1); the main body (1) is provided with a servo motor (2), a feed Mouth (3), steel plate (4), mixing rod (5), rotating baffle (6), screening hole (7), tilt plate (8), pH detector (9), temperature detector (10), heating Block (11), magnetic enzyme recovery tank (12), filter tank (13), liquid storage tank (14), controller (15), acid addition pipe (16), water inlet pipe (19) and outlet (20 ).
  • the main body (1) includes a first layer, a second layer, a third layer, and a fourth layer from top to bottom. Rotating baffles are provided between the layers.
  • the main body (1) The first, second and fourth layers are symmetrically equipped with steel plates (4) inside; a servo motor (2) is installed inside the main body (1), and a mixing rod (5) is connected to the lower end of the servo motor (2).
  • a heating block (11) is installed inside the second and third layers.
  • a pH detector (9) and a temperature detector (10) are installed on the inner walls of the second and third layers. The main body (1) rotates between each layer.
  • Screening holes (7) are provided on the left and right sides of the baffle, an inclined plate (8) is provided at the lower end of the first layer of screening holes of the main body (1), and a surface magnetic enzyme recovery tank is provided at the lower end of the second and third layer screening holes of the main body (1).
  • (12) in the form of a slider for easy removal, the main body (1) is provided with a filter tank (13), which is also installed at the bottom in the form of a slider, and the bottom of the filter tank (13) has a filter screen.
  • the main body (1) also includes an alkali addition pipeline (17) and an enzyme addition pipeline (18).
  • connection between the main body (1) and the servo motor (2) is a fixed connection, and the mixing rods (5) are evenly distributed along the vertical centerline of the servo motor.
  • the body (1) is internally coated with an internal insulating material.
  • the steel plates (4) are symmetrically distributed on the insulating material inside the main body, and a controller (15) is provided on the front surface of the main body.
  • the connection method is electrical connection.
  • the screening holes (7) are evenly distributed along both sides of the rotating baffle (6), and the rotating baffle (6) is electrically connected to the controller (15), and the controller (15) 15) Control the rotation of the rotating baffle (6).
  • the heating blocks (11) are annularly symmetrically distributed inside the main body (1), and the connection between the controller (15) and the heating block (11) is an electrical connection.
  • the magnetic enzyme recovery tank (12) is distributed at the lower end of the screening hole (7), the magnetic enzyme recovery tank (12) is provided with a magnet, and the magnetic enzyme recovery tank (12) and the main body (1 ) form a sliding structure.
  • the filter tank (13) is distributed at the bottom of the main body (1), and a filter screen is installed on the bottom layer.
  • a sliding structure is formed between the filter tank (13) and the main body (1).
  • the discharge port (20) is located on the side of the liquid storage tank (14) and is connected to a pump to discharge the liquid in the liquid storage tank (14) from the main body (1).
  • the second purpose of this application document is to use the above device to provide a method for preparing aromatic rapeseed oil assisted by a high-voltage AC pulse electric field, which includes the following steps:
  • the user when using the above device to prepare rapeseed oil, the user first inserts the enzyme recovery tank (12) and the filter tank (13) into the main body (1), and then inserts the crushed rapeseed into the main body (1).
  • the material port (3) is poured into the main body (1).
  • the user turns on the servo motor (2).
  • the servo motor (2) and the mixing rod (5) cooperate with each other to make the material evenly mixed, and then pass through
  • the controller (15) commands a high-voltage AC pulse electric field to be formed between the steel plates (4) on the first layer of the main body (1) to destroy the plant cell walls and release more oil;
  • the rotating baffle (6) set up subsequently opens the exposed screening hole (7), and the material slides into the second layer of the main body (1) along the inclined plate (8), and the water inlet pipe (19) is commanded to open through the controller (15).
  • a high-voltage AC pulse electric field is formed between the second steel plate (4) of the main body (1), and the temperature and pH of the feed liquid are monitored through the pH detector (9) and temperature detector (10).
  • the controller Open the set acid adding pipe (16) and alkali adding pipe (17) to adjust the pH, and at the same time command the heating block (12) to open and adjust the temperature, and then release the immobilized cellulase through the set enzyme adding pipe (18) for processing;
  • the set rotating baffle (6) opens the exposed screening hole (7), and the material slides along the inclined surface of the enzyme recovery tank (12) into the third layer of the main body (1), where the immobilized cellulase is due to the recovery tank (12) The surface is magnetic and adheres to the recovery tank.
  • the temperature and pH of the feed liquid are monitored through the set pH detector (9) and temperature detector (10).
  • the controller opens the set acid addition pipe (16) Adjust the pH with the alkali adding pipe (17), and at the same time command the heating block (12) to open and adjust the temperature, and then release the immobilized alkaline endoprotease through the set enzyme adding pipe for processing;
  • the set rotating baffle (6) opens the exposed screening hole (7), and the material slides along the inclined surface of the recovery tank (12) into the fourth layer of the main body (1), where the immobilized alkaline endoprotease is recovered due to The surface of the tank (12) is magnetic and attached to the recovery tank.
  • a high-voltage AC pulse electric field is formed between the steel plates (4) on the fourth layer of the main body (1) to achieve the effect of demulsification;
  • the set rotating baffle (6) opens to expose the filter tank (13).
  • the material liquid passes through the liquid storage tank (14) and follows the discharge port (20)
  • the solid matter flows out and the solid matter adheres to the filter tank (13).
  • a high-voltage alternating current pulsed electric field is used to increase the permeability of the rapeseed cell plasma membrane through electrical stimulation, destroy the plant cell structure, and increase the dissolution pathways of intracellular substances.
  • the electric field intensity is 25-35kV/cm
  • the material residence time is 180-200s
  • the pulse frequency is 750-850Hz
  • the duty cycle is 0.5-0.6.
  • step 3 a pulsed electric field is used instead of the traditional high-temperature enzyme inactivation process to avoid the loss of part of the flavor and nutrients.
  • step 3 the ratio of oil to water is 1:3-5 (w/v, g/mL).
  • step 3 the electric field intensity is 65-75kV/cm, the pulse frequency is 750-850Hz, and the duty cycle is 0.5-0.6.
  • the immobilized cellulase used is immobilized with ferric oxide nanoparticles containing carriers.
  • step 4 the temperature of enzymatic hydrolysis is 40 to 45°C, the pH is 7.5 to 8.0, and the mixture is stirred for 1 to 2 hours.
  • step 5 the immobilized alkaline endoprotease used is immobilized with carrier-containing ferroferric oxide nanoparticles.
  • step 5 the temperature of enzymatic hydrolysis is 60-65°C, the pH is 8.5-9.0, and the mixture is stirred for 4-4.5 hours.
