CN111264702A - Antioxidant microemulsion for feed and preparation method and application thereof - Google Patents

Antioxidant microemulsion for feed and preparation method and application thereof Download PDF

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Publication number
CN111264702A
CN111264702A CN202010141923.4A CN202010141923A CN111264702A CN 111264702 A CN111264702 A CN 111264702A CN 202010141923 A CN202010141923 A CN 202010141923A CN 111264702 A CN111264702 A CN 111264702A
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parts
antioxidant
feed
microemulsion
acid
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勾连军
颜世敢
夏锋
刘伟
李永强
周根斌
李长亮
王怡
李峰
王德林
王福达
勾翔
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Jiangsu Aozhong Biological Technology Co ltd
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Jiangsu Aozhong Biological Technology Co ltd
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    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23K—FODDER
    • A23K20/00—Accessory food factors for animal feeding-stuffs
    • A23K20/10—Organic substances
    • A23K20/158—Fatty acids; Fats; Products containing oils or fats
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23K—FODDER
    • A23K20/00—Accessory food factors for animal feeding-stuffs
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23K—FODDER
    • A23K20/00—Accessory food factors for animal feeding-stuffs
    • A23K20/10—Organic substances
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23K—FODDER
    • A23K20/00—Accessory food factors for animal feeding-stuffs
    • A23K20/10—Organic substances
    • A23K20/105—Aliphatic or alicyclic compounds
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23K—FODDER
    • A23K20/00—Accessory food factors for animal feeding-stuffs
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    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23K—FODDER
    • A23K20/00—Accessory food factors for animal feeding-stuffs
    • A23K20/10—Organic substances
    • A23K20/142—Amino acids; Derivatives thereof
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23K—FODDER
    • A23K20/00—Accessory food factors for animal feeding-stuffs
    • A23K20/20—Inorganic substances, e.g. oligoelements
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23K—FODDER
    • A23K20/00—Accessory food factors for animal feeding-stuffs
    • A23K20/20—Inorganic substances, e.g. oligoelements
    • A23K20/26—Compounds containing phosphorus
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
    • A23L3/34—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals
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    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
    • A23L3/34—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals
    • A23L3/3454—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals in the form of liquids or solids
    • A23L3/3463—Organic compounds; Microorganisms; Enzymes
    • A23L3/3481—Organic compounds containing oxygen
    • A23L3/349—Organic compounds containing oxygen with singly-bound oxygen
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
    • A23L3/34—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals
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    • A23L3/3463—Organic compounds; Microorganisms; Enzymes
    • A23L3/3481—Organic compounds containing oxygen
    • A23L3/3508—Organic compounds containing oxygen containing carboxyl groups
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
    • A23L3/34—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals
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    • A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
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    • A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
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    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A40/00—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production
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Abstract

The invention discloses an antioxidant microemulsion for feed and a preparation method and application thereof, wherein the antioxidant microemulsion comprises the following raw materials: the antioxidant is prepared from the components of ethylenediamine tetraacetic acid, tea polyphenol, grape seed extract, polypeptide amino acid, modified antioxidant, stearic acid, silicon dioxide, phosphoric acid, ethanol and water, and is safe, so that the problem of safety risk of the antioxidant in the prior art is solved, the antioxidant performance of grease is improved, target treatment is performed on metal ions, the fusion degree of the antioxidant and feed is improved, and the antioxidant has good antioxidant performance.

Description

Antioxidant microemulsion for feed and preparation method and application thereof
Technical Field
The invention belongs to the field of feed additives, and particularly relates to an antioxidant microemulsion for feed as well as a preparation method and application thereof.
Background
The oil and fat component is an important component of the feed and is an important energy supply substance. However, the fat components are easy to oxidize and deteriorate, so that the nutritional value is reduced, the heat energy is reduced, and meanwhile, the toxic and harmful substances such as aldehyde, ketone, acid, hydroperoxide and the like generated by fat peroxidation and rancidity are harmful to the health of animals.
The feed contains various oxidation promoting factors, such as iron, copper and other ions in the feed can promote the oxidation reaction under the high-temperature and high-humidity environment. In order to avoid the oxidation of the oil in the feed, an antioxidant is usually added into the feed to delay the oxidation process of the oil.
The antioxidant has antioxidant effect mechanism including ① chemical reaction with oxygen to lower the oxygen content in the system, such as L-ascorbic acid and its derivative, ② interruption of chain reaction in oxidation process to destroy oxidation process, such as tocopherol, tea polyphenol, dilauryl thiodipropionate and propyl gallate, ③ blocking catalytic heavy metal ion and oxidation inducing matter, prolonging the induction period of oxidation, slowing down the reaction speed, such as citric acid, phosphoric acid, tartaric acid, malic acid and other synergist, and ④ inhibiting and weakening enzyme activity, such as acetic acid.
Most of the feed antioxidants currently on the market are composed of Ethoxyquinoline (EQ), ditertiary-butylhydroxytoluene, tert-butylhydroxyanisole and other components, and a ph regulator and a carrier component. However, ethoxyquin has a less than ideal antioxidant effect on grease, but has a better vitamin protection effect, and can lead to deeper color change of products during storage of the products. European Union 2017, G/SPS/EU/190 bulletin: the addition of ethoxyquinoline to animal feed was discontinued due to the carcinogenic genotoxicity of ethoxyquinoneimine and P-Phenetidine (P-Phenetidine) remaining in ethoxyquinoline.
