CN113040277A - Composite vitamin nanoemulsion for livestock and preparation method and application thereof - Google Patents

Composite vitamin nanoemulsion for livestock and preparation method and application thereof Download PDF

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CN113040277A
CN113040277A CN202110375014.1A CN202110375014A CN113040277A CN 113040277 A CN113040277 A CN 113040277A CN 202110375014 A CN202110375014 A CN 202110375014A CN 113040277 A CN113040277 A CN 113040277A
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vitamin
parts
nanoemulsion
water
livestock
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高平
梁金兰
陈振威
李云
刘为和
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GUANGZHOU HESHENGTANG ANIMAL PHARMACEUTICAL CO Ltd
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GUANGZHOU HESHENGTANG ANIMAL PHARMACEUTICAL CO Ltd
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    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23KFODDER
    • A23K20/00Accessory food factors for animal feeding-stuffs
    • A23K20/10Organic substances
    • A23K20/174Vitamins
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23KFODDER
    • A23K20/00Accessory food factors for animal feeding-stuffs
    • A23K20/10Organic substances
    • A23K20/105Aliphatic or alicyclic compounds
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23KFODDER
    • A23K20/00Accessory food factors for animal feeding-stuffs
    • A23K20/20Inorganic substances, e.g. oligoelements
    • A23K20/22Compounds of alkali metals
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, 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
    • A23L3/00Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
    • A23L3/34Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals
    • A23L3/3409Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals in the form of gases, e.g. fumigation; Compositions or apparatus therefor
    • A23L3/3418Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals in the form of gases, e.g. fumigation; Compositions or apparatus therefor in a controlled atmosphere, e.g. partial vacuum, comprising only CO2, N2, O2 or H2O
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, 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
    • A23L3/00Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
    • A23L3/34Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals
    • A23L3/3454Preservation 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
    • A23L3/3463Organic compounds; Microorganisms; Enzymes
    • A23L3/3526Organic compounds containing nitrogen
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, 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
    • A23L3/00Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
    • A23L3/34Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals
    • A23L3/3454Preservation 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
    • A23L3/358Inorganic compounds
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23VINDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00Food compositions, function of food ingredients or processes for food or foodstuffs

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Polymers & Plastics (AREA)
  • Food Science & Technology (AREA)
  • Engineering & Computer Science (AREA)
  • Health & Medical Sciences (AREA)
  • Nutrition Science (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Animal Husbandry (AREA)
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  • Inorganic Chemistry (AREA)
  • Microbiology (AREA)
  • Medicinal Preparation (AREA)
  • Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)

Abstract

The invention belongs to the technical field of vitamin preparations in animal husbandry, and particularly relates to a composite vitamin nanoemulsion for livestock and a preparation method and application thereof. The composite vitamin nanoemulsion for livestock comprises the following components: vitamin A acetate, 25-hydroxy vitamin D3Vitamin D3Vitamin E, water-soluble vitamins, emulsifiers, co-emulsifiers, stabilizers and preservatives; pH6.0-7.0. The oil-in-water type composite vitamin nanometer for animals prepared by the inventionThe emulsion has the particle size of 20-30nm, can be completely dissolved with water, reduces the viscosity of the compound vitamin water solution, and effectively solves the problems of easy precipitation, low bioavailability and poor absorption after dissolution; by adding the emulsifier, the solubility of the fat-soluble vitamin is increased, and the bioavailability is improved; by adding a plurality of water-soluble vitamins, the production performance of the livestock and poultry is improved; the long-term stability of the vitamin is effectively improved by adding the stabilizer and filling nitrogen for treatment.

Description

Composite vitamin nanoemulsion for livestock and preparation method and application thereof
Technical Field
The invention relates to the technical field of vitamin preparations in animal husbandry, in particular to a composite vitamin nanoemulsion for livestock and a preparation method and application thereof.
Background
Vitamins have been used as nutritional supplements for animal organisms, and are well accepted and welcomed by livestock and poultry feeders. They are involved in various links of animal life activities, such as maintaining normal functions of nervous system, and participating in synthesis and metabolism of protein and fat, and have good promoting effects on improving immunity and rapid growth of livestock and fowl. With intensive and specialized feeding of livestock and poultry, the demand of vitamins is increasing day by day. Vitamin preparations in the current market mainly contain instant multivitamins, are difficult to be uniformly mixed when put in, and easily cause vitamin poisoning phenomena of insufficient vitamin supplement or excessive local vitamin; or the precipitate is easy to generate when dissolved, and the water drinking device is blocked.