  • a pulsed electric field is used for demulsification treatment, in which the electric field intensity is 35-40kV/cm, the pulse frequency is 550-600Hz, and the duty cycle is 0.6-0.7
  • step 6 the preferred electric field intensity is 40kV/cm, the pulse frequency is 600Hz, and the duty cycle is 0.7.
  • the centrifugation speed is 4500-6000 r/min, and the centrifugation is performed at room temperature for 10-20 minutes.
  • the present invention uses a water-enzyme method to extract rapeseed oil, and uses biological enzymes to degrade the cell structure of the oil tissue and the ultrastructure of lipopolysaccharide and lipoprotein, thereby increasing the fluidity of the oil in the oil tissue and freeing it from the oil. It further promotes phenols and other substances to enter the oil, and due to the protection of the water phase and emulsion layer during the extraction process, some proteins and phenolic substances are protected from oxidation, thereby further improving the oxidative stability, shelf life, nutrition, flavor, and sensory properties of the oil. etc. performance.
  • high-voltage AC pulsed electric field treatment technology is applied three times.
  • the oil seeds are treated with high-voltage AC pulsed electric field, replacing the traditional steaming and frying process.
  • the conditions are mild and high-voltage current is generated through discharge to destroy plant cells and change Its permeability enables the substances in cells to effectively flow out, promotes the release of volatile components, and enhances the taste of oil, thereby improving the oil extraction rate and oil flavor in the subsequent pressing process.
  • the mixed system of oil and water is treated with high-voltage AC pulsed electric field to make it more evenly dispersed in the water.
  • the instantaneous pulsed electric field is used to act on the microbial cells, causing the cell membrane to form pores, increase the permeability, expand the cells, and eventually rupture. Instead, it inactivates microorganisms and at the same time inactivates the enzymes contained in the system.
  • high-voltage AC pulsed electric field is a cold treatment that can preserve the inherent components of rapeseed while sterilizing and sterilizing enzymes, saving energy consumption.
  • the third pulsed electric field treatment can also effectively increase the vibration and collision of droplets in the oil, improve the coalescence efficiency of the droplets, and play a role in demulsification. It can also be adjusted according to the oil working conditions. Electric field strength, pulse frequency, duty cycle and other parameters to obtain the optimal demulsification effect.
  • the enzyme used in the present invention is a self-made immobilized enzyme.
  • Cellulase and alkaline endoprotease are immobilized with ferric oxide nanoparticles containing carriers. Due to their magnetic properties, they are easy to recover and can realize the reuse of enzymes. , reduce production costs and improve production efficiency.
  • the device of the present invention can make the rapeseed evenly mixed by cooperating with the servo motor and the mixing rod, and the rotary baffle and the filter hole can cooperate with each other to control the processing time and flow rate.
  • the enzyme recovery efficiency is improved, and the filter tank is used to remove solids, reducing the difficulty of the centrifugal operation and preventing impurities from affecting the purity of the subsequent oil.
  • the sliding structure can facilitate its cleaning and replace.
  • Figure 1 is a process flow diagram of the method of the present invention.
  • Figure 5 is a schematic structural diagram of the device of the present invention.
  • Figure 6 is an appearance view of the device of the present invention.
  • Figure 7 is a schematic cross-sectional view of the device of the present invention.
  • the color determination of rapeseed oil refers to GB/T 22460-2008 "Determination of the color of Lovibond in animal and vegetable oils and fats"; the acid value determination refers to GB/T 5530-2005 “Determination of the acid value and acidity of animal and vegetable oils and fats”; the determination of peroxide value refers to GB/T 5538-2005 “Determination of peroxide value of oils and fats”; moisture and volatile content refer to GB/T 5528-2008.
  • the determination of oxidative stability refers to NY/T 2001-2011 "Determination of oxidative stability of rapeseed oil, accelerated oxidation test”; the determination of polyphenol content refers to LS/T 6119-2017 "Spectrophotometric method for the determination of polyphenols in vegetable oils. ⁇ ;
  • the method for measuring the demulsification rate is as follows: weigh 5g of rapeseed emulsion in a 50mL beaker, and take it out after being treated with a high-voltage AC pulse electric field of a certain electric field intensity, electric field frequency and duty cycle. Centrifuge at 4500r/min for 10 minutes at room temperature to obtain free oil, water phase mixture and residue.
  • the demulsification rate is calculated according to the following formula (1).
  • the oil production rate is calculated according to formula (2):
  • Example 1 A device for preparing aromatic rapeseed oil through high-voltage AC pulse electric field-assisted catalytic extraction
  • the main body (1) is provided with a servo motor (2), a feed port (3), a steel plate (4), and a mixing rod (5) , rotating baffle (6), screening hole (7), tilt plate (8), pH detector (9), temperature detector (10), heating block (11), magnetic enzyme recovery tank (12), filter tank (13), liquid storage tank (14), controller (15), acid addition pipe (16), water inlet pipe (19) and outlet (20).
  • the main body (1) includes the first layer, the second layer, the third layer and the fourth layer from top to bottom. Rotating baffles are provided between the layers.
  • the first, second and fourth layers of the main body (1) are symmetrically installed inside.
  • the second and third layers are equipped with heating block (11), the inner walls of the second and third layers are equipped with a pH detector (9) and a temperature detector (10), and screening holes (7) are provided on the left and right sides of the rotating baffle between each layer of the main body (1) ), the main body (1) is provided with an inclined plate (8) at the lower end of the first layer of screening holes, and the lower end of the second and third layer screening holes of the main body (1) is provided with a surface magnetic enzyme recovery tank (12), which is in the form of a slider for easy removal. , the main body (1) is provided with a filter tank (13), which is also installed at the bottom in the form of a slider. The bottom of the filter tank (13) has a filter screen.
  • the main body (1) also includes an alkali adding pipeline (17) and an enzyme adding pipeline (18).
  • connection between the main body (1) and the servo motor (2) is a fixed connection, and the mixing rods (5) are evenly distributed along the vertical center line of the servo motor.
  • the body (1) is internally coated with internal insulating material.
  • the steel plate (4) is symmetrically distributed on the insulating material inside the main body, and a controller (15) is provided on the front surface of the main body.
  • the connection between the controller (15) and the steel plate (4) is electrical connection.
  • the screening holes (7) are evenly distributed along both sides of the rotating baffle (6).
  • the rotating baffle (6) is electrically connected to the controller (15), and the controller (15) controls the rotation of the rotating baffle (6).
  • the heating block (11) is annularly symmetrically distributed inside the main body (1), and the connection between the controller (15) and the heating block (11) is electrical connection.
  • the magnetic enzyme recovery tank (12) is distributed at the lower end of the screening hole (7).
  • the magnetic enzyme recovery tank (12) is provided with a magnet, and a sliding structure is formed between the magnetic enzyme recovery tank (12) and the main body (1).
  • the filter tank (13) is distributed at the bottom of the main body (1), and the bottom layer is equipped with a filter.