Tert-butyl hydroxyanisole and propyl gallate (PG for short) are also common feed antioxidants at present, and the preparation form of the antioxidant is granular crystals, so that the antioxidant cannot be completely fused with feed, is high in cost and is not suitable for production of a large amount of feed antioxidants. Ethoxyquinoline (EQ) has poor antioxidant effect on certain oils and fats, has potential safety hazard, has side effect on animal immunity, and can reduce the disease resistance of animals after long-term use of ethoxyquinoline-containing feed (the latest progress of feed antioxidant application, Chinese feed additive 2015, 12: 1-4). The tert-butyl hydroquinone has the best antioxidation effect on the fish oil, but has higher price and limited use.
The 2, 6-di-tert-butyl-4-methylphenol (BHT) and the Butyl Hydroxy Anisole (BHA) have low cost, but have certain side effects, and the effect is not as good as that of tert-butyl hydroquinone. Meanwhile, antioxidants such as 2, 6-di-tert-butyl-4-methylphenol (BHT), Butyl Hydroxyanisole (BHA) and the like are crystalline particles, and BHT and feed are still respectively and independently present under the observation of a microscope, and even when BHT is fed into an animal body, BHT still exists in a particle state, solid components cannot be directly contacted with free radicals, so that the antioxidant effect cannot be fully exerted, and the antioxidant effect is not good.
Disclosure of Invention
The invention provides an antioxidant microemulsion for feed and a preparation method and application thereof, and solves the problems that in the prior art, an antioxidant has safety risk, oil and fat have poor antioxidant property, target treatment is not carried out on metal ions, a powder form cannot be completely fused with feed, and the antioxidant effect cannot be fully exerted.
The specific technical scheme is as follows:
an antioxidant microemulsion for feed comprises the following raw materials in parts by weight: 10-15 parts of ethylene diamine tetraacetic acid, 5-15 parts of tea polyphenol, 5-15 parts of grape seed extract, 30-40 parts of polypeptide amino acid, 25-30 parts of modified antioxidant, 3-5 parts of stearic acid, 2-5 parts of silicon dioxide, 3-5 parts of phosphoric acid, 5-15 parts of ethanol and 40-50 parts of water.
Preferably, the feed comprises the following raw materials in parts by weight: 12 parts of ethylenediamine tetraacetic acid, 7 parts of tea polyphenol, 5 parts of grape seed extract, 30 parts of polypeptide amino acid, 30 parts of modified antioxidant, 4 parts of stearic acid, 3 parts of silicon dioxide, 3 parts of phosphoric acid, 7 parts of ethanol and 45 parts of water.
Preferably, the modified antioxidant comprises the following raw materials in parts by weight: 20-25 parts of antioxidant, 15-20 parts of soybean oil and 5-10 parts of emulsifier.
Preferably, the preparation method of the modified antioxidant is as follows: treating the antioxidant in a high pressure machine, then crushing the antioxidant by airflow to obtain powdery solid, then preparing oxygen into plasma at the temperature of 2600-; heating and mixing the soybean oil and the superfine particles in corresponding parts, cooling in a water bath, adding the emulsifier under nitrogen flow, controlling the reaction temperature to be 45-50 ℃, and continuously stirring for 8 hours to react to obtain the modified antioxidant.
Preferably, the antioxidant consists of di-tert-butyl hydroxy toluene, tert-butyl hydroquinone and 2, 6-di-tert-butyl-p-cresol, wherein the mass ratio of the tert-butyl hydroquinone to the 2, 6-di-tert-butyl-p-cresol is 5: 1.
A preparation method of the antioxidant microemulsion for feed comprises the following steps:
firstly, mixing stearic acid, phosphoric acid, ethanol and water together, and uniformly stirring to prepare a water phase; slowly adding the aqueous phase solution into a modified oxidant while stirring, uniformly stirring, then adding the corresponding parts of ethylenediamine tetraacetic acid, tea polyphenol, grape seed extract and polypeptide amino acid into a vacuum ionization reaction chamber, wherein the temperature is 45 ℃, the vacuum degree is 0.1MPa, the pulse arc discharge is 10kV and 10ms, the reaction time is 40min, and after the reaction is finished, introducing nitrogen and cooling to normal temperature; and adding the product into a stainless steel reaction tank, adding silicon dioxide, stirring for 1h, and cooling to normal temperature.
A grease for feed containing the antioxidant microemulsion for feed as set forth in any one of claims 1 to 4.
Preferably, the content of the antioxidant microemulsion for feed is 0.08-0.12 wt%.
Preferably, a feed comprising the grease for feed as claimed in claim 7.
Preferably, the addition amount of the grease for feedstuff is 0.01-0.1 wt%.
Has the advantages that:
1. the invention provides an antioxidant microemulsion for feed, which adopts safe components without toxicity and side effects, solves the problem of safety risk of antioxidants in the prior art, improves the antioxidant property of oil, performs target treatment on metal ions, improves the fusion degree of the antioxidants and the feed, and fully exerts the antioxidant effect.
2. The invention has particularly remarkable anti-oxidation effect on grease, simultaneously takes the anti-oxidation effect on protein into account, and can more thoroughly solve the anti-oxidation problem of the feed. The EDTA is adopted, so that the metal ions in the feed are effectively treated, the metal ions are reduced, the process that the carbon-hydrogen bond on the methyl carbon atom adjacent to the double bond of the fatty acid is cracked to generate hydrogen atoms and free radicals is inhibited, the reaction speed of the first-stage reaction can be effectively inhibited, and the purpose of resisting oxidation is achieved.