At present, vitamin preparations also have a trend towards liquid preparations, but most of the market is conventional emulsion, and although the defects of premix and instant multivitamin can be overcome to some extent, the following problems still exist: the latex particles have larger particle size, are easy to block the nipple of the drinking fountain and create proper propagation conditions for pathogenic microorganisms; the product has poor stability, and the color of the visible light is easy to deepen and the turbidity phenomenon appears; the compatibility of the system is poor, and the system is difficult to be compounded with other beneficial components; the vitamins are single.
For example, chinese patent CN111838424A discloses a preparation method and application of a water-in-oil type liquid vitamin premix, which is a water-in-oil type liquid vitamin concentrate prepared by mixing A, B, C three groups of liquid vitamin ingredients and then spontaneously emulsifying. The premix avoids the reaction or degradation among vitamins through reasonable compatibility, and improves the stability of the vitamins; the water-in-oil type vitamin concentrated solution is formed through spontaneous emulsification, so that the energy consumption is reduced; the spraying process is completed after the oil is diluted, so that the high feed water content caused by the dilution with water in the oil-in-water type liquid vitamin spraying process is avoided, and the risk of feed mildew is reduced. However, when the premix is used in the actual clinical compound feed, the premix is found to consume a large amount of labor; in the aspect of drinking water, the water-in-oil type vitamins cannot be completely dissolved with water, and the bioavailability of the vitamins can be reduced.
For another example, chinese patent CN111149943A discloses a liquid vitamin for broiler chicken and its preparation method, wherein the liquid vitamin contains: 5-10 parts of thiamine hydrochloride, 10-20 parts of methionine, 10-20 parts of lysine, 5-20 parts of sorbitol, 65-15 parts of vitamin B, 0.5-1 part of tea polyphenol, 35-10 parts of vitamin D, 5-10 parts of vitamin E oil, 5-10 parts of vitamin A ester, 5-10 parts of vitamin C, 1-10 parts of emulsifier and 10-50 parts of organic solvent, and the preparation method is prepared by the working procedures of emulsification, heating, alcohol dissolving, water dissolving, cooling, filtration, subpackaging and the like. The liquid vitamin of the invention achieves nanometer liquid drops through an emulsification technology to enable an organism to quickly absorb the liquid vitamin, supplements vitamins required by the organism and reduces various stresses. But the preparation process needs heating, and the energy consumption is large; and the vitamins belong to heat-sensitive substances, the requirement on temperature control is high, and improper control easily causes high temperature, so that the vitamins are oxidized and deteriorated, and the titer of the vitamins is reduced.
Therefore, the development of the compound vitamin nano-emulsion which has good water solubility, high stability and bioavailability, small emulsion particle size and comprehensive vitamin types is necessary.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide the composite vitamin nanoemulsion for the livestock, which has the advantages of good water solubility, high stability, low production cost, simple preparation process, easy operation and contribution to large-scale production.
In order to solve the technical problems, the invention provides the following technical scheme:
in one aspect, the invention provides a composite vitamin nanoemulsion for livestock, which comprises the following components: vitamin A acetate, 25-hydroxy vitamin D3Vitamin D3Vitamin C and vitamin CRaw vitamin E, water-soluble vitamins, an emulsifier, a co-emulsifier, a stabilizer and a preservative; pH6.0-7.0.
Preferably, the water-soluble vitamins include, but are not limited to, vitamin B1Vitamin B2Vitamin B6Vitamin B12One or more of vitamin C, pantothenic acid, nicotinamide, folic acid and D-biotin.
More preferably, the water-soluble vitamin is vitamin B1Vitamin B2Vitamin B6Vitamin B12Nicotinamide and folic acid.
Preferably, the emulsifier includes, but is not limited to OP-10 or TX-10.
More preferably, the emulsifier is OP-10.
Preferably, the coemulsifier comprises one or a combination of more of propylene glycol, glycerol, polyethylene glycol 400 and N-methyl pyrrolidone.
More preferably, the co-emulsifier is propylene glycol.
