CN111548853A - Preparation method of edible oil capable of effectively reducing aflatoxin content - Google Patents

Preparation method of edible oil capable of effectively reducing aflatoxin content Download PDF

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CN111548853A
CN111548853A CN202010436248.8A CN202010436248A CN111548853A CN 111548853 A CN111548853 A CN 111548853A CN 202010436248 A CN202010436248 A CN 202010436248A CN 111548853 A CN111548853 A CN 111548853A
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oil
preparation
aflatoxin
treating agent
nitrate hexahydrate
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崔艳兰
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    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B1/00Production of fats or fatty oils from raw materials
    • C11B1/06Production of fats or fatty oils from raw materials by pressing
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B1/00Production of fats or fatty oils from raw materials
    • C11B1/02Pretreatment
    • C11B1/04Pretreatment of vegetable raw material
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B3/00Refining fats or fatty oils
    • C11B3/02Refining fats or fatty oils by chemical reaction
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B3/00Refining fats or fatty oils
    • C11B3/10Refining fats or fatty oils by adsorption

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Microbiology (AREA)
  • General Chemical & Material Sciences (AREA)
  • Edible Oils And Fats (AREA)

Abstract

The invention provides a preparation method of edible oil capable of effectively reducing aflatoxin content, which comprises the steps of taking nickel nitrate hexahydrate, yttrium nitrate hexahydrate, gadolinium nitrate hexahydrate, polyacrylonitrile and the like as raw materials to prepare a magnetic treating agent, taking chitosan, bacillus subtilis CMCC63501, perillaldehyde, linalool and the like as raw materials to prepare an additive, firstly squeezing an oil-containing plant raw material to obtain crude oil, then adding the treating agent into the crude oil, realizing adsorption and catalytic degradation of aflatoxin under the condition of natural illumination, adding the additive, continuing catalytic degradation of residual aflatoxin, and finally enriching and removing the treating agent by using magnets. The invention effectively reduces the content of aflatoxin in the production process of edible oil, can inhibit the generation of aflatoxin in the preservation process of the edible oil depending on the action of the additive, comprehensively controls the content of aflatoxin in the edible oil, and has good popularization value.

Description

Preparation method of edible oil capable of effectively reducing aflatoxin content
Technical Field
The invention relates to the technical field of edible oil preparation, in particular to an edible oil preparation method capable of effectively reducing aflatoxin content.
Background
Common edible oils in daily life include rapeseed oil, peanut oil, hemp oil, corn oil, olive oil, camellia oil, palm oil, sunflower oil, soybean oil, sesame oil, linseed oil (linseed oil), grape seed oil, walnut oil, peony seed oil, etc.
Aflatoxin has been classified as a class 1 carcinogen by the cancer research institution of the world health organization, and is a highly toxic substance. The aflatoxin has a destructive effect on human and animal liver tissues, and can cause liver cancer and even death in severe cases. Aflatoxins (aflatoxins) are a group of compounds with similar chemical structures, and 12 have been isolated and identified, including b1, b2, g1, g2, m1, m2, p1, q, h1, gm, b2a, and toxol. The basic structure of aflatoxin is difuran ring and coumarin, b1 is dihydrofuran phthalazone derivative, namely contains one difuran ring and one phthalazone (coumarin), the former is basic toxic structure, and the latter is related to carcinogenesis. m1 is a metabolite derived from aflatoxin b1 by hydroxylation in vivo. Aflatoxin b1 is most commonly found in naturally contaminated foods. It is also most toxic and carcinogenic.
Aflatoxins are found in soil, animals and plants, various nuts, especially peanuts and walnuts. Aflatoxins are also commonly found in corn, macaroni, flavored milks, dairy products, edible oils, and the like. The allowable amount standard of aflatoxin in corn, peanut kernel, peanut oil and corn germ oil is 20 mug/kg, the allowable amount standard of aflatoxin in rice and edible oil is 10 mug/kg, the allowable amount standard of aflatoxin in other grains, beans and fermented foods is 5 mug/kg, and infant milk replacers cannot be detected in China. The highest allowable amount standard of aflatoxin in food and feed recommended by the world health organization is 15 mug/kg, 30-50 mug/kg is low toxicity, 50-100 mug/kg is poisoning, 100-1000 mug/kg is high toxicity, and more than 1000 mug/kg is extremely toxicity.