  • a sliding structure is formed between the filter tank (13) and the main body (1).
  • the discharge port (20) is located on the side of the liquid storage tank (14) and is connected to the pump to discharge the liquid in the liquid storage tank (14) from the main body (1).
  • the rotating baffle (6) set up subsequently opens the exposed screening hole (7), and the material slides into the second layer of the main body (1) along the inclined plate (8), and the water inlet pipe (19) is commanded to open through the controller (15).
  • a high-voltage AC pulse electric field is formed between the second steel plate (4) of the main body (1), and the temperature and pH of the feed liquid are monitored through the pH detector (9) and temperature detector (10).
  • the controller Open the set acid adding pipe (16) and alkali adding pipe (17) to adjust the pH, and at the same time command the heating block (12) to open and adjust the temperature, and then release enzyme A through the set enzyme adding pipe (18).
  • the set rotating baffle (6) opens the exposed screening hole (7), and the material slides along the inclined surface of the enzyme recovery tank (12) into the third layer of the main body (1).
  • enzyme A due to the recovery tank (12) ) surface is magnetic and adheres to the recovery tank.
  • the temperature and pH of the feed liquid are monitored through the set pH detector (9) and temperature detector (10).
  • the controller opens the set acid addition pipe (16) and alkali Add the pipe (17) to adjust the pH, and at the same time command the heating block (12) to turn on and adjust the temperature, and then release enzyme B through the set enzyme adding pipe.
  • the rotating baffle (6) After processing for a period of time, the rotating baffle (6) is set to open the exposed screening hole (7), and the material slides along the inclined surface of the recovery tank (12) into the fourth layer of the main body (1), in which the enzyme B is The surface is magnetic and adheres to the recovery tank. Through the command of the controller (15), a high-voltage AC pulse electric field is formed between the steel plates (4) on the fourth layer of the main body (1) to achieve the effect of demulsification. After processing for a period of time, the set rotating baffle (6) opens to expose the filter tank (13). Under the action of the external pump of the main body (1), the material liquid flows out through the liquid storage tank (14) and along the discharge port (20). , the solid matter adheres to the filter tank (13). After use, close the device, open the enzyme recovery tank (12) and the filter tank (13), and make it convenient to process the solid residue and enzyme, thus completing the entire process. The use process of oil making equipment.
  • the magnetic microspheres After mixing evenly, use a syringe to inject the ferromagnetic fluid into the 10wt% CaCl 2 aqueous solution to prepare magnetic microspheres. . After the magnetic microspheres were soaked for 1 hour, they were washed with distilled water to remove free Ca 2+ adhered to the surface, and then cross-linked with 0.5% glutaraldehyde for 1.5 hours, and then washed with distilled water. Finally, the microspheres were incubated at 4°C overnight to harden. Dry at 35°C for 12 hours to obtain the immobilized enzyme.
  • the first high-voltage AC pulse electric field treatment The crushed rapeseed is subjected to high-voltage AC pulse electric field pretreatment.
  • the intensity of the pulse electric field is 25kV/cm
  • the material residence time is 180s
  • the pulse frequency is 850Hz
  • the duty cycle is 0.5.
  • the second high-voltage AC pulsed electric field treatment Mix 5 grams of treated rapeseed and distilled water at a mass ratio of 1:3 (w/v, g/mL). The mixture was subjected to high-voltage AC pulse electric field treatment, with a voltage pulse electric field intensity of 75 kV/cm, a pulse frequency of 850 Hz, and a duty cycle of 0.5.
  • 5Second enzyme treatment Lower the temperature to 60°C, adjust the pH to 9.0, add immobilized alkaline endoprotease, and mix and stir for 4 hours. After the enzymatic hydrolysis is completed, the magnetically immobilized alkaline endoprotease is separated.
  • the third high-voltage pulse treatment The mixture after separation of the immobilized enzyme is subjected to high-voltage AC pulse electric field treatment, with a voltage pulse electric field intensity of 40kV/cm, a pulse frequency of 600Hz, and a duty cycle of 0.7.
  • the third high-voltage pulse treatment The mixture after separation of the immobilized enzyme is subjected to high-voltage AC pulse electric field treatment.
  • the high-voltage pulse electric field intensity is 15, 20, 25, 30, 35, 40, 45, 50, 55, 60kV/ cm, pulse frequency 600Hz, duty cycle 0.7;
  • the third high-voltage pulse treatment The mixture after separation of the immobilized enzyme is subjected to high-voltage AC pulse electric field treatment, with a high-voltage AC pulse electric field intensity of 40kV/cm and a pulse frequency of 300, 350, 400, 450, 500, 550, 600, 650, 700, 750Hz, duty cycle 0.7;
  • the third high-voltage pulse treatment The mixture after separation of the immobilized enzyme is treated with a high-voltage AC pulse electric field.
  • the intensity of the high-voltage AC pulse electric field is 40kV/cm, the pulse frequency is 600Hz, and the duty cycle is 0.1, 0.3, 0.5, and 0.7. ,0.8,0.9;
  • Comparative Example 1 Traditional water enzymatic method
  • Screening Clean and remove a small amount of weed seeds, grain seeds, seed shells, etc.
  • Crushing Use a grinder to crush the dried rapeseed.
  • First enzyme treatment heat to 50°C and adjust pH to 6.0, cellulase, stir at 50°C for 1 hour.
  • Second enzyme treatment increase the temperature to 60°C, adjust the pH to 9.0, add immobilized alkaline endoprotease, and mix and stir for 4 hours. Raise the temperature to 90°C and hold for 10 minutes.
  • Centrifugation Centrifuge the resulting suspension at 4500r/min for 10 minutes at room temperature, and take the upper layer of fat to obtain rapeseed oil.
  • Comparative Example 2 Using immobilized enzyme (without high-voltage AC pulsed electric field treatment)
  • Screening Clean and remove a small amount of weed seeds, grain seeds, seed shells, etc.
  • Crushing Use a grinder to crush the dried rapeseed.
  • First enzyme treatment heat to 40°C, adjust pH to 8.0, add immobilized cellulase, and stir at 40°C for 1 hour. Separation of magnetically immobilized cellulase.
  • Second enzyme treatment lower the temperature to 60°C, adjust the pH to 9.0, add immobilized alkaline endoprotease, and mix and stir for 4 hours. After the enzymatic hydrolysis is completed, the magnetically immobilized alkaline endoprotease is separated again. Raise the temperature to 90°C and hold for 10 minutes.
  • Centrifugation Centrifuge the resulting suspension at 4500r/min for 10 minutes at room temperature, and take the upper layer of fat to obtain rapeseed oil.
  • Table 1 shows the extraction rate, color, acid value, peroxide value, moisture evaporator volatile components, and oxidation completion time of the rapeseed oil prepared in Example 6 and Comparative Examples 1-2.