Preferably, the stabilizer includes but is not limited to BHT, BHA, TBHQ, PG, sodium metabisulfite, EDTA-2Na or their combination.
More preferably, the stabilizer is BHT, BHA, sodium metabisulfite and EDTA-2 Na.
Preferably, the preservative includes but is not limited to one or a combination of potassium sorbate, sodium sorbate and sodium benzoate.
More preferably, the preservative is sodium benzoate.
Preferably, each 1L of the composite vitamin nanoemulsion for livestock consists of the following components: 5-10 parts of vitamin A acetate, 25-hydroxy vitamin D31-3 parts of vitamin D34-6 parts of vitamin E10-30 parts of ammonium sulfate hydrochloride, 1-3 parts of riboflavin, 20-40 parts of nicotinamide and vitamin B61-2 parts of folic acid, 0.13-0.2 part of vitamin B120.01-0.02 part of emulsifier, 100-400 parts of auxiliary emulsifier, 150-400 parts of auxiliary emulsifier, 0.4-5 parts of stabilizer and 3-5 parts of preservative; pH6.0-7.0; injection of drugsThe volume is adjusted to 1L by water.
In a specific embodiment, each 1L of the composite vitamin nanoemulsion for livestock consists of the following components: vitamin A acetate 8 parts, 25-hydroxy vitamin D32 parts of vitamin D34 parts of vitamin E10 parts, 2 parts of ammonium sulfate hydrochloride, 0.02 part of riboflavin, 20 parts of nicotinamide and vitamin B61 part, 0.2 part of folic acid and vitamin B120.012 part, OP-10100 part, 150 parts of propylene glycol, 0.1 part of BHT, 0.1 part of BHA, 0.3 part of EDTA-2Na, 4 parts of sodium metabisulfite and 4 parts of sodium benzoate; pH6.0-7.0; the volume of the water for injection is up to 1L.
On the other hand, the invention provides a preparation method of the composite vitamin nanoemulsion for livestock, which comprises the following steps:
s1, uniformly mixing an emulsifier and a co-emulsifier in proportion; then sequentially adding vitamin A acetate and 25-hydroxy vitamin D according to the proportion3Vitamin D3Mixing vitamin E and ultrasonic wave uniformly until forming a clear and uniform light yellow transparent liquid for later use;
s2, sequentially dissolving the water-soluble vitamins, the stabilizer and the preservative in the water for injection according to the proportion, and stirring until the water-soluble vitamins, the stabilizer and the preservative are completely dissolved for later use;
s3, slowly adding the solution prepared in the step S1 into the solution obtained in the step S2 while stirring, fixing the volume with water for injection, and adjusting the pH value to 6.0-7.0 to obtain a compound vitamin primary emulsion; homogenizing the vitamin complex primary emulsion, and performing nanometer granulation to obtain nanometer emulsion with nanometer emulsion particle size of 20-30 nm; filtering the mixture by a folding filter element microporous membrane filter with the aperture of 0.22 mu m, filling nitrogen, and finally subpackaging by adopting an aseptic packaging process to obtain the composite vitamin nanoemulsion for livestock.
On the other hand, the invention also provides the application of the composite vitamin nanoemulsion for livestock in improving the production performance of livestock.
Compared with the prior art, the invention has the following beneficial effects:
(1) the invention can ensure the solubility of fat-soluble vitamin by reasonably controlling the proportion of OP-10 and propylene glycol, and can reduce the dosage of emulsifier at the same time, replace the use of expensive Tween and span emulsifiers, and greatly reduce the cost.
(2) The invention further adopts antioxidant BHT, wherein the mass ratio of BHA is 1: 1, the stability of fat-soluble vitamins can be better improved; sodium metabisulfite is added to enhance the stability of the water-soluble vitamins; meanwhile, metal ion complexing agent EDTA-2Na is added, and nitrogen is filled, so that the conditions of oxidation, color change, unstable titer and the like in the storage process of the vitamin complex nanoemulsion are effectively prevented.