Aflatoxins may be produced both from the source of the food oil and during storage. The aflatoxin has stable chemical properties, can be destroyed only at a high temperature of over 280 ℃, is not sensitive to heat, and can not be completely removed even after being treated for 20 hours at 100 ℃. Therefore, the method is very important for fundamentally controlling the content of the aflatoxin.
Patent CN107008226B discloses a process for removing aflatoxin and benzopyrene in peanut oil, which comprises preparing adsorbent from diatomite, calcite, kaolinite, sepiolite, polystyrene microspheres and the like, and removing aflatoxin by adsorption method. However, the method is only suitable for removing the aflatoxin in the production process of the edible oil, and the production of aflatoxin in the preservation process of the edible oil cannot be controlled.
Disclosure of Invention
The invention aims to provide a preparation method of edible oil capable of effectively reducing the content of aflatoxin, and aims to solve the technical problems of reducing the content of aflatoxin in the production process of edible oil and inhibiting the generation of aflatoxin in the storage process.
In order to realize the purpose, the invention provides a preparation method of edible oil for effectively reducing the content of aflatoxin, which comprises the following steps:
(1) preparation of the treating agent: adding nickel nitrate hexahydrate, yttrium nitrate hexahydrate and gadolinium nitrate hexahydrate into N, N' -dimethylformamide, uniformly oscillating by ultrasonic waves, adding polyacrylonitrile, stirring to prepare spinning solution, performing electrostatic spinning, drying and calcining to obtain a treating agent for later use;
(2) preparation of the additive: dissolving chitosan in 0.2-0.3 mol/L acetic acid solution, adding lecithin, uniformly oscillating by ultrasonic waves, averagely dividing into two parts, adding perillaldehyde and linalool oil into one part, adding bacillus subtilis CMCC63501 into the other part, respectively emulsifying, combining, and freeze-drying in vacuum to obtain an additive for later use;
(3) and (2) squeezing the oil-containing plant raw materials to obtain crude oil, adding the treating agent obtained in the step (1) into the crude oil, naturally illuminating for 20-30 minutes, adding the additive obtained in the step (2), continuously illuminating for 3-5 minutes, and enriching and removing the treating agent by using a magnet.
Preferably, in the step (1), the mass-to-volume ratio of nickel nitrate hexahydrate, yttrium nitrate hexahydrate, gadolinium nitrate hexahydrate, N' -dimethylformamide and polyacrylonitrile is 1 g: 3-5 g: 1.2-1.5 g: 800-1000 mL: 50-80 g.
Preferably, in the step (1), the process conditions of ultrasonic oscillation are as follows: oscillating at 300-500W for 30-40 min.
Preferably, in the step (1), the preparation process conditions of the spinning solution are as follows: stirring for 15-18 hours at 70-80 ℃.
Preferably, in the step (1), the process conditions of electrostatic spinning are as follows: the feeding speed of the spinning solution is 1.3-1.5 mL/h, the spinning voltage is 15-18 kV, and the spinning distance is 16-18 cm.
Preferably, in the step (1), the drying process conditions are as follows: carrying out ventilation drying for 10-12 hours at the temperature of 30-45 ℃; the calcination process conditions are as follows: calcining at 450-480 ℃ for 80-100 minutes.
Preferably, in the step (2), the mass-to-volume ratio of the chitosan, the acetic acid solution, the lecithin, the bacillus subtilis CMCC63501, the perillaldehyde and the linalool oil is 0.1 g: 50-60 mL: 0.05-0.08 g: 0.08-0.1 g: 0.05-0.08 g: 0.1 to 0.2 g.
Preferably, in the step (2), the specific method of emulsification is as follows: and (3) firstly carrying out vortex oscillation for 15-20 s, and then repeatedly passing through the membrane for 2-3 times by using a membrane emulsifier, wherein the membrane passing speed is 35-40 mL/min.
Preferably, in the step (2), the vacuum freeze-drying process conditions are as follows: freezing at the temperature of minus 40 ℃ to minus 50 ℃ for 8-10 hours, vacuumizing to 2-3 Pa, heating to 20-30 ℃, and keeping the vacuum degree for treatment for 6-8 hours.