3. The method adopts modified antioxidant, the antioxidant is put into a high pressure machine for treatment, then the antioxidant is crushed by airflow to obtain powdery solid, then oxygen is made into plasma by a high-frequency plasma generator, and the powdery solid is decomposed into superfine particles in a plasma reaction furnace; heating and mixing soybean oil and superfine particles in corresponding parts, cooling in a water bath, adding an emulsifier under nitrogen flow, controlling the reaction temperature to be 45-50 ℃, continuously stirring for 8 hours to react to obtain a modified antioxidant, and performing a synergistic effect with tea polyphenol and a grape seed extract in a subsequent process to avoid negative effects of the conventional antioxidant on the tea polyphenol and the grape seed extract, so that the chain growth of oxygen radicals can be inhibited, and the start of the reaction in the termination period of an oxidation process is effectively inhibited; the oxidation of the grease can cause a large amount of protein oxidation, which is indirectly called as a catalyst in the protein oxidation process, and by the technical means, oxygen free radicals can be effectively eliminated, and the reaction is controlled in the second stage and does not progress downwards, so that the antioxidation effect is improved.
4. The invention adopts the steps of mixing stearic acid, phosphoric acid, ethanol and water together, and uniformly stirring to prepare a water phase; slowly adding the aqueous phase solution into a modified oxidant while stirring, uniformly stirring, then adding the corresponding parts of ethylenediamine tetraacetic acid, tea polyphenol, grape seed extract and polypeptide amino acid into a vacuum ionization reaction chamber, wherein the temperature is 45 ℃, the vacuum degree is 0.1MPa, the pulse arc discharge is 10kV and 10ms, the reaction time is 40min, and after the reaction is finished, introducing nitrogen and cooling to normal temperature; the method comprises the steps of adding the product into a stainless steel reaction tank, adding silicon dioxide, stirring for 1 hour, and cooling to normal temperature, organically combining the components into a copolymer on the premise of not influencing the functions of the components, preparing an emulsion, and combining the emulsion with feed more fully to achieve a good antioxidant effect.
5. Because EDTA belongs to indissolvable particles, and the method of adding the emulsifier has obvious inhibiting effect on the dissolution of various composite organic matters and the exertion of the functions of all components, the invention adopts the grafting copolymerization technology under vacuum ionization, namely that the temperature in a vacuum ionization reaction chamber is 45 ℃, the vacuum degree is 0.1MPa, the pulse arc discharge is 10kV and 10ms, the reaction time is 40min, and after the reaction is finished, nitrogen is introduced to be reduced to the normal temperature; adding the product into a stainless steel reaction tank, adding silicon dioxide, stirring for 1h, and cooling to normal temperature, wherein polypeptide amino acid is adopted as a main stem, EDTA, tea polyphenol and grape seed extract are adopted as branched chains, the polypeptide amino acid has long molecular chain, is non-toxic and free of side effect, is easy to absorb and decompose, and does not harm livestock and the like; according to the invention, polypeptide amino acid is used as a main stem, EDTA, tea polyphenol and grape seed extract are used as branched chains to form a graft copolymer, and then stearic acid and silicon dioxide are added to form an emulsion, so that the oxidation of the feed can be effectively prevented.
6. The invention solves the problem of slow diffusion of the liquid antioxidant by adding the antioxidant component, simultaneously adding absolute ethyl alcohol and phosphoric acid instead of adopting a single common solvent
7. The Tween-80 and span-80 emulsifiers are adopted to form a uniform microemulsion through emulsification, so that two antioxidant components can be better mixed and dissolved in the emulsion, the synergistic oxidation resistance of the two antioxidant components is exerted, the oxidation resistance effect is improved, meanwhile, the prepared microemulsion is a thermodynamic stable system, the stable state can be kept for a long time, and the synergistic oxidation resistance effect among the antioxidant components is more durable.
8. The antioxidant microemulsion for feed prepared by the invention has wide application range, is suitable to be used as an additive to be added into feed grease, fish meal and bone meal to play an antioxidation role, and can also be used as feed grease to be directly added into various premixes, concentrated materials and complete materials to be used.
Detailed Description
The present invention will be described in detail and clearly with reference to the following examples.
Example 1:
the antioxidant microemulsion for feed comprises the following raw materials, by weight, 10 parts of ethylenediamine tetraacetic acid, 6 parts of tea polyphenol, 7 parts of grape seed extract, 35 parts of polypeptide amino acid, 28 parts of modified antioxidant, 4 parts of stearic acid, 3 parts of silicon dioxide, 4 parts of phosphoric acid, 8 parts of ethanol and 45 parts of water.
The modified antioxidant comprises the following raw materials in parts by weight: 25 parts of antioxidant, 15 parts of soybean oil and 8 parts of emulsifier; the antioxidant consists of di-tert-butyl hydroxy toluene, tert-butyl hydroquinone and 2, 6-di-tert-butyl-p-cresol, wherein the mass ratio of the tert-butyl hydroquinone to the 2, 6-di-tert-butyl-p-cresol is 5: 1; the emulsifier comprises two components of Tween-80 and span-80, wherein the mass percentages of the Tween-80 and the span-80 are respectively 20: 17.
the preparation method of EDTA in the antioxidant microemulsion for feed comprises the following steps:
in a 800L stainless steel condensation reaction tank, chloroacetic acid, ice and 30% sodium hydroxide solution are added according to the mass ratio of 1:1:1.35, and 84% ethylenediamine is added under stirring. After the temperature is kept at 15 ℃ for 1h, 10L of 30% sodium hydroxide solution is added in batches each time, the next batch is added after the phenolphthalein indicator does not show alkalinity after each addition, and finally the reactant shows alkalinity. Keeping at room temperature for 12h, heating to 90 deg.C, adding activated carbon, filtering, washing the residue with water, and collecting the final solution with a total volume of about 600L. Adding concentrated hydrochloric acid until the pH value is not less than 3, and separating out crystals. Filtering and washing with water until no chlorine radical is generated. Drying to obtain the EDTA.