(3) The invention also adds imported raw material 25-hydroxy vitamin D325-hydroxy vitamin D3More common than vitamin D3Has more effective absorption and higher biological activity, and has stronger absorption of calcium, bone calcium regulation and phosphorus promotion. Direct 25-hydroxyvitamin D supplementation3Not only shorten common vitamin D3In the metabolic process of the organism, the burden of the liver is lightened, and the influence on the absorption and utilization in the case of liver and kidney dysfunction due to intestinal tract injury is avoided. Can effectively assist livestock and poultry to absorb calcium ions, is beneficial to the skeletal development of livestock and poultry, supplements calcium required by livestock and poultry, prevents osteoporosis and improves the laying rate of poultry animals; meanwhile, a plurality of water-soluble vitamins are added, so that the production performance of the livestock and poultry can be greatly improved.
(4) The composite vitamin nanoemulsion for livestock adopts a nano-emulsification technology, is simple in process operation, does not need any heating equipment in the emulsification process, simplifies the whole preparation process, and ensures the valence of the vitamin; the emulsion particle size of the prepared oil-in-water type compound vitamin nano-emulsion is 20-30nm, and simultaneously, the oil-in-water type compound vitamin nano-emulsion can be completely dissolved with water, so that the viscosity of a compound vitamin water solution is reduced; the high-speed centrifugation is not layered, has stable and uniform clear solution, and solves the problems of easy precipitation, low bioavailability and poor absorption after dissolution.
Detailed Description
The present invention will be further illustrated in detail with reference to the following specific examples, which are not intended to limit the present invention but are merely illustrative thereof. The experimental methods used in the following examples are not specifically described, and the materials, reagents and the like used in the following examples are generally commercially available under the usual conditions without specific descriptions.
The terms:
vitamin B1Also known as ammonium sulfate hydrochloride.
Vitamin B2The alias riboflavin.
Example 1
1. Prescription composition
A composite vitamin nanoemulsion for livestock, wherein each 1L of the composite vitamin nanoemulsion for livestock comprises the following components: vitamin A acetate 8.0g, 25-hydroxy vitamin D32.0g, vitamin D34.0g, vitamin E10.0 g, ammonium sulfate hydrochloride 2.0g, riboflavin 20mg, nicotinamide 20g, vitamin B61g, folic acid 200mg, vitamin B1212mg, OP-10100 mL, propylene glycol 150mL, BHT 0.1g, BHA 0.1g, EDTA-2Na 0.3g, sodium metabisulfite 4g, sodium benzoate 4.0 g; adjusting pH to 6.0-7.0, and diluting injection water to 1L.
Wherein, vitamin a acetate: 25-hydroxy vitamin D3: vitamin D3: vitamin E: emulsifier: the mass ratio of the auxiliary emulsifier is 0.08: 0.02: 0.04: 0.1: 1: 1.5.
2. preparation method
The preparation method of the composite vitamin nanoemulsion for livestock specifically comprises the following steps:
(1) adding OP-10 and propylene glycol into a stirring liquid preparation tank in sequence according to a certain proportion, stirring and mixing uniformly, and then adding vitamin A acetate and 25-hydroxy vitamin D3Vitamin D3Sequentially adding vitamin E into the liquid preparation tank, and uniformly mixing by ultrasonic wave until a clear and uniform light yellow transparent liquid is formed for later use;
(2) dissolving water-soluble vitamins, stabilizer and preservative in water for injection in sequence according to a certain proportion, and stirring until all the components are dissolved for later use;
(3) slowly adding the solution prepared in the step (1) into the solution prepared in the step (2) while stirring, finally fixing the volume with water for injection, and adjusting the pH value to 6.0-7.0 to obtain a compound vitamin primary emulsion; finally, carrying out homogenizing nanometer granulation treatment on the vitamin complex primary emulsion to obtain nanometer emulsion with the particle size of 20-30 nm; filtering with a folding filter element microporous membrane filter with the aperture of 0.22 mu m, filling nitrogen, and subpackaging by adopting an aseptic packaging process to obtain the veterinary compound vitamin nanoemulsion.
Example 2
1. Prescription composition
A composite vitamin nanoemulsion for livestock, wherein each 1L of the composite vitamin nanoemulsion for livestock comprises the following components: vitamin A acetate 5.0g, 25-hydroxy vitamin D32.0g, vitamin D35.0g, vitamin E20.0 g, ammonium sulfate hydrochloride 2.0g, riboflavin 20mg, nicotinamide 20g, vitamin B61g, folic acid 200mg, vitamin B1212mg, OP-10130 mL, propylene glycol 150mL, BHT 0.1g, BHA 0.1g, EDTA-2Na 0.4g, sodium metabisulfite 4g, sodium benzoate 4.0 g; adjusting pH to 6.0-7.0, and diluting injection water to 1L.