Preferably, in step (3), the oil-containing plant material is selected from any one or more of, but not limited to, rapeseed, peanut kernel, soybean, corn, olive fruit, walnut kernel, sunflower seed, sesame, grape seed, linseed, and peony seed.
Preferably, in the step (3), the specific method of pressing is as follows:
(A) firstly, drying the oil-containing plant raw material, and crushing to obtain powder with the particle size of 0.5 mm;
(B) pretreating the powder by adopting a steam explosion technology, and then micronizing the powder to below 200 nm;
(C) and (C) squeezing the powder treated in the step (B) by using a screw oil press to obtain crude oil.
Further preferably, in the step (B), the process conditions of the steam explosion technology are as follows: and (3) loading the powder into a blasting cavity of steam blasting equipment, keeping the powder for 1 minute under the condition of 1MPa, and then quickly releasing the pressure.
More preferably, in the step (B), the micronization is carried out by a jet mill under the following working conditions: the air pressure was 1200kPa, the feed rate was 200r/min, the classification frequency was 35Hz, and the crushing time was 60 minutes.
Further preferably, the specific method of step (C) is: and (3) idling the screw oil press for 3 minutes, feeding the material while the material is hot, and starting squeezing when the temperature of the machine body reaches 70 ℃ until no oil flows out.
Preferably, in the step (3), the mass ratio of the crude oil to the treating agent to the additive is 1: 0.01-0.02: 0.005-0.008.
Preferably, in the step (3), the treating agent can be repeatedly used after being treated at the high temperature of 300 ℃ to degrade aflatoxin.
The invention has the following beneficial effects:
the method comprises the steps of preparing a magnetic treating agent by using nickel nitrate hexahydrate, yttrium nitrate hexahydrate, gadolinium nitrate hexahydrate, polyacrylonitrile and the like as raw materials, preparing an additive by using chitosan, bacillus subtilis CMCC63501, perillaldehyde, linalool and the like as raw materials, squeezing an oil-containing plant raw material to obtain crude oil, adding the treating agent into the crude oil, realizing adsorption and catalytic degradation of aflatoxin under a natural illumination condition, adding the additive, continuing catalytic degradation of the rest aflatoxin, and finally enriching and removing the treating agent by using a magnet. The invention effectively reduces the content of aflatoxin in the production process of edible oil, can inhibit the generation of aflatoxin in the preservation process of the edible oil depending on the action of the additive, comprehensively controls the content of aflatoxin in the edible oil, and has good popularization value.
Carbon fibers prepared by using polyacrylonitrile through electrostatic spinning, drying and calcining have good adsorption effect because micropores (occupied positions before hydrogen and oxygen atoms escape in the calcining process) are distributed on the surfaces of the carbon fibers, and the large specific surface area increases the light absorption area and ensures the photocatalytic efficiency. On the basis, nickel, yttrium and gadolinium are introduced to realize the doping of the carbon fiber, wherein the nickel endows the treating agent with magnetism, so that the treating agent can be conveniently enriched and removed by using a magnet after being used, and the treating agent can be repeatedly used after being treated at the high temperature of 300 ℃ to degrade aflatoxin, thereby greatly reducing the treatment cost; the doping of nickel, yttrium and gadolinium enables the surface of the carbon fiber to form defects, the specific surface area is further increased, and the photocatalytic efficiency is improved. Electrons on yttrium are transferred to the surface of carbon fiber, carrier separation and transfer are promoted, the photocatalytic efficiency is improved, the energy level structure of gadolinium can play a role in electron conduction bridging, the forbidden band energy level of yttrium is filled, the wavelength red shift is excited, catalytic degradation can be realized under natural light, and the photocatalytic efficiency is further improved.
Under the emulsification effect of lecithin, amino groups, hydroxyl groups and the like of chitosan form a net through hydrogen bonds, so that the coating effect on the bacillus subtilis CMCC63501, the perillaldehyde and the linalool oil is realized, the problem that the bacillus subtilis CMCC63501 is difficult to store at normal temperature is solved, and the phenomenon that the perillaldehyde and the linalool oil volatilize at normal temperature and lose corresponding effects is avoided. The bacillus subtilis CMCC63501 inhibits the growth of aspergillus flavus and the like with metabolites through micro-ecological environment competitive inhibition, and eliminates the generation of aflatoxin from the root.