The preparation method of tea polyphenol comprises the following steps:
in a refluxing reaction chamber as follows 1:10 adding tea dust and 60% ethanol solution, refluxing for 3 hours, filtering and retaining filtrate; and adding the residue into 80% ethanol solution according to the ratio of 1:10, refluxing for 2 hours, filtering and storing the filtrate. And after two times of reflux, combining the filter liquor, adding activated carbon for adsorption for 1 hour, washing with water until the filter liquor is colorless, eluting with NaOH solution, neutralizing, and drying with hot water bath to obtain a finished product.
The preparation method of the grape seed extract comprises the following steps:
mixing fermented grape seed with petroleum ether, standing for 6 hr for defatting, and pulverizing with pulverizer. Cleaning fine sand, sieving with 200 mesh sieve, mixing with grape seed powder at a ratio of 2:1, and placing into an extraction chamber. Pumping n-hexane into the extraction chamber via a high-pressure pump, and heating the extraction chamber to 80 deg.C and 40 MPa. After 20 minutes, the heating was stopped, and after 30 minutes of standing, nitrogen gas was introduced and the extract was collected by nitrogen-blown concentration.
The preparation method of the polypeptide comprises the following steps:
pretreatment of raw materials: unfreezing the frozen fish, cleaning with clear water, and uniformly chopping into meat paste;
preparing fish paste: dispersing meat paste in distilled water to form fish paste, wherein the mass ratio of the meat paste to the distilled water is 1: 2;
engraulis japonicus enzymolysis: adding a phosphate buffer solution into the fish paste to regulate the pH value to 6.5, and then adding exogenous enzyme into the fish paste for enzymolysis to form an enzymolysis solution;
enzyme deactivation: after the enzymolysis reaction is finished, the enzymolysis liquid is placed in a boiling water bath to be heated until the enzyme is inactivated.
The preparation method of the modified antioxidant comprises the following steps:
treating an antioxidant in a high-pressure machine, then crushing by airflow to obtain powdery solid, then preparing oxygen into plasma at 2600 ℃ by using a high-frequency plasma generator, and then decomposing the powdery solid into superfine particles in a plasma reaction furnace under the conditions of 1000 ℃ and 0.8 second of residence time; heating and mixing the soybean oil and the superfine particles in corresponding parts, cooling in a water bath, adding the emulsifier under nitrogen flow, controlling the reaction temperature to be 48 ℃, and continuously stirring for 8 hours to react to obtain the modified antioxidant.
After preparing the raw materials, firstly mixing stearic acid, phosphoric acid, ethanol and water together, and uniformly stirring to prepare a water phase; slowly adding the aqueous phase solution into a modified oxidant while stirring, uniformly stirring, then adding the corresponding parts of ethylenediamine tetraacetic acid, tea polyphenol, grape seed extract and polypeptide amino acid into a vacuum ionization reaction chamber, wherein the temperature is 45 ℃, the vacuum degree is 0.1MPa, the pulse arc discharge is 10kV and 10ms, the reaction time is 40min, and after the reaction is finished, introducing nitrogen and cooling to normal temperature; and adding the product into a stainless steel reaction tank, adding silicon dioxide, stirring for 1h, and cooling to normal temperature to obtain the antioxidant microemulsion for the feed. The antioxidant microemulsion for the feed is microemulsion. The microemulsion is an emulsion with the particle size of 5-100 nanometers.
Example 2:
the antioxidant microemulsion for feed comprises the following raw materials in parts by weight: 12 parts of ethylenediamine tetraacetic acid, 7 parts of tea polyphenol, 5 parts of grape seed extract, 30 parts of polypeptide amino acid, 30 parts of modified antioxidant, 4 parts of stearic acid, 3 parts of silicon dioxide, 3 parts of phosphoric acid, 7 parts of ethanol and 45 parts of water.
The modified antioxidant comprises the following raw materials in parts by weight: 20 parts of antioxidant, 17 parts of soybean oil and 10 parts of emulsifier; the antioxidant consists of di-tert-butyl hydroxy toluene, tert-butyl hydroquinone and 2, 6-di-tert-butyl-p-cresol, wherein the mass ratio of the tert-butyl hydroquinone to the 2, 6-di-tert-butyl-p-cresol is 5: 1; the emulsifier comprises two components of Tween-80 and span-80, wherein the mass percentages of the Tween-80 and the span-80 are respectively 16: 35.
the preparation method of EDTA comprises the following steps:
in a 800L stainless steel condensation reaction tank, chloroacetic acid, ice and 30% sodium hydroxide solution are added according to the mass ratio of 1:1:1.5, and 85% ethylenediamine is added under stirring. After the temperature is kept at 20 ℃ for 1h, 10L of 30% sodium hydroxide solution is added in batches each time, the next batch is added after the phenolphthalein indicator does not show alkalinity after each addition, and finally the reactant is alkaline. Keeping at room temperature for 12h, heating to 90 deg.C, adding activated carbon, filtering, washing the residue with water, and collecting the final solution with a total volume of about 600L. Adding concentrated hydrochloric acid until the pH value is not less than 3, and separating out crystals. Filtering and washing with water until no chlorine radical is generated. Drying to obtain the EDTA.
The preparation method of tea polyphenol comprises the following steps:
in a refluxing reaction chamber as follows 1:12 adding tea dust and 60% ethanol solution, refluxing for 3 hours, filtering and retaining filtrate; adding the residue into 80% ethanol solution according to the ratio of 1:12, refluxing for 2 hours, filtering and storing the filtrate. After twice reflux, the filter liquor is merged, then added with active carbon for adsorption for 1 hour and washed until colorless, then eluted by NaOH solution, neutralized and dried by hot water bath to obtain the finished product
The preparation method of the grape seed extract comprises the following steps:
mixing fermented grape seed with petroleum ether, standing for 6 hr for defatting, and pulverizing with pulverizer. Cleaning fine sand, sieving with 200 mesh sieve, mixing with grape seed powder at a ratio of 2.25:1, and placing into an extraction chamber. Pumping n-hexane into the extraction chamber via a high-pressure pump, and heating the extraction chamber to 80 deg.C and 40 MPa. After 20 minutes, the heating was stopped, and after 30 minutes of standing, nitrogen gas was introduced and the extract was collected by nitrogen-blown concentration.