Wherein, vitamin a acetate: 25-hydroxy vitamin D3: vitamin D3: vitamin E: emulsifier: the mass ratio of the auxiliary emulsifier is 0.05: 0.02: 0.05: 0.2: 1.3: 1.5.
2. preparation method
The specific steps of the preparation method of the composite vitamin nanoemulsion for livestock of the embodiment are the same as those of the embodiment 1.
Example 3
1. Prescription composition
A composite vitamin nanoemulsion for livestock, wherein each 1L of the composite vitamin nanoemulsion for livestock comprises the following components: vitamin A acetate 10.0g, 25-hydroxy vitamin D32.0g, vitamin D36.0g, 25.0g of vitamin E, 2.0g of ammonium sulfate hydrochloride, 20mg of riboflavin, 20g of nicotinamide and vitamin B61g, folic acid 200mg, vitamin B1212mg, OP-10300 mL, 100mL of propylene glycol, 0.1g of BHT, 0.1g of BHA, 0.4g of EDTA-2Na, 5g of sodium metabisulfite and 4.0g of sodium benzoate; adjusting pH to 6.0-7.0, and diluting injection water to 1L.
Wherein, vitamin a acetate: 25-hydroxy vitamin D3: vitamin D3: vitamin E: emulsifier: the mass ratio of the auxiliary emulsifier is 0.1: 0.02: 0.06: 0.25: 3: 1.
2. preparation method
The specific steps of the preparation method of the composite vitamin nanoemulsion for livestock of the embodiment are the same as those of the embodiment 1.
Comparative example 1
The difference from example 1 is that: adding 1.0g of 25-hydroxy vitamin D3The other components and contents were the same as in example 1.
Wherein, vitamin a acetate: 25-hydroxy vitamin D3: vitamin D3: vitamin E: emulsifier: the mass ratio of the auxiliary emulsifier is 0.08: 0.01: 0.04: 0.1: 1: 1.5.
the other operations and steps are the same as in example 1.
Comparative example 2
The difference from example 1 is that: without the addition of 25-hydroxy vitamin D3The other components and contents were the same as in example 1.
The other operations and steps are the same as in example 1.
Comparative example 3
The difference from example 1 is that: EDTA-2Na and sodium metabisulfite are not added, and only the weight ratio of 1: BHT and BHA of 1 as stabilizers, the remaining components and contents were the same as in example 1.
The other operations and steps are the same as in example 1.
Comparative example 4
The difference from example 1 is that: the pH of the solution was adjusted to 4.0-5.0, and the remaining components and contents were the same as in example 1.
The other operations and steps are the same as in example 1.
Comparative example 5
The difference from example 1 is that: the pH of the solution was adjusted to 7.0-8.0, and the remaining components and contents were the same as in example 1.
The other operations and steps are the same as in example 1.
Effect test
Test example 1 emulsification Effect test
1. Particle diameter distribution
The complex vitamin nano-emulsions for animals of examples 1 to 3 and comparative examples 1 to 5 were diluted 100 times with distilled water, and the particle size distribution thereof was measured with a laser particle size analyzer.
2. Type of nanoemulsion
Whether the vitamin complex nanoemulsion is an oil-in-water (O/W) type or a water-in-oil (W/O) type is judged by a dyeing method, and the judgment is carried out according to the diffusion speed of red oil-soluble dye Sudan red and blue water-soluble dye methylene blue in the nanoemulsion. If the red oil-soluble dye Sudan red rapidly diffuses, the vitamin complex nanoemulsion is of a water-in-oil (W/O) type; if the blue water-soluble dye rapidly diffuses methylene blue, the vitamin complex nanoemulsion is of an oil-in-water (O/W) type.
As shown in Table 1, the complex vitamin nano-emulsions for animals of examples 1 to 3 and comparative examples 1 to 5 were all oil-in-water (O/W) type, and had particle diameters of 20 to 30 nm.