The perillaldehyde has strong electron receiving capacity, so that the respiration effect and the cell membrane function of the mould are influenced, the permeable barrier of the cell membrane is damaged, and the mould is dead; the main component of the linalool oil is linalool, and the hydroxyl group of the linalool has an electron-withdrawing induction effect, so that the electron receiving capacity of perillaldehyde is further enhanced, and the stronger the electron receiving capacity of aldehydes is, the stronger the inhibition effect on mold is, so that the perillaldehyde and the linalool synergistically improve the inhibition effect on mold such as aspergillus flavus and the like, and the generation of aflatoxin in the edible oil preservation process is effectively inhibited. However, perillaldehyde also has an inhibitory effect on bacillus subtilis CMCC63501, so in the preparation of the additive, a method of preparing and combining separately should be adopted.
After the treating agent is added into the crude oil, the catalytic degradation of low-polarity aflatoxin components is realized through natural illumination, and then the additive is added, so that on one hand, along with the dissipation of the additive in the crude oil, polar groups such as amino groups and hydroxyl groups brought by chitosan adsorb the high-polarity aflatoxin components in the crude oil, and then the high-polarity aflatoxin components are adsorbed and catalytically decomposed by the treating agent, and the thorough removal of various aflatoxin components in the crude oil is realized; on the other hand, chitosan has polar groups such as amino groups and hydroxyl groups, so that the chitosan is not good in dispersibility in the edible oil, and part of lipophilic groups of the lecithin in the additive are exposed in the dissipation and adsorption processes, so that the chitosan is well dispersed in the edible oil.
In addition to the objects, features and advantages described above, other objects, features and advantages of the present invention are also provided. The present invention will be described in further detail below.
Detailed Description
The following is a detailed description of embodiments of the invention, but the invention can be implemented in many different ways, as defined and covered by the claims.
The bacillus subtilis CMCC63501 provided by the invention is purchased from Kyork Kai microbial science and technology limited in Guangdong.
For comparison, peanut kernels were used as the oil-containing vegetable materials in examples and comparative examples, but the oil-containing vegetable materials of the present invention are not limited to peanut kernels.
Example 1:
a preparation method of edible oil for effectively reducing aflatoxin content comprises the following specific steps:
(1) preparation of the treating agent: adding nickel nitrate hexahydrate, yttrium nitrate hexahydrate and gadolinium nitrate hexahydrate into N, N' -dimethylformamide, uniformly oscillating by ultrasonic waves, adding polyacrylonitrile, stirring to prepare spinning solution, performing electrostatic spinning, drying and calcining to obtain a treating agent for later use;
(2) preparation of the additive: dissolving chitosan in 0.2mol/L acetic acid solution, adding lecithin, uniformly oscillating by ultrasonic waves, averagely dividing into two parts, adding perillaldehyde and linalool oil into one part, adding bacillus subtilis CMCC63501 into the other part, respectively emulsifying, combining, and freeze-drying in vacuum to obtain the additive for later use;
(3) and (2) squeezing the oil-containing plant raw materials to obtain crude oil, adding the treating agent obtained in the step (1) into the crude oil, naturally illuminating for 30 minutes, adding the additive obtained in the step (2), continuously illuminating for 3 minutes, and enriching and removing the treating agent by using a magnet.
In the step (1), the mass-to-volume ratio of nickel nitrate hexahydrate, yttrium nitrate hexahydrate, gadolinium nitrate hexahydrate, N' -dimethylformamide and polyacrylonitrile is 1 g: 5 g: 1.2 g: 1000mL of: 50 g.
In the step (1), the process conditions of ultrasonic oscillation are as follows: the mixture was shaken at 500W for 30 minutes.
In the step (1), the preparation process conditions of the spinning solution are as follows: stirred at 80 ℃ for 15 hours.
In the step (1), the electrostatic spinning process conditions are as follows: the feed rate of the spinning solution was 1.5 mL/hr, the spinning voltage was 15kV, and the spinning distance was 18 cm.
In the step (1), the drying process conditions are as follows: ventilating and drying for 12 hours at 30 ℃; the calcination process conditions are as follows: calcining at 450 ℃ for 100 minutes.