  • Table 2 shows the trace components of rapeseed oil prepared in Example 6 and Comparative Examples 1-2.
  • the oil yield of rapeseed oil prepared by high-pressure pulse-assisted low-temperature catalytic extraction used in the present invention reaches 84.21%. Compared with the traditional aqueous enzymatic method, the extraction rate is higher.
  • the tocopherol content is 900.40mg/kg
  • the plant polyphenol content is 162.21mg/kg
  • the phytosterol content is 6752.36mg/kg
  • the ⁇ -carotene content is 6.89mg/kg, which is higher than that of rapeseed oil without high-voltage AC pulse electric field treatment.
  • Medium to high, and the oxidation induction time of rapeseed oil prepared by the method is relatively long, reaching 7 to 8 hours.
  • the present invention uses pulsed electric fields to change the permeability of plant seed cell membranes, increase the oil yield, and at the same time achieve the goals of enzyme inactivation and demulsification through physical means. Compared with the general water enzymatic method, the conditions are milder. , can maximize the retention of biologically active substances such as tocopherols, polyphenols, antioxidants and phytosterols in rapeseed. At the same time, immobilized enzymes are used for enzymatic hydrolysis, which can be recycled through simple methods.

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Abstract

本发明提高了一种高压交流脉冲电场辅助制备菜籽油的装置和方法，利用高压交流脉冲型电场改变植物种子细胞膜的通透性，加大出油率，同时，利用高压交流脉冲型电场达到灭酶、破乳的效果，具有工艺简单，处理温度低等特点，能最大限度保留菜籽中的生育酚、多酚、抗氧化剂和植物甾醇等生物活性物质，降低高温处理带来的危害，保证菜籽油的风味，提高菜籽油的品质。使用固定化酶进行酶解，用含载体的四氧化三铁纳米颗粒进行固定化，该方法制备的固定化酶通过简单的方法即可回收利用，可使酶重复使用，同时增加酶稳定性。

Description

一种高压交流脉冲电场辅助制备菜籽油的装置和方法 技术领域
本发明涉及油脂加工技术领域，具体涉及一种高压交流脉冲电场辅助制备菜籽油的装置和方法。
背景技术
菜籽油气味香醇，营养丰富。人体对菜籽油的吸收率很高，可达99％。具有补虚、润肠、清肝利胆、促进大脑发育、帮助眼睛抵抗各种强光的刺激，预防老年性眼病，小儿弱视等功效。高油酸菜籽油中富含油酸及亚油酸等不饱和脂肪酸以及维生素E，能够软化血管，延缓衰老。甾醇含量也较豆油等常见植物油高，且种类繁多，有些甾醇还具有特殊的生理功能。菜籽油的磷脂有利于血管、神经、大脑的发育，菜籽油的胆固醇很少或几乎不含。低芥酸菜籽油的饱和脂肪酸含量很低，油酸含量达60％以上，且有合理含量的亚油酸和亚麻酸，因而低芥酸菜籽油被称为“最健康的食用植物油”。菜籽油与其他食用植物油的植物甾醇含量相比，菜籽油中的胆固醇含量较低，而对身体健康有益的菜籽甾醇、菜油甾醇和豆甾醇含量为食用植物油中最高。菜籽多酚是油菜籽独有的一类重要次级代谢产物，具有抗肿瘤、降血糖、抑菌、清除自由基等生物活性，是一种潜在的重要天然抗氧化剂。
目前我国油菜籽制油工艺绝大多数采用带壳高温预榨-浸出制油工艺。产品为毛油和菜籽饼粕。由于高温预榨，毛油多为深褐色，需要精制，因此，菜籽油的风味和营养成分也会受到不同程度的损失。而浸出阶段，目前多采用6#溶剂油(正己烷含量约为30％)，而随着己烷被列入有害空气污染物组，使用己烷提取菜籽油最近也成为其安全性和环境影响的焦点。在实验室和中试工业规模水平上，已经尝试了水酶法用于从许多含油种子/果实中提取油。与传统技术相比，由于完全避免了有机溶剂，该过程温和而安全。尽管有这些优点，水酶法的缺点也十分明显。首先，现阶段酶制剂价格仍然较高，提高了生产成本，导致多年来水酶法大多停留在实验室研究和中试阶段，其工业应用一直受到限制。其次，植物油脂提取过程中，由于细胞壁坚硬、厚实、成分复杂，往往需要多种酶的协同作用，这导致部分油料破壁效果欠佳，提油率低。此外水酶法提取油脂过程中，形成的乳化层和残渣层中残油率高，导致提油率较低。
发明内容
本发明的目的在于克服现有技术存在的不足，提供一种高压交流脉冲型电场辅助催化制备浓香菜籽油的装置和方法，具备处理温度低，能最大限度保留菜籽的风味，以及生育酚、多酚、抗氧化剂和植物甾醇等生物活性物质的优势。