The preparation method of the polypeptide comprises the following steps:
pretreatment of raw materials: unfreezing the frozen fish, cleaning with clear water, and uniformly chopping into meat paste;
preparing fish paste: dispersing meat paste in distilled water to form fish paste, wherein the mass ratio of the meat paste to the distilled water is 1: 2.75;
engraulis japonicus enzymolysis: adding a phosphate buffer solution into the fish paste to regulate the pH value to 6.5, and then adding exogenous enzyme into the fish paste for enzymolysis to form an enzymolysis solution;
enzyme deactivation: after the enzymolysis reaction is finished, the enzymolysis liquid is placed in a boiling water bath to be heated until the enzyme is inactivated.
Treating an antioxidant in a high-pressure machine, then crushing by airflow to obtain powdery solid, then preparing oxygen into plasma at 2700 ℃ by using a high-frequency plasma generator, and then decomposing the powdery solid into superfine particles in a plasma reaction furnace under the conditions of 1500 ℃ and 0.9 second of residence time; heating and mixing the soybean oil and the superfine particles in corresponding parts, cooling in a water bath, adding the emulsifier under nitrogen flow, controlling the reaction temperature to be 50 ℃, and continuously stirring for 8 hours to react to obtain the modified antioxidant.
After preparing the raw materials, firstly mixing stearic acid, phosphoric acid, ethanol and water together, and uniformly stirring to prepare a water phase; slowly adding the aqueous phase solution into a modified oxidant while stirring, uniformly stirring, then adding the corresponding parts of ethylenediamine tetraacetic acid, tea polyphenol, grape seed extract and polypeptide amino acid into a vacuum ionization reaction chamber, wherein the temperature is 45 ℃, the vacuum degree is 0.1MPa, the pulse arc discharge is 10kV and 10ms, the reaction time is 40min, and after the reaction is finished, introducing nitrogen and cooling to normal temperature; and adding the product into a stainless steel reaction tank, adding silicon dioxide, stirring for 1h, and cooling to normal temperature to obtain the antioxidant microemulsion for the feed. The antioxidant microemulsion for the feed is microemulsion. The microemulsion is an emulsion with the particle size of 5-100 nanometers.
Example 3:
the antioxidant microemulsion for feed comprises the following raw materials in parts by weight: 15 parts of ethylenediamine tetraacetic acid, 9 parts of tea polyphenol, 10 parts of grape seed extract, 40 parts of polypeptide amino acid, 30 parts of modified antioxidant, 5 parts of stearic acid, 5 parts of silicon dioxide, 5 parts of phosphoric acid, 10 parts of ethanol and 50 parts of water.
The modified antioxidant comprises the following raw materials in parts by weight: 23 parts of antioxidant, 18 parts of soybean oil and 7 parts of emulsifier; the antioxidant consists of di-tert-butyl hydroxy toluene, tert-butyl hydroquinone and 2, 6-di-tert-butyl-p-cresol, wherein the mass ratio of the tert-butyl hydroquinone to the 2, 6-di-tert-butyl-p-cresol is 5: 1; the emulsifier comprises two components of Tween-80 and span-80, wherein the mass percentages of the Tween-80 and the span-80 are respectively 25: 30.
the preparation method of EDTA comprises the following steps:
in a 800L stainless steel condensation reaction tank, chloroacetic acid, ice and 30% sodium hydroxide solution are added according to the mass ratio of 1:1.5:2, and 84% ethylenediamine is added under stirring. After the temperature is kept at 20 ℃ for 1h, 10L of 30% sodium hydroxide solution is added in batches each time, the next batch is added after the phenolphthalein indicator does not show alkalinity after each addition, and finally the reactant is alkaline. After keeping at room temperature for 19h, heating to 90 ℃, adding activated carbon, filtering, washing filter residues with water, and finally obtaining a solution with the total volume of about 600L. Adding concentrated hydrochloric acid until the pH value is not less than 3, and separating out crystals. Filtering and washing with water until no chlorine radical is generated. Drying to obtain the EDTA.
The preparation method of tea polyphenol comprises the following steps:
in a refluxing reaction chamber as follows 1:15 adding tea dust and 60% ethanol solution, refluxing for 3 hours, filtering and retaining filtrate; adding the residue into 80% ethanol solution according to the ratio of 1:15, refluxing for 2 hours, filtering and storing the filtrate. After twice reflux, the filter liquor is merged, then added with active carbon for adsorption for 1 hour and washed until colorless, then eluted by NaOH solution, neutralized and dried by hot water bath to obtain the finished product
The preparation method of the grape seed extract comprises the following steps:
mixing fermented grape seed with petroleum ether, standing for 6 hr for defatting, and pulverizing with pulverizer. Cleaning fine sand, sieving with 200 mesh sieve, mixing with grape seed powder at a ratio of 3:1, and placing into an extraction chamber. Pumping n-hexane into the extraction chamber via a high-pressure pump, and heating the extraction chamber to 80 deg.C and 40 MPa. After 30 minutes, the heating was stopped, and after 30 minutes of standing, nitrogen gas was introduced and the extract was collected by nitrogen-blown concentration.