TABLE 1 dyeing results
Figure BDA0003009304230000061
Figure BDA0003009304230000071
Test example 2 stability test
1. Long term stability test
The test aims at the content of the vitamin A acetate in the nano milk as a research target because the vitamin A acetate in the three fat-soluble vitamins has the worst stability, is easy to decompose under the light and is easy to oxidize and is a main influence factor.
The detection method comprises the following steps: according to the test of the stability investigation test method in 2015 of the pharmacopoeia of the people's republic of China, the samples prepared in examples 1-3 and comparative examples 1-5 are tested under the conditions of the temperature of 25 +/-2 ℃ and the humidity of 60% +/-5%, and the content of the vitamin A acetate in the composite vitamin nanoemulsion of each test group is detected by a high performance liquid chromatograph under the liquid phase detection conditions that: mobile phase: methanol: water (98: 2); flow rate: 0.2 ml/min; detection wavelength: 326 nm.
The results are shown in Table 2 below.
TABLE 2 test results
Figure BDA0003009304230000072
According to the detection data in the table 2, the stability of the vitamin A acetate content of the vitamin A complex nanoemulsion prepared in the embodiments 1-3 and the comparative examples 1-2 is higher, and the vitamin A acetate content is still more than 97% after the vitamin A complex nanoemulsion is placed for 6 months, which shows that the stability of the prepared vitamin A complex nanoemulsion is better by controlling the type and the mass ratio of the stabilizer and adjusting the pH value of the solution to 6.0-7.0; and when the types of the stabilizing agents are changed and the pH of the solution is not changed within the protection range of the invention in the comparative examples 3-5, the stability of the obtained vitamin complex nanoemulsion is obviously reduced, so that the vitamin complex nanoemulsion prepared by using the formula disclosed by the invention has better stability.
2. High temperature stability test
The test aims at the content of the vitamin A acetate in the nano milk as a research target because the vitamin A acetate in the three fat-soluble vitamins has the worst stability, is easy to decompose under the light and is easy to oxidize and is a main influence factor.
The detection method comprises the following steps: according to the test of the stability investigation test method in 2015 of the pharmacopoeia of the people's republic of China, the samples prepared in examples 1-3 and comparative examples 1-5 are tested under the conditions of 40 +/-2 ℃ and 75% +/-10% humidity respectively, and the content of the vitamin A acetate in the composite vitamin nanoemulsion of each test group is detected by a high performance liquid chromatograph under the liquid phase detection conditions that: mobile phase: methanol: water (98: 2); flow rate: 0.2 ml/min; detection wavelength: 326 nm.
The results are given in Table 3 below.
TABLE 3 test results
Figure BDA0003009304230000081
According to the detection data in the table 3, the stability of the vitamin A acetate content of the vitamin A complex nanoemulsion prepared in the embodiments 1-3 and the comparative examples 1-2 is higher, and the vitamin A acetate content is still over 75% after the vitamin A complex nanoemulsion is placed for 6 months, which shows that the stability of the prepared vitamin A complex nanoemulsion is better by controlling the type and the mass ratio of the stabilizer and adjusting the pH value of the solution to 6.0-7.0; and when the types of the stabilizers are changed and the pH of the solution is not changed within the protection range of the invention in the comparative examples 3-5, the stability of the obtained vitamin complex nanoemulsion is obviously reduced, and the conclusion of the compound vitamin complex nanoemulsion is consistent with that of a long-term stability test, namely, a clinical effect test of the laying hen in test example 3
1. Test materials
(1) Blank control group: and (4) distilled water.
(2) Drug control group: commercially available vitamin nanoemulsion, example 1, comparative example 2.
2. Test method
1600 feathers of healthy 250-day-old Roman powder laying hens with similar body weight and production performance are selected and randomly divided into 4 groups of 400 laying hens. The blank group of normal drinking water is not added with any additive component, and the water is continuously and freely drunk for 30 days; the commercial nanoemulsion, example 1, comparative example 1 and comparative example 2 were 1mL of water or 1g of water, 1L of water, and water was continuously and freely drunk for 30 days. The laying rate, the egg breaking rate and the feed-egg ratio of each group of experiments are recorded every day after one month of the experiments, and the specific data are shown in the following table 4.