利用交流脉冲电场改变植物种子细胞膜的通透性，加大出油率。同时在水酶法提取后期，交流脉冲电场可有效增加油液中液滴的振动和碰撞，提高液滴聚结效率，具有较好的破乳效果。而在水酶法提取时，使用固定化酶代替传统游离形式的酶。与游离形式酶相比，不仅具有良好的温度、pH适应性，还可通过简单的方法回收再利用而酶活力损耗少。并且与产物的分离纯化较容易。
本发明第一个目的在于提供了一种利用高压交流脉冲型电场辅助萃取制备浓香菜籽油的装置，包括主体(1)；所述主体(1)设置有伺服电机(2)、进料口(3)、钢板(4)、混合杆(5)、旋转挡板(6)、筛选孔(7)、倾斜板(8)、pH检测仪(9)、温度检测仪(10)、加热块(11)、磁性酶回收槽(12)、过滤槽(13)、储液槽(14)、控制器(15)、酸添加管道(16)、进水管(19)和出料口(20)。
在本发明一种实施方式中，所述主体(1)从上到下包括第一层、第二层、第三层、第四层，层与层之间设置有旋转挡板，主体(1)第一、二、四层内部对称装有钢板(4)；所述主体(1)内部安装有伺服电机(2)，且伺服电机(2)的下端连接有混合杆(5)，所述第二层和第三层内部装有加热块(11)，第二层和第三层内壁装有pH检测仪(9)和温度检测仪(10)，主体(1)每层之间的旋转挡板左右两侧均设置筛选孔(7)，主体(1)第一层筛选孔下端设置有倾斜板(8)，主体(1)第二、三层筛选孔下端设置表面磁性的酶回收槽(12)，以滑块的形式便于取出，主体(1)设置有过滤槽(13)，同样以滑块的形式安装于底部，过滤槽(13)底部具有过滤网。
在本发明一种实施方式中，所述主体(1)还包括碱添加管道(17)、酶添加管道(18)。
在本发明一种实施方式中，所述主体(1)与伺服电机(2)之间的连接方式为固定连接，且混合杆(5)沿着伺服电机的竖直中心线均匀分布。
在本发明一种实施方式中，所述主体(1)内部涂覆有内部绝缘材料。
在本发明一种实施方式中，所述钢板(4)对称分布于主体内部绝缘材料上，且主体的前表面设置有控制器(15)，控制器(15)与钢板(4)之间的连接方式为电性连接。
在本发明一种实施方式中，所述筛选孔(7)沿着旋转挡板(6)两侧均匀分布，旋转挡板(6)与控制器(15)电性连接，所述控制器(15)控制旋转挡板(6)旋转。
在本发明一种实施方式中，所述加热块(11)环形对称分布于主体(1)内部，控制器(15)与加热块(11)之间的连接方式为电性连接。
在本发明一种实施方式中，所述磁性酶回收槽(12)分布于筛选孔(7)下端，磁性酶回收槽(12)设置有磁铁，且磁性酶回收槽(12)和主体(1)之间构成滑动结构。
在本发明一种实施方式中，所述过滤槽(13)分布于主体(1)底部，底层装有过滤网， 过滤槽(13)与主体(1)之间构成滑动结构。
在本发明一种实施方式中，所述出料口(20)位于储液槽(14)侧面与泵相连，将储液槽(14)中的液体排出主体(1)。
本申请文件第二个目的是使用上述装置提供一种高压交流脉冲电场辅助制备浓香菜籽油的方法，包括以下步骤：
①将菜籽原料筛选，清理，晒干，粉碎；
②对粉碎后的菜籽进行脉冲电场预处理；
③加入水混合，并对混合物进行第二次脉冲电场处理；
④加入固定化纤维素酶，酶水解结束后分离去除固定化酶；
⑤加入固定化碱性内切蛋白酶，酶水解结束后分离去除固定化酶；
⑥对所得混合物进行第三次脉冲电场处理；
⑦离心分离取上层，即得菜籽油。
在本发明一种实施方式中，使用上述装置制备菜籽油时，使用者首先将酶回收槽(12)和过滤槽(13)插入主体(1)内部，随后将粉碎的菜籽顺着进料口(3)倒入主体(1)内，与此同时，使用者将伺服电机(2)开启，通过伺服电机(2)与混合杆(5)相互配合，能够使得物料匀混合，随后通过控制器(15)命令使得主体(1)第一层的钢板(4)之间形成高压交流脉冲型电场，破坏植物细胞壁释放更多的油脂；
随后设置的旋转挡板(6)打开暴露筛选孔(7)，物料顺着倾斜板(8)滑入主体(1)第二层，通过控制器(15)命令进水管道(19)打开，同时使主体(1)第二层钢板(4)之间形成高压交流脉冲型电场，通过设置的pH检测仪(9)和温度检测仪(10)对料液的温度和pH进行监测，控制器打开设置的酸添加管道(16)和碱添加管道(17)调节pH，同时命令加热块(12)开启调节温度，然后通过设置的酶添加管道(18)释放固定化纤维素酶，进行处理；
处理完成后，设置的旋转挡板(6)打开暴露筛选孔(7)，物料顺着酶回收槽(12)倾斜表面滑入主体(1)第三层，其中固定化纤维素酶由于回收槽(12)表面具有磁性而附着在回收槽上，通过设置的pH检测仪(9)和温度检测仪(10)对料液的温度和pH进行监测，控制器打开设置的酸添加管道(16)和碱添加管道(17)调节pH，同时命令加热块(12)开启调节温度，然后通过设置的酶添加管道释放固定化碱性内切蛋白酶，进行处理；
处理完成后，设置的旋转挡板(6)打开暴露筛选孔(7)，物料顺着回收槽(12)倾斜表面滑入主体(1)第四层，其中固定化碱性内切蛋白酶由于回收槽(12)表面具有磁性而附着在回收槽上，通过控制器(15)命令使得主体(1)第四层的钢板(4)之间形成高压交流 脉冲型电场起到破乳的效果；
破乳处理完成后，设置的旋转挡板(6)打开暴露过滤槽(13)，在主体(1)外泵的作用下，料液经过储液槽(14)顺着出料口(20)流出，固形物附着在过滤槽(13)中，使用结束后，关闭装置，拉开酶回收槽(12)和过滤槽(13)，便能够方便对固形物残渣和酶进行处理，就这样完成整个使用上述装置制备菜籽油的过程。
在本发明一种实施方式中，所述步骤②中，使用高压交流脉冲型电场通过电刺激增大油菜籽细胞质膜通透性，破坏植物细胞结构，增加胞内物质溶出的途径。
在本发明一种实施方式中，所述步骤②中，电场强度为25～35kV/cm，物料停留时间180～200s，脉冲频率750～850Hz，占空比0.5～0.6。
在本发明一种实施方式中，所述步骤③中，使用脉冲电场代替传统高温灭酶过程，避免部分风味和营养物质的损失。
在本发明一种实施方式中，所述步骤③中，油料与水的比例为1:3～5(w/v，g/mL)。
在本发明一种实施方式中，所述步骤③中，电场强度为65～75kV/cm，脉冲频率750～850Hz，占空比0.5～0.6。
在本发明一种实施方式中，所述步骤④中，所用固定化纤维素酶，是以含载体的四氧化三铁纳米颗粒进行固定化的。
在本发明一种实施方式中，所述步骤④中，酶水解的温度为40～45℃，pH为7.5～8.0，搅拌1～2h。
在本发明一种实施方式中，所述步骤⑤中，所用固定化碱性内切蛋白酶，是以含载体的四氧化三铁纳米颗粒进行固定化的。