The preparation method of the polypeptide comprises the following steps:
pretreatment of raw materials: unfreezing the frozen fish, cleaning with clear water, and uniformly chopping into meat paste;
preparing fish paste: dispersing meat paste in distilled water to form fish paste, wherein the mass ratio of the meat paste to the distilled water is 1: 3;
engraulis japonicus enzymolysis: adding a phosphate buffer solution into the fish paste to regulate the pH value to 7, and then adding exogenous enzyme into the fish paste for enzymolysis to form an enzymolysis solution;
enzyme deactivation: after the enzymolysis reaction is finished, the enzymolysis liquid is placed in a boiling water bath to be heated until the enzyme is inactivated.
Treating an antioxidant in a high-pressure machine, then crushing by airflow to obtain powdery solid, then preparing oxygen into plasma at the temperature of 2750 ℃ by using a high-frequency plasma generator, and then decomposing the powdery solid into superfine particles in a plasma reaction furnace under the conditions of 1300 ℃ and the residence time of 0.7 second; heating and mixing the soybean oil and the superfine particles in corresponding parts, cooling in a water bath, adding the emulsifier under nitrogen flow, controlling the reaction temperature to be 45 ℃, and continuously stirring for 8 hours to react to obtain the modified antioxidant.
After preparing the raw materials, firstly mixing stearic acid, phosphoric acid, ethanol and water together, and uniformly stirring to prepare a water phase; slowly adding the aqueous phase solution into a modified oxidant while stirring, uniformly stirring, then adding the corresponding parts of ethylenediamine tetraacetic acid, tea polyphenol, grape seed extract and polypeptide amino acid into a vacuum ionization reaction chamber, wherein the temperature is 45 ℃, the vacuum degree is 0.1MPa, the pulse arc discharge is 10kV and 10ms, the reaction time is 40min, and after the reaction is finished, introducing nitrogen and cooling to normal temperature; and adding the product into a stainless steel reaction tank, adding silicon dioxide, stirring for 1h, and cooling to normal temperature to obtain the antioxidant microemulsion for the feed. The antioxidant microemulsion for the feed is microemulsion. The microemulsion is an emulsion with the particle size of 5-100 nanometers.
Example 4:
the antioxidant microemulsion for feed comprises the following raw materials in parts by weight: 11 parts of ethylenediamine tetraacetic acid, 10 parts of tea polyphenol, 15 parts of grape seed extract, 35 parts of polypeptide amino acid, 30 parts of modified antioxidant, 3 parts of stearic acid, 4 parts of silicon dioxide, 3 parts of phosphoric acid, 5 parts of ethanol and 40 parts of water.
The modified antioxidant comprises the following raw materials in parts by weight: 21 parts of antioxidant, 20 parts of soybean oil and 5 parts of emulsifier; the antioxidant consists of di-tert-butyl hydroxy toluene, tert-butyl hydroquinone and 2, 6-di-tert-butyl-p-cresol, wherein the mass ratio of the tert-butyl hydroquinone to the 2, 6-di-tert-butyl-p-cresol is 5: 1; the emulsifier comprises two components of tween-80 and span-80, wherein the mass percentages of the tween-80 and the span-80 are respectively 21: 32.
the preparation method of EDTA comprises the following steps:
in a 800L stainless steel condensation reaction tank, chloroacetic acid, ice and 30% sodium hydroxide solution are added according to the mass ratio of 1:2:2.5, and 90% ethylenediamine is added under stirring. After the temperature is kept at 35 ℃ for 1h, 10L of 30% sodium hydroxide solution is added in batches each time, the next batch is added after the phenolphthalein indicator does not show alkalinity after each addition, and finally the reactant shows alkalinity. After keeping at room temperature for 24h, heating to 90 ℃, adding activated carbon, filtering, washing filter residues with water, and finally obtaining a solution with the total volume of about 600L. Adding concentrated hydrochloric acid until the pH value is not less than 3, and separating out crystals. Filtering and washing with water until no chlorine radical is generated. Drying to obtain the EDTA.
The preparation method of tea polyphenol comprises the following steps:
in a refluxing reaction chamber as follows 1:25 adding tea dust and 60% ethanol solution, refluxing for 3 hr, filtering and retaining filtrate; adding 80% ethanol solution into the residue according to the ratio of 1:25, refluxing for 2 hours, filtering and storing the filtrate. After twice reflux, the filter liquor is merged, then added with active carbon for adsorption for 1 hour and washed until colorless, then eluted by NaOH solution, neutralized and dried by hot water bath to obtain the finished product
The preparation method of the grape seed extract comprises the following steps:
mixing fermented grape seed with petroleum ether, standing for 6 hr for defatting, and pulverizing with pulverizer. Cleaning fine sand, sieving with 200 mesh sieve, mixing with grape seed powder at a ratio of 3:1, and placing into an extraction chamber. Pumping n-hexane into the extraction chamber via a high pressure pump, and heating the extraction chamber to 100 deg.C and 40 MPa. After 20 minutes, the heating was stopped, and after 30 minutes of standing, nitrogen gas was introduced and the extract was collected by nitrogen-blown concentration.
The preparation method of the polypeptide comprises the following steps:
pretreatment of raw materials: unfreezing the frozen fish, cleaning with clear water, and uniformly chopping into meat paste;
preparing fish paste: dispersing meat paste in distilled water to form fish paste, wherein the mass ratio of the meat paste to the distilled water is 1: 5;
engraulis japonicus enzymolysis: adding a phosphate buffer solution into the fish paste to regulate the pH value to 7.5, and then adding exogenous enzyme into the fish paste for enzymolysis to form an enzymolysis solution;
enzyme deactivation: after the enzymolysis reaction is finished, the enzymolysis liquid is placed in a boiling water bath to be heated until the enzyme is inactivated.