In the step (2), the mass volume ratio of the chitosan, the acetic acid solution, the lecithin, the bacillus subtilis CMCC63501, the perillaldehyde and the linalool oil is 0.1 g: 50mL of: 0.08 g: 0.08 g: 0.08 g: 0.1 g.
In the step (2), the specific method for emulsification is as follows: vortex for 20s, then pass through the membrane repeatedly for 2 times by the membrane emulsifier, the membrane passing speed is 40 mL/min.
In the step (2), the process conditions of vacuum freeze drying are as follows: freezing at-40 deg.C for 10 hr, vacuumizing to 2Pa, heating to 30 deg.C, and maintaining vacuum degree for 6 hr.
In the step (3), the oil-containing plant material is peanut kernels.
In the step (3), the specific method for squeezing is as follows:
(A) firstly, drying the oil-containing plant raw material, and crushing to obtain powder with the particle size of 0.5 mm;
(B) pretreating the powder by adopting a steam explosion technology, and then micronizing the powder to below 200 nm;
(C) and (C) squeezing the powder treated in the step (B) by using a screw oil press to obtain crude oil.
In the step (B), the process conditions of the steam explosion technology are as follows: and (3) loading the powder into a blasting cavity of steam blasting equipment, keeping the powder for 1 minute under the condition of 1MPa, and then quickly releasing the pressure.
In the step (B), carrying out superfine grinding by using a jet mill under the working conditions of: the air pressure was 1200kPa, the feed rate was 200r/min, the classification frequency was 35Hz, and the crushing time was 60 minutes.
The specific method of the step (C) is as follows: and (3) idling the screw oil press for 3 minutes, feeding the material while the material is hot, and starting squeezing when the temperature of the machine body reaches 70 ℃ until no oil flows out.
In the step (3), the mass ratio of the crude oil to the treating agent to the additive is 1: 0.02: 0.005.
in the step (3), the treating agent can be repeatedly used after being treated at the high temperature of 300 ℃ to degrade aflatoxin.
Example 2:
a preparation method of edible oil for effectively reducing aflatoxin content comprises the following specific steps:
(1) preparation of the treating agent: adding nickel nitrate hexahydrate, yttrium nitrate hexahydrate and gadolinium nitrate hexahydrate into N, N' -dimethylformamide, uniformly oscillating by ultrasonic waves, adding polyacrylonitrile, stirring to prepare spinning solution, performing electrostatic spinning, drying and calcining to obtain a treating agent for later use;
(2) preparation of the additive: dissolving chitosan in 0.3mol/L acetic acid solution, adding lecithin, uniformly oscillating by ultrasonic waves, averagely dividing into two parts, adding perillaldehyde and linalool oil into one part, adding bacillus subtilis CMCC63501 into the other part, respectively emulsifying, combining, and freeze-drying in vacuum to obtain the additive for later use;
(3) and (2) squeezing the oil-containing plant raw materials to obtain crude oil, adding the treating agent obtained in the step (1) into the crude oil, naturally illuminating for 20 minutes, adding the additive obtained in the step (2), continuously illuminating for 5 minutes, and enriching and removing the treating agent by using a magnet.
In the step (1), the mass-to-volume ratio of nickel nitrate hexahydrate, yttrium nitrate hexahydrate, gadolinium nitrate hexahydrate, N' -dimethylformamide and polyacrylonitrile is 1 g: 3 g: 1.5 g: 800 mL: 80 g.
In the step (1), the process conditions of ultrasonic oscillation are as follows: shaking at 300W for 40 minutes.
In the step (1), the preparation process conditions of the spinning solution are as follows: stirred at 70 ℃ for 18 hours.
In the step (1), the electrostatic spinning process conditions are as follows: the feed rate of the spinning solution was 1.3 mL/hr, the spinning voltage was 18kV, and the spinning distance was 16 cm.
In the step (1), the drying process conditions are as follows: ventilating and drying for 10 hours at the temperature of 45 ℃; the calcination process conditions are as follows: calcining at 480 ℃ for 80 minutes.
In the step (2), the mass volume ratio of the chitosan, the acetic acid solution, the lecithin, the bacillus subtilis CMCC63501, the perillaldehyde and the linalool oil is 0.1 g: 60mL of: 0.05 g: 0.1 g: 0.05 g: 0.2 g.