在本发明一种实施方式中，所述步骤⑤中，酶水解的温度为60～65℃，pH为8.5～9.0，搅拌4～4.5h。
在本发明一种实施方式中，所述步骤⑥中，使用脉冲电场进行破乳处理，其中电场强度为35～40kV/cm，脉冲频率550～600Hz，占空比0.6～0.7
在本发明一种实施方式中，所述步骤⑥中，优选的电场强度为40kV/cm，脉冲频率600Hz，占空比0.7。
在本发明一种实施方式中，所述步骤⑦中，离心转速为4500～6000r/min，室温下离心10～20min。
有益效果：
本发明采用水酶法提取菜籽油，采用生物酶对油料组织的细胞结构以及脂多糖和脂蛋白的超微结构进行降解，从而增加油料组织中油的流动性，使其从油料中游离出来，进一步促 使酚类等物质进入油脂，并且由于提取过程中水相及乳化层的保护，使一些蛋白质及酚类物质免受氧化，从而进一步提高油脂的氧化稳定性、货架期、营养、风味、感官等性能。
本发明所述方法中三次应用高压交流脉冲型电场处理技术，第一次对油料种子进行高压交流脉冲型电场处理，替换传统蒸炒工艺，条件温和，通过放电产生高压电流，破坏植物细胞，改变其通透性，使细胞内的物质能够有效流出，促进挥发性成分释放，提升油料气滋味，以提高后续压榨工艺油脂提取率和油脂风味。第二次对油料和水的混合体系进行高压交流脉冲型电场处理，使其在水中分散更加均匀，同时利用瞬间脉冲电场作用微生物细胞，致使细胞膜形成细孔，渗透性增强，细胞膨胀，最终破裂而是微生物失活，同时钝化体系中含有的酶。相比于传统高温灭酶，高压交流脉冲型电场是一种冷处理，能保存油菜籽固有成分的同时，杀菌灭酶，节约能耗。第三次脉冲电场处理除了具有杀菌灭酶，还可有效地增加油液中液滴的振动和碰撞，提高液滴聚结效率，起到破乳的作用，同时还可根据油液工况调节电场强度、脉冲频率、占比空等参数以获得最优的破乳效果。
本发明采用的酶为自制的固定化酶，用含载体的四氧化三铁纳米颗粒对纤维素酶和碱性内切蛋白酶进行固定化，由于其具有磁性，回收方便，可实现酶的重复利用，降低生产成本，提高生产效率。
本发明的装置通过设置的伺服电机与混合杆相互配合，能够使得油菜籽均匀混合，并且设置的旋转挡板和过滤孔相互配合控制处理时长和流速。
通过设置滑动结构的酶回收槽和过滤槽，提高酶的回收效率，利用过滤槽除去固形物，降低离心操作的难度避免杂质影响后续油的纯度，而且设置的滑动结构能够方便对其进行清洗和更换。
附图说明
图1本发明方法的工艺流程图
图2不同强度的电场处理下的破乳率
图3不同脉冲频率的电场处理下的破乳率
图4不同占空比的电场处理下的破乳率
图5为本发明装置的结构示意图
图6为本发明装置的外观图
图7为本发明装置的剖面示意图
图中：(1)主体；(2)伺服电机；(3)进料口；(4)钢板；(5)混合杆；(6)旋转挡板；(7)筛选孔；(8)倾斜板；(9)pH检测仪；(10)温度检测仪；(11)加热块； (12)磁性酶回收槽；(13)过滤槽；(14)储液槽；(15)控制器；(16)酸添加管道；(17)碱添加管道；(18)酶添加管道；(19)进水管；(20)出料口。
具体实施方式
菜籽油的色泽测定参考GB/T 22460-2008《动植物油脂罗维朋色泽的测定》；酸值测定参考GB/T 5530-2005《动植物油脂酸值和酸度测定》；过氧化值的测定参考GB/T 5538-2005《油脂过氧化值测定》；水分及挥发物含量参考GB/T 5528-2008。氧化稳定性的测定参考NY/T 2001-2011《菜籽油氧化稳定性的测定加速氧化试验》；多酚含量的测定参考LS/T 6119-2017《粮油检测植物油中多酚的测定分光光度法》；破乳率测定方法如下：用50mL烧杯称取5g菜籽乳状液，经一定电场强度，电场频率和占空比的高压交流脉冲型电场处理后取出。4500r/min室温下离心10min，得游离油、水相混合液和残余物，破乳率按下式(1)计算。出油率按下式(2)计算：
Figure PCTCN2022135462-appb-000001
Figure PCTCN2022135462-appb-000002
以下对本发明的原理和特征进行描述，所举实例只用于解释本发明，并非限定本发明的范围。
实施例1：一种高压交流脉冲型电场辅助催化萃取制备浓香菜籽油的装置
一种高压交流脉冲型电场辅助催化萃取制备浓香菜籽油的装置，所述主体(1)设置有伺服电机(2)、进料口(3)、钢板(4)、混合杆(5)、旋转挡板(6)、筛选孔(7)、倾斜板(8)、pH检测仪(9)、温度检测仪(10)、加热块(11)、磁性酶回收槽(12)、过滤槽(13)、储液槽(14)、控制器(15)、酸添加管道(16)、进水管(19)和出料口(20)。
主体(1)从上到下包括第一层、第二层、第三层、第四层，层与层之间设置有旋转挡板，主体(1)第一、二、四层内部对称装有钢板(4)；所述主体(1)内部安装有伺服电机(2)，且伺服电机(2)的下端连接有混合杆(5)，所述第二层和第三层内部装有加热块(11)，第二层和第三层内壁装有pH检测仪(9)和温度检测仪(10)，主体(1)每层之间的旋转挡板左右两侧均设置筛选孔(7)，主体(1)第一层筛选孔下端设置有倾斜板(8)，主体(1)第二、三层筛选孔下端设置表面磁性的酶回收槽(12)，以滑块的形式便于取出，主体(1)设置有过滤槽(13)，同样以滑块的形式安装于底部，过滤槽(13)底部具有过滤网。
主体(1)还包括碱添加管道(17)、酶添加管道(18)。
主体(1)与伺服电机(2)之间的连接方式为固定连接，且混合杆(5)沿着伺服电机的竖直中心线均匀分布。
主体(1)内部涂覆有内部绝缘材料。
钢板(4)对称分布于主体内部绝缘材料上，且主体的前表面设置有控制器(15)，控制器(15)与钢板(4)之间的连接方式为电性连接。
筛选孔(7)沿着旋转挡板(6)两侧均匀分布，旋转挡板(6)与控制器(15)电性连接，所述控制器(15)控制旋转挡板(6)旋转。
加热块(11)环形对称分布于主体(1)内部，控制器(15)与加热块(11)之间的连接方式为电性连接。
磁性酶回收槽(12)分布于筛选孔(7)下端，磁性酶回收槽(12)设置有磁铁，且磁性酶回收槽(12)和主体(1)之间构成滑动结构。
过滤槽(13)分布于主体(1)底部，底层装有过滤网，过滤槽(13)与主体(1)之间构成滑动结构。
出料口(20)位于储液槽(14)侧面与泵相连，将储液槽(14)中的液体排出主体(1)。