TABLE 4 egg production, egg breakage and feed-egg ratio before and after use of different groups
Figure BDA0003009304230000091
As can be seen from the data in Table 4 above, the vitamin complex nanoparticles prepared in example 1 of the present invention were added to drinking waterAfter the milk is fed, the laying rate is improved by 6.27 percent, and the egg breaking rate and the feed-egg ratio are reduced by 0.47 percent and 0.33 percent; compared with the commercial nanoemulsion group, the laying rate of the group 1 is higher by 2.63%, and the egg breaking rate and the feed-egg ratio are reduced by 0.14% and 0.17%; compared with the commercially available nanoemulsion group, the nano-emulsion group of the invention in the embodiment 1 can effectively improve the laying rate, reduce the egg breakage rate and the feed-egg ratio, has high bioavailability and can improve the economic benefit. Compared with comparative example 1 and comparative example 2, the laying rate of the composition of example 1 is respectively 1.09% and 2.01%, the egg breaking rate and the feed-egg ratio are respectively reduced by 0.02%, 0.08%, 0.04 and 0.14, which shows that 25-hydroxy vitamin D is added3Can better improve the production performance of the laying fowl to a certain extent.
Test example 4 clinical effect test of broiler chicken
1. Test materials
(1) Blank control group: and (4) distilled water.
(2) Drug control group: commercial nanoemulsion, example 1 and comparative examples 1 and 2.
2. Test method
1000 healthy 22-day-old broilers with similar body weight are selected and randomly divided into 4 groups of 250 broilers. Feeding the blank group normally without adding any additive component, and freely drinking water; the commercial nano-emulsion, the example 1, the comparative example 1 and the comparative example 2 are free drinking water with 1L of water as 1mL or 1 g; the water was allowed to drink freely for 20 days. The 42 days old are shown in the column, and the data of each test group is recorded as shown in the following table 5.
TABLE 5 daily gain, feed conversion ratio and slaughter weight before and after use of different groups
Figure BDA0003009304230000101
According to the detection data in the table 5, after the composite vitamin nanoemulsion prepared in the embodiment 1 of the invention is added into drinking water, compared with a blank group, the daily gain of the broiler chicken is increased by 1.67g, the feed-meat ratio is reduced by 0.29, and the slaughter weight is increased by 52 g; compared with the market nanoemulsion group, the daily gain of the broiler chickens is increased by 1.38g, the feed-meat ratio is reduced by 0.27, and the slaughter weight is increased by 16 g; illustrating embodiments of the inventionThe 1 composite vitamin nano-emulsion can obviously improve the production performance of the broiler chicken, reduce the feed-meat ratio and improve the breeding benefit. Compared with comparative example 1 and comparative example 2, the daily gain of the broiler chickens is respectively improved by 0.45g and 0.88g, the feed-meat ratio is respectively reduced by 0.18 and 0.2, and the slaughter weight is respectively increased by 9g and 11g, which shows that 25-hydroxy vitamin D is added3And then, the production performance of the broiler chicken is improved to a certain extent.
Finally, it should be noted that the above-mentioned contents are only used for illustrating the technical solutions of the present invention, and not for limiting the protection scope of the present invention, and that the simple modifications or equivalent substitutions of the technical solutions of the present invention by those of ordinary skill in the art can be made without departing from the spirit and scope of the technical solutions of the present invention.

Claims (10)

1. The composite vitamin nanoemulsion for livestock is characterized by comprising the following components: vitamin A acetate, 25-hydroxy vitamin D3Vitamin D3Vitamin E, water-soluble vitamins, emulsifiers, co-emulsifiers, stabilizers and preservatives; pH6.0-7.0.
2. The composite vitamin nanoemulsion for veterinary use as claimed in claim 1, wherein the water-soluble vitamin is vitamin B1Vitamin B2Vitamin B6Vitamin B12One or more of vitamin C, pantothenic acid, nicotinamide, folic acid and D-biotin.
3. The complex vitamin nanoemulsion of claim 1, wherein the emulsifier is OP-10 or TX-10.
4. The composite vitamin nanoemulsion for veterinary use as claimed in claim 1, wherein the co-emulsifier is one or more of propylene glycol, glycerol, polyethylene glycol 400 and N-methylpyrrolidone.
5. The composite vitamin nanoemulsion for veterinary use