In the step (2), the specific method for emulsification is as follows: vortex for 15s, and then pass through the membrane repeatedly 3 times by membrane emulsifier at a speed of 35 mL/min.
In the step (2), the process conditions of vacuum freeze drying are as follows: freezing at-50 deg.C for 8 hr, vacuumizing to 3Pa, heating to 20 deg.C, and maintaining vacuum degree for 8 hr.
In the step (3), the oil-containing plant material is peanut kernels.
In the step (3), the specific method for squeezing is as follows:
(A) firstly, drying the oil-containing plant raw material, and crushing to obtain powder with the particle size of 0.5 mm;
(B) pretreating the powder by adopting a steam explosion technology, and then micronizing the powder to below 200 nm;
(C) and (C) squeezing the powder treated in the step (B) by using a screw oil press to obtain crude oil.
In the step (B), the process conditions of the steam explosion technology are as follows: and (3) loading the powder into a blasting cavity of steam blasting equipment, keeping the powder for 1 minute under the condition of 1MPa, and then quickly releasing the pressure.
In the step (B), carrying out superfine grinding by using a jet mill under the working conditions of: the air pressure was 1200kPa, the feed rate was 200r/min, the classification frequency was 35Hz, and the crushing time was 60 minutes.
The specific method of the step (C) is as follows: and (3) idling the screw oil press for 3 minutes, feeding the material while the material is hot, and starting squeezing when the temperature of the machine body reaches 70 ℃ until no oil flows out.
In the step (3), the mass ratio of the crude oil to the treating agent to the additive is 1: 0.01: 0.008.
in the step (3), the treating agent can be repeatedly used after being treated at the high temperature of 300 ℃ to degrade aflatoxin.
Example 3:
a preparation method of edible oil for effectively reducing aflatoxin content comprises the following specific steps:
(1) preparation of the treating agent: adding nickel nitrate hexahydrate, yttrium nitrate hexahydrate and gadolinium nitrate hexahydrate into N, N' -dimethylformamide, uniformly oscillating by ultrasonic waves, adding polyacrylonitrile, stirring to prepare spinning solution, performing electrostatic spinning, drying and calcining to obtain a treating agent for later use;
(2) preparation of the additive: dissolving chitosan in 0.25mol/L acetic acid solution, adding lecithin, uniformly oscillating by ultrasonic waves, averagely dividing into two parts, adding perillaldehyde and linalool oil into one part, adding bacillus subtilis CMCC63501 into the other part, respectively emulsifying, combining, and freeze-drying in vacuum to obtain the additive for later use;
(3) and (2) squeezing the oil-containing plant raw materials to obtain crude oil, adding the treating agent obtained in the step (1) into the crude oil, naturally illuminating for 25 minutes, adding the additive obtained in the step (2), continuously illuminating for 4 minutes, and enriching and removing the treating agent by using a magnet.
In the step (1), the mass-to-volume ratio of nickel nitrate hexahydrate, yttrium nitrate hexahydrate, gadolinium nitrate hexahydrate, N' -dimethylformamide and polyacrylonitrile is 1 g: 4 g: 1.3 g: 900 mL: 70 g.
In the step (1), the process conditions of ultrasonic oscillation are as follows: shaking at 400W for 35 minutes.
In the step (1), the preparation process conditions of the spinning solution are as follows: stirred at 75 ℃ for 17 hours.
In the step (1), the electrostatic spinning process conditions are as follows: the feed rate of the spinning solution was 1.4 mL/hr, the spinning voltage was 16kV, and the spinning distance was 17 cm.
In the step (1), the drying process conditions are as follows: ventilating and drying at 40 ℃ for 11 hours; the calcination process conditions are as follows: calcined at 460 ℃ for 90 minutes.
In the step (2), the mass volume ratio of the chitosan, the acetic acid solution, the lecithin, the bacillus subtilis CMCC63501, the perillaldehyde and the linalool oil is 0.1 g: 55mL of: 0.06 g: 0.09 g: 0.07 g: 0.15 g.
In the step (2), the specific method for emulsification is as follows: vortex for 18s, then pass through the membrane repeatedly for 2 times by the membrane emulsifier, the membrane passing speed is 38 mL/min.
In the step (2), the process conditions of vacuum freeze drying are as follows: freezing at-45 deg.C for 9 hr, vacuumizing to 2Pa, heating to 25 deg.C, and maintaining vacuum degree for 7 hr.