工作原理：对于这类的菜籽油制油装置，使用前，使用者首先将酶回收槽(12)和过滤槽(13)插入主体(1)内部，随后将粉碎的菜籽顺着进料口(3)倒入主体(1)内，与此同时，使用者将伺服电机(2)开启，通过伺服电机(2)与混合杆(5)相互配合，能够使得物料匀混合，随后通过控制器(15)命令使得主体(1)第一层的钢板(4)之间形成高压交流脉冲型电场，破坏植物细胞壁释放更多的油脂。随后设置的旋转挡板(6)打开暴露筛选孔(7)，物料顺着倾斜板(8)滑入主体(1)第二层，通过控制器(15)命令进水管道(19)打开，同时使主体(1)第二层钢板(4)之间形成高压交流脉冲型电场，通过设置的pH检测仪(9)和温度检测仪(10)对料液的温度和pH进行监测，控制器打开设置的酸添加管道(16)和碱添加管道(17)调节pH，同时命令加热块(12)开启调节温度，然后通过设置的酶添加管道(18)释放酶A。处理一段时间后，设置的旋转挡板(6)打开暴露筛选孔(7)，物料顺着酶回收槽(12)倾斜表面滑入主体(1)第三层，其中酶A由于回收槽(12)表面具有磁性而附着在回收槽上，通过设置的pH检测仪(9)和温度检测仪(10)对料液的温度和pH进行监测，控制器打开设置的酸添加管道(16)和碱添加管道(17)调节pH，同时命令加热块(12)开启调节温度，然后通过设置的酶添加管道释放酶B。处理一段时间后，设置的旋转挡板(6)打开暴露筛选孔(7)，物料顺着回收槽(12)倾斜表面滑入主体(1)第四层，其中酶B由于回收槽(12)表面具有磁性而附着在回收槽上，通过控制器(15)命令使得主 体(1)第四层的钢板(4)之间形成高压交流脉冲型电场起到破乳的效果。处理一段时间后，设置的旋转挡板(6)打开暴露过滤槽(13)，在主体(1)外泵的作用下，料液经过储液槽(14)顺着出料口(20)流出，固形物附着在过滤槽(13)中，使用结束后，关闭装置，拉开酶回收槽(12)和过滤槽(13)，编能够方便对固形物残渣和酶进行处理，就这样完成整个制油装置的使用过程。
实施例2：固定化酶的制备
将海藻酸钠溶于蒸馏水中，得到2.0％(w/v，g/mL)的海藻酸钠溶液，加入1.6％(w/v，g/mL)的Fe 3O 4纳米颗粒搅拌30min。将混合物加热至80℃，在氮气气氛下搅拌1h。将铁磁流体进一步超声分散20min，离心去除少量大团聚体(1000×g，10min)进行纯化。将碱性内切蛋白酶(30000U)或纤维素酶(30000U)溶液共10mL加入到100mL的磁流体中，混合均匀后，用注射器将铁磁流体注入到10wt％CaCl 2水溶液中，制备磁性微球。磁性微球浸泡1h后，用蒸馏水洗涤，去除粘附在表面的游离Ca 2+，然后用0.5％戊二醛交联1.5h，再用蒸馏水洗涤。最后，将微球在4℃下孵育一夜，使其变硬。在35℃下干燥12h，得到固定化酶。
实施例3
①筛选，清理除去菜籽原料中的杂草种子，谷物种子，籽壳等杂质；清洗，将筛选后的菜籽用清水清洗，洗掉菜籽表面的尘土，沥干，在阳光下晒干水分；破碎，用研磨机对晒干后的油菜籽进行粉碎。
②第一次高压交流脉冲型电场处理：对粉碎后的菜籽进行高压交流脉冲型电场预处理，压脉冲电场强度为为25kV/cm，物料停留时间180s，脉冲频率850Hz，占空比0.5。
③第二次高压交流脉冲型电场处理：将5克处理过的油菜籽与蒸馏水1:3(w/v，g/mL)的质量比混合。对混合物进行高压交流脉冲型电场处理，压脉冲电场强度为75kV/cm，脉冲频率850Hz，占空比0.5。
④第一次酶处理：加热至40℃，并调节pH至8.0，加入固定化纤维素酶，在40℃下搅拌1小时。将具有磁性的固定化纤维素酶分离。
⑤第二次酶处理：降低温度至60℃，并调节pH为9.0，加入固定化碱性内切蛋白酶，混合搅拌4小时。酶水解结束后，分离具有磁性的固定化碱性内切蛋白酶。
⑥第三次高压脉冲处理：对分离固定化酶后的混合物进行高压交流脉冲型电场处理，压脉冲电场强度40kV/cm，脉冲频率600Hz，占空比0.7。
⑦离心。将所得悬浮液室温下以4500r/min的转速离心10min，取上层油脂，即得菜籽油。
实施例4：高压交流脉冲型电场破乳条件(电场强度)优化
(1)-(5)同实施例3步骤(1)-(5)；
(6)第三次高压脉冲处理：对分离固定化酶后的混合物进行高压交流脉冲型电场处理，高压脉冲电场强度15、20、25、30、35、40、45、50、55、60kV/cm，脉冲频率600Hz，占空比0.7；
(7)将所得悬浮液室温下以4500r/min的转速离心10min，得游离油、水相混合液和残余物，计算破乳率。
实施例5：高压交流脉冲型电场破乳条件(电场频率)优化
(1)-(5)同实施例3步骤(1)-(5)；
(6)第三次高压脉冲处理：对分离固定化酶后的混合物进行高压交流脉冲型电场处理，高压交流脉冲型电场强度40kV/cm，脉冲频率300、350、400、450、500、550、600、650、700、750Hz，占空比0.7；
(7)将所得悬浮液室温下以4500r/min的转速离心10min，得游离油、水相混合液和残余物，计算破乳率。
实施例6：高压交流脉冲型电场破乳破乳(占空比)优化
(1)-(5)同实施例3步骤(1)-(5)；
(6)第三次高压脉冲处理：对分离固定化酶后的混合物进行高压交流脉冲型电场处理，高压交流脉冲型电场强度40kV/cm，脉冲频率600Hz，占空比0.1、0.3、0.5、0.7、0.8、0.9；
(7)将所得悬浮液室温下以4500r/min的转速离心10min，得游离油、水相混合液和残余物，计算破乳率。
对比例1：传统水酶法
筛选：清理除去少量杂草种子，谷物种子，籽壳等。
清洗：将筛选后的菜籽用清水清洗，洗掉菜籽表面的尘土，沥干，在阳光下晒干水分。
破碎：用研磨机对晾晒后的油菜籽进行粉碎。
加水混合：将5克处理过的油菜籽与蒸馏水1:3(w/v，g/mL)的质量比混合，煮沸4min。
第一次酶处理：加热至50℃，并调节pH至6.0，纤维素酶，在50℃下搅拌1小时。
第二次酶处理：升高温度至60℃，并调节pH为9.0，加入固定化碱性内切蛋白酶，混合 搅拌4小时。升温至90℃保持10min。
离心：将所得悬浮液室温下以4500r/min的转速离心10min，取上层油脂，即得菜籽油。
对比例2：使用固定化酶(未经高压交流脉冲型电场处理)
筛选：清理除去少量杂草种子，谷物种子，籽壳等。