Treating antioxidant in a high pressure machine, pulverizing with gas flow to obtain powdered solid, making oxygen into plasma at 2800 deg.C with a high frequency plasma generator, and decomposing the powdered solid into superfine particles at 1450 deg.C and residence time of 1.0 s in a plasma reaction furnace; heating and mixing the soybean oil and the superfine particles in corresponding parts, cooling in a water bath, adding the emulsifier under nitrogen flow, controlling the reaction temperature to be 45 ℃, and continuously stirring for 8 hours to react to obtain the modified antioxidant.
After preparing the raw materials, firstly mixing stearic acid, phosphoric acid, ethanol and water together, and uniformly stirring to prepare a water phase; slowly adding the aqueous phase solution into a modified oxidant while stirring, uniformly stirring, then adding the corresponding parts of ethylenediamine tetraacetic acid, tea polyphenol, grape seed extract and polypeptide amino acid into a vacuum ionization reaction chamber, wherein the temperature is 45 ℃, the vacuum degree is 0.1MPa, the pulse arc discharge is 10kV and 10ms, the reaction time is 40min, and after the reaction is finished, introducing nitrogen and cooling to normal temperature; and adding the product into a stainless steel reaction tank, adding silicon dioxide, stirring for 1h, and cooling to normal temperature to obtain the antioxidant microemulsion for the feed. The antioxidant microemulsion for the feed is microemulsion. The microemulsion is an emulsion with the particle size of 5-100 nanometers.
The antioxidant microemulsion for feed prepared by the invention can be added into grease for feed, and the content of the antioxidant microemulsion for feed in the grease for feed is 0.08-0.12 wt%. The grease for feed can be added into feed, and the addition amount of the grease for feed in the feed is 0.01-0.1 wt%.
And (3) experimental detection:
1. measurement of antioxidant Property
The oxidation objects of the feed are mainly protein and grease in the feed. A common feed is selected, after the product of the invention and a commercial product are added, sampling examination is carried out on 7 th, 14 th, 28 th, 35 th and 60 th days after storage respectively, and color, smell and character of the samples are measured respectively.
1.1 color, odor, Properties measurement
Figure 158596DEST_PATH_IMAGE002
Figure 13420DEST_PATH_IMAGE004
Figure 980108DEST_PATH_IMAGE006
According to the experimental results, the feed product without the additive has obvious peculiar smell and discoloring in about 1 month, and the commercial product feed with the additive has peculiar smell and discoloring when being detected on the last 60 days. The added feed of the invention has no obvious discoloration and off-flavor in the detection process of 60 days.
1.2 TBA (Thiobabital acid number)
The product obtained in example 1 was added to soybean oil, fish oil, and soybean oil, respectively, at the same content to a final concentration of 200ppm, and the mixture was filled in a reagent bottle, sealed, placed in a thermostat at 40 ℃ and a humidity of 75%, and the thiobarbituric acid value (TAB) was measured at regular intervals.
Comparative example was set up in this experiment:
the other experimental procedure for group a was the same as in example 1 except that BHT was used instead of the modified antioxidant;
the other experimental procedure of group B was the same as in example 1 except that TBHQ was used instead of the modified antioxidant; and a blank control group.
The results of the measurements are shown in the following table.
Figure 375317DEST_PATH_IMAGE008
From the above table, it can be seen that the TBA (thiobarbituric acid number) of the product of the invention is lowest in soybean oil, fish oil or lard, compared to the blank control and the product made with the addition of conventional antioxidants, indicating that the product obtained with the feedstock and procedure of the invention has good oxidation resistance.
1.2 determination of nutrient content of feed
1.2.1 protein assay
The nitrogen content of the sample is measured by the Kjeldahl method, namely, in the presence of a catalyst, the organic matter is destroyed by sulfuric acid, and the nitrogen-containing matter is converted into ammonium sulfate. Adding strong base and distilling to make ammonia escape, after using boric acid to absorb it, using standard hydrochloric acid to titrate and measure the nitrogen content, and multiplying by 6.25 of conversion coefficient of nitrogen and protein to calculate crude protein content.
Figure 127372DEST_PATH_IMAGE010
The amount of protein reduction in the experiment is the amount of protein oxidation. From the table above it is clear that the feed without any addition had a protein loss of 61.3% during the period tested. The reduction rate of protein content of the feed product added with the invention in tested 60 days is 9.54 percent, and the reduction rate of the feed added with the commercial product is 28.5 percent. It can be seen that the antioxidant effect of the product of the invention is obviously superior to that of the product sold in the market.
1.2.2 measurement of crude fat
The determination of the feed fat is carried out by placing the sample in a first stage, repeatedly extracting with a fat-soluble solvent, and extracting the fat. The experiment was carried out by immersion method.
Figure 949835DEST_PATH_IMAGE012
The fat reduction amount in the experiment is the oxidation amount of the fat. From the graph it is clear that the feed without any additions lost 55.4% of fat during the period tested. The reduction rate of the fat content of the feed product added with the feed additive is 1.64 percent within 60 days, and the reduction rate of the feed added with the commercial product is 22.5 percent. Therefore, both the antioxidant and the antioxidant play a role in resisting fat oxidation, but the antioxidant effect of the product is obviously superior to that of the product sold in the market.
As can be seen from the table above, the feed added with the product of the invention is superior to the two groups in the experimental process in both physical properties and contents of protein and grease. The experimental data fully prove that the invention can effectively inhibit the oxidation of the oil and the protein in the feed and improve the oxidation resistance of the feed.
2. Determination of free metal ions
The metal ions were not measured by the conventional ashing method in this experiment because all organic components were destroyed by the ashing method and all forms of metal ions were measured. After EDTA is chelated with metal ions, the metal ions exist in a complex form, and free metal ions with a catalytic effect cannot be generated. Therefore, the experiment measures the free metal ions, and the atomic absorption spectrometry is adopted to measure the free metal ions in the aqueous solution.