In the step (3), the oil-containing plant material is peanut kernels.
In the step (3), the specific method for squeezing is as follows:
(A) firstly, drying the oil-containing plant raw material, and crushing to obtain powder with the particle size of 0.5 mm;
(B) pretreating the powder by adopting a steam explosion technology, and then micronizing the powder to below 200 nm;
(C) and (C) squeezing the powder treated in the step (B) by using a screw oil press to obtain crude oil.
In the step (B), the process conditions of the steam explosion technology are as follows: and (3) loading the powder into a blasting cavity of steam blasting equipment, keeping the powder for 1 minute under the condition of 1MPa, and then quickly releasing the pressure.
In the step (B), carrying out superfine grinding by using a jet mill under the working conditions of: the air pressure was 1200kPa, the feed rate was 200r/min, the classification frequency was 35Hz, and the crushing time was 60 minutes.
The specific method of the step (C) is as follows: and (3) idling the screw oil press for 3 minutes, feeding the material while the material is hot, and starting squeezing when the temperature of the machine body reaches 70 ℃ until no oil flows out.
In the step (3), the mass ratio of the crude oil to the treating agent to the additive is 1: 0.015: 0.006.
in the step (3), the treating agent can be repeatedly used after being treated at the high temperature of 300 ℃ to degrade aflatoxin.
Comparative example 1
Gadolinium nitrate hexahydrate is omitted in the preparation of the treating agent.
The rest is the same as example 1.
Comparative example 2
When preparing the additive, the bacillus subtilis CMCC63501, the perillaldehyde and the linalool are added together.
The rest is the same as example 1.
Comparative example 3
Bacillus subtilis CMCC63501 was omitted when preparing the additive.
The rest is the same as example 1.
Comparative example 4
The linalool oil is omitted when the additive is prepared.
The rest is the same as example 1.
Comparative example 5
The chitosan is omitted when the additive is prepared.
The rest is the same as example 1.
Comparative example 6
The method of the step (3) is as follows: squeezing the oil-containing plant raw materials to obtain crude oil, adding the treating agent obtained in the step (1) into the crude oil, naturally irradiating for 33 minutes, adding the additive obtained in the step (2), and enriching and removing the treating agent by using a magnet.
The rest is the same as example 1.
Test examples
The aflatoxin B of the edible oil obtained in the examples 1-3 and the comparative examples 1-5 is determined by referring to a third method-a high performance liquid chromatography post-derivation method of GB/T5009.22-2016 (determination of aflatoxin B and G groups in food)1Content (0 month), respectively inspecting aflatoxin B in the solution after the solution is left open for 1 month and stored in a sealed manner for 18 months at 30 ℃ in a dark place1And (4) content. The results are shown in Table 1.
TABLE 1 aflatoxins B in edible oils1Results of content investigation
Figure BDA0002502383180000081
Figure BDA0002502383180000091
As can be seen from Table 1, the edible oils obtained in examples 1 to 3 had a low aflatoxin content, which is far below the national standard (10. mu.g/kg).