清洗：将筛选后的菜籽用清水清洗，洗掉菜籽表面的尘土，沥干，在阳光下晒干水分。
破碎：用研磨机对晾晒后的油菜籽进行粉碎。
加水混合：将5克处理过的油菜籽与蒸馏水1:3(w/v，g/mL)的质量比混合，煮沸4min。
第一次酶处理：加热至40℃，并调节pH至8.0，加入固定化纤维素酶，在40℃下搅拌1小时。将具有磁性的固定化纤维素酶分离。
第二次酶处理：降低温度至60℃，并调节pH为9.0，加入固定化碱性内切蛋白酶，混合搅拌4小时。酶水解结束后再次分离具有磁性的固定化碱性内切蛋白酶。升温至90℃保持10min。
离心：将所得悬浮液室温下以4500r/min的转速离心10min，取上层油脂，即得菜籽油。
表1为实施例6和对比例1-2制取的菜籽油的提取率、色泽、酸价、过氧化值、水分机挥发成分、氧化完成时间。
表2为实施例6和对比例1-2制取的菜籽油的微量成分。
表1实施例6和对比例1-2制取的菜籽油的提取率、色泽、酸价、过氧化值、水分机挥发成分、氧化完成时间
Figure PCTCN2022135462-appb-000003
表2实施例6和对比例1-2制取的菜籽油的微量成分
Figure PCTCN2022135462-appb-000004
Figure PCTCN2022135462-appb-000005
由上表可知，本发明采用的高压脉冲辅助低温催化萃取制备的菜籽油，其出油率达到84.21％，相比于未传统水酶法，提取率更高。生育酚含量900.40mg/kg，植物多酚含量162.21mg/kg，植物甾醇的含量6752.36mg/kg、β-胡萝卜素的含量6.89mg/kg，比未经高压交流脉冲型电场处理的菜籽油中高，且所述方法制备的菜籽油的氧化诱导时间都相对较长达到7～8小时，这一结果与油脂中的植物多酚、β-胡萝卜素等微量成分含量是一致的，这些微量成分使上述方法制备的菜籽油具有较强的氧化稳定性，这意味着其产品货架期也更长。可能的原因是：本发明利用脉冲电场改变植物种子细胞膜的通透性，加大出油率，同时通过物理方式达到灭酶、破乳等目的，与一般的水酶法相比，条件更加温和，能最大限度保留菜籽中的生育酚、多酚、抗氧化剂和植物甾醇等生物活性物质。同时使用固定化酶进行酶解，通过简单的方法即可回收利用。
以上显示和描述了本发明的基本原理、主要特征和优点。本发明不受上述实施例的限制，上述实施例和说明书中的描述只是说明本发明的原理，在不脱离本发明精神和范围的前提下，本发明还会有各种变化和改进，这些变化和改进都落入要求保护的本发明范围。本发明要求保护范围由所附的权利要求书及其等效物界定。

Claims (10)

  1. 一种利用高压交流脉冲型电场辅助制备浓香菜籽油的装置，其特征在于，包括主体(1)；所述主体(1)设置有伺服电机(2)、进料口(3)、钢板(4)、混合杆(5)、旋转挡板(6)、筛选孔(7)、倾斜板(8)、pH检测仪(9)、温度检测仪(10)、加热块(11)、磁性酶回收槽(12)、过滤槽(13)、储液槽(14)、控制器(15)、酸添加管道(16)、进水管(19)和出料口(20)；
    所述主体(1)从上到下包括第一层、第二层、第三层、第四层，层与层之间设置有旋转挡板，主体(1)第一、二、四层内部对称装有钢板(4)；所述主体(1)内部安装有伺服电机(2)，且伺服电机(2)的下端连接有混合杆(5)，所述第二层和第三层内部装有加热块(11)，第二层和第三层内壁装有pH检测仪(9)和温度检测仪(10)，主体(1)每层之间的旋转挡板左右两侧均设置筛选孔(7)，主体(1)第一层筛选孔下端设置有倾斜板(8)，主体(1)第二、三层筛选孔下端设置表面磁性的酶回收槽(12)，以滑块的形式便于取出，主体(1)设置有过滤槽(13)，同样以滑块的形式安装于底部，过滤槽(13)底部具有过滤网；
    所述主体(1)还包括碱添加管道(17)、酶添加管道(18)。
  2. 根据权利要求1所述装置，其特征在于，所述主体(1)与伺服电机(2)之间的连接方式为固定连接，且混合杆(5)沿着伺服电机的竖直中心线均匀分布。
  3. 根据权利要求1所述装置，其特征在于，所述主体(1)内部涂覆有内部绝缘材料。
  4. 根据权利要求1所述装置，其特征在于，所述钢板(4)对称分布于主体内部绝缘材料上，且主体的前表面设置有控制器(15)，控制器(15)与钢板(4)之间的连接方式为电性连接。
  5. 根据权利要求1所述装置，其特征在于，所述筛选孔(7)沿着旋转挡板(6)两侧均匀分布，旋转挡板(6)与控制器(15)电性连接，所述控制器(15)控制旋转挡板(6)旋转。
  6. 根据权利要求1所述装置，其特征在于，所述加热块(11)环形对称分布于主体(1)内部，控制器(15)与加热块(11)之间的连接方式为电性连接。
  7. 根据权利要求1所述装置，其特征在于，所述磁性酶回收槽(12)分布于筛选孔(7)下端，磁性酶回收槽(12)设置有磁铁，且磁性酶回收槽(12)和主体(1)之间构成滑动结构。
  8. 根据权利要求1所述装置，其特征在于，所述过滤槽(13)分布于主体(1)底部，底层装有过滤网，过滤槽(13)与主体(1)之间构成滑动结构。
  9. 根据权利要求1所述装置，其特征在于，所述出料口(20)位于储液槽(14)侧面与 泵相连，将储液槽(14)中的液体排出主体(1)。
  10. 一种高压交流脉冲电场辅助低温制备菜籽油的方法，其特征在于，包括以下步骤：
    ①将菜籽原料筛选，清理，晒干，粉碎；
    ②对粉碎后的菜籽进行脉冲电场预处理；
    ③加入水混合，并对混合物进行第二次脉冲电场处理；
    ④加入固定化纤维素酶，酶水解结束后分离去除固定化纤维素酶；
    ⑤加入固定化碱性内切蛋白酶，酶水解结束后分离去除固定化碱性内切蛋白酶；
    ⑥对所得混合物进行第三次脉冲电场处理；
    ⑦离心分离取上层，即得菜籽油；
    所述步骤②～⑦是在权利要求1～9所述装置中进行；
    所述步骤⑥中，使用脉冲电场进行破乳处理，其中电场强度为35～40kV/cm，脉冲频率550～600Hz，占空比0.6～0.7。
PCT/CN2022/135462 2022-06-30 2022-11-30 一种高压交流脉冲电场辅助制备菜籽油的装置和方法 Ceased WO2024001031A1 (zh)

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