Figure 905284DEST_PATH_IMAGE014
It is clear from the table above that the feed had a free iron reduction of 0.39% during the test period without any addition. The free iron reduction in the feed product of the invention was 92.7% within 60 days of testing and 5.49% with the commercial product feed. It can be seen that the free iron ion content of the commercial product is not reduced basically, but the free iron ion content of the product is greatly reduced.
Figure 41867DEST_PATH_IMAGE016
It is clear from the table above that the feed had a reduction of 0.1% in free copper ions during the test period without any addition. The decrease in free copper ions in the feed product of the invention was 93.3% within 60 days of testing and 10.2% with the commercial product feed. Therefore, the effect of the commercial product on reducing the content of free copper ions is poor, and the product greatly reduces the content of the free copper ions.
The experimental results show that the trend of the feed added with the commercial product is the same as that of the feed without the addition of the commercial product, and the metal ions are not changed basically, so that the commercial feed does not reduce the free metal ions. The product added with the feed of the invention can obviously reduce the content of free metal ions.
It is to be understood that the invention is not limited to the specific embodiments described above, but is intended to cover various insubstantial modifications of the inventive process concepts and solutions, or its application to other applications without modification.

Claims (10)

1. The antioxidant microemulsion for feed is characterized by comprising the following raw materials in parts by weight: 10-15 parts of ethylene diamine tetraacetic acid, 5-15 parts of tea polyphenol, 5-15 parts of grape seed extract, 30-40 parts of polypeptide amino acid, 25-30 parts of modified antioxidant, 3-5 parts of stearic acid, 2-5 parts of silicon dioxide, 3-5 parts of phosphoric acid, 5-15 parts of ethanol and 40-50 parts of water.
2. The antioxidant microemulsion for feed of claim 1, which comprises the following raw materials in parts by weight: 12 parts of ethylenediamine tetraacetic acid, 7 parts of tea polyphenol, 5 parts of grape seed extract, 30 parts of polypeptide amino acid, 30 parts of modified antioxidant, 4 parts of stearic acid, 3 parts of silicon dioxide, 3 parts of phosphoric acid, 7 parts of ethanol and 45 parts of water.
3. The antioxidant microemulsion as claimed in claim 1, wherein the modified antioxidant comprises the following raw materials in parts by weight: 20-25 parts of antioxidant, 15-20 parts of soybean oil and 5-10 parts of emulsifier.
4. The antioxidant microemulsion for feed of claim 1, wherein the modified antioxidant is prepared by the following method: treating the antioxidant in a high pressure machine, then crushing the antioxidant by airflow to obtain powdery solid, then preparing oxygen into plasma at the temperature of 2600-; heating and mixing the soybean oil and the superfine particles in corresponding parts, cooling in a water bath, adding the emulsifier under nitrogen flow, controlling the reaction temperature to be 45-50 ℃, and continuously stirring for 8 hours to react to obtain the modified antioxidant.
5. The antioxidant microemulsion as claimed in claim 3, wherein the antioxidant comprises di-tert-butylhydroxytoluene, tert-butylhydroquinone and 2, 6-di-tert-butyl-p-cresol, and the mass ratio of tert-butylhydroquinone to 2, 6-di-tert-butyl-p-cresol is 5: 1.
6. The preparation method of the antioxidant microemulsion for feed is characterized by comprising the following steps:
firstly, mixing stearic acid, phosphoric acid, ethanol and water together, and uniformly stirring to prepare a water phase; slowly adding the aqueous phase solution into a modified oxidant while stirring, uniformly stirring, then adding the corresponding parts of ethylenediamine tetraacetic acid, tea polyphenol, grape seed extract and polypeptide amino acid into a vacuum ionization reaction chamber, wherein the temperature is 45 ℃, the vacuum degree is 0.1MPa, the pulse arc discharge is 10kV and 10ms, the reaction time is 40min, and after the reaction is finished, introducing nitrogen and cooling to normal temperature; and adding the product into a stainless steel reaction tank, adding silicon dioxide, stirring for 1h, and cooling to normal temperature.
7. A grease for feed containing the antioxidant microemulsion for feed as set forth in any one of claims 1 to 4.
8. The grease as claimed in claim 7, wherein the antioxidant microemulsion for feedstuff is contained in an amount of 0.08 to 0.12 wt%.
9. A feed comprising the grease for feed as claimed in claim 7.
10. The feed according to claim 9, wherein the amount of the grease for feed is 0.01 to 0.1 wt%.
CN202010141923.4A 2020-03-04 2020-03-04 Antioxidant microemulsion for feed and preparation method and application thereof Pending CN111264702A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103518975A (en) * 2013-10-23 2014-01-22 麦仑(漳州)生物科技有限公司 Compound antioxidant for animal feeds as well as preparation method of compound antioxidant
CN106947594A (en) * 2017-05-10 2017-07-14 仲恺农业工程学院 Microemulsion for delaying oxidation of feed oil and preparation method thereof
CN109880133A (en) * 2019-01-21 2019-06-14 久耀电子科技（江苏）有限公司 A kind of fluorine resin mixture film and copper-clad plate preparation method

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103518975A (en) * 2013-10-23 2014-01-22 麦仑(漳州)生物科技有限公司 Compound antioxidant for animal feeds as well as preparation method of compound antioxidant
CN106947594A (en) * 2017-05-10 2017-07-14 仲恺农业工程学院 Microemulsion for delaying oxidation of feed oil and preparation method thereof
CN109880133A (en) * 2019-01-21 2019-06-14 久耀电子科技（江苏）有限公司 A kind of fluorine resin mixture film and copper-clad plate preparation method

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Application publication date: 20200612