In the comparative example 1, gadolinium nitrate hexahydrate is omitted during preparation of the treating agent, the electronic conduction bridging effect of gadolinium is avoided, and the photocatalytic degradation effect of the treating agent on aflatoxin is obviously poor; comparative example 2 when preparing the additive, bacillus subtilis CMCC63501, perillaldehyde and linalool are added together, and the perillaldehyde influences the activity of the bacillus subtilis and further influences the inhibition effect on aflatoxin; comparative example 3 omits the bacillus subtilis CMCC63501 when preparing the additive, and comparative example 4 omits the linalool oil when preparing the additive, and lacks the synergistic effect of the components, thus influencing the inhibiting effect on the aflatoxin; the comparative example 5 omits the chitosan, thereby influencing the removal of the low-polarity aflatoxin and the inhibition effect on the aflatoxin in the subsequent storage process; comparative example 6 after adding the treating agent, natural light irradiation for 33 minutes, adding the additive, namely adding the additive and then not carrying out natural light irradiation treatment, losing the interaction of the treating agent and the additive, influencing the treatment effect on the crude oil and the inhibition effect on the aflatoxin in the preservation process.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (9)

1. The preparation method of the edible oil for effectively reducing the content of the aflatoxin is characterized by comprising the following specific steps of:
(1) preparation of the treating agent: adding nickel nitrate hexahydrate, yttrium nitrate hexahydrate and gadolinium nitrate hexahydrate into N, N' -dimethylformamide, uniformly oscillating by ultrasonic waves, adding polyacrylonitrile, stirring to prepare spinning solution, performing electrostatic spinning, drying and calcining to obtain a treating agent for later use;
(2) preparation of the additive: dissolving chitosan in 0.2-0.3 mol/L acetic acid solution, adding lecithin, uniformly oscillating by ultrasonic waves, averagely dividing into two parts, adding perillaldehyde and linalool oil into one part, adding bacillus subtilis CMCC63501 into the other part, respectively emulsifying, combining, and freeze-drying in vacuum to obtain an additive for later use;
(3) and (2) squeezing the oil-containing plant raw materials to obtain crude oil, adding the treating agent obtained in the step (1) into the crude oil, naturally illuminating for 20-30 minutes, adding the additive obtained in the step (2), continuously illuminating for 3-5 minutes, and enriching and removing the treating agent by using a magnet.
2. The method according to claim 1, wherein in the step (1), the mass-to-volume ratio of nickel nitrate hexahydrate, yttrium nitrate hexahydrate, gadolinium nitrate hexahydrate, N' -dimethylformamide and polyacrylonitrile is 1 g: 3-5 g: 1.2-1.5 g: 800-1000 mL: 50-80 g.
3. The preparation method according to claim 1, wherein in the step (1), the process conditions of the ultrasonic oscillation are as follows: oscillating at 300-500W for 30-40 min.
4. The preparation method according to claim 1, wherein the process conditions for preparing the spinning solution in step (1) are as follows: stirring for 15-18 hours at 70-80 ℃.
5. The preparation method according to claim 1, wherein in the step (1), the electrostatic spinning process conditions are as follows: the feeding speed of the spinning solution is 1.3-1.5 mL/h, the spinning voltage is 15-18 kV, and the spinning distance is 16-18 cm.
6. The preparation method according to claim 1, wherein in the step (2), the mass-to-volume ratio of the chitosan, the acetic acid solution, the lecithin, the bacillus subtilis CMCC63501, the perillaldehyde and the linalool oil is 0.1 g: 50-60 mL: 0.05-0.08 g: 0.08-0.1 g: 0.05-0.08 g: 0.1 to 0.2 g.
7. The preparation method according to claim 1, wherein in the step (2), the specific method of emulsification is: and (3) firstly carrying out vortex oscillation for 15-20 s, and then repeatedly passing through the membrane for 2-3 times by using a membrane emulsifier, wherein the membrane passing speed is 35-40 mL/min.
8. The method according to claim 1, wherein in the step (3), the pressing is performed by the following method:
(A) firstly, drying the oil-containing plant raw material, and crushing to obtain powder with the particle size of 0.5 mm;
(B) pretreating the powder by adopting a steam explosion technology, and then micronizing the powder to below 200 nm;
(C) and (C) squeezing the powder treated in the step (B) by using a screw oil press to obtain crude oil.
9. The preparation method according to claim 1, wherein in the step (3), the mass ratio of the crude oil to the treating agent to the additive is 1: 0.01-0.02: 0.005-0.008.
CN202010436248.8A 2020-05-21 2020-05-21 Preparation method of edible oil capable of effectively reducing aflatoxin content Withdrawn CN111548853A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113831961A (en) * 2021-09-22 2021-12-24 中国农业大学 Walnut oil extraction method
CN114984258A (en) * 2021-03-02 2022-09-02 中国农业科学院油料作物研究所 Green method for efficiently inhibiting growth of aspergillus flavus spores producing toxin

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114984258A (en) * 2021-03-02 2022-09-02 中国农业科学院油料作物研究所 Green method for efficiently inhibiting growth of aspergillus flavus spores producing toxin
CN114984258B (en) * 2021-03-02 2023-09-26 中国农业科学院油料作物研究所 Green method for efficiently inhibiting growth of toxic aspergillus flavus spores
CN113831961A (en) * 2021-09-22 2021-12-24 中国农业大学 Walnut oil extraction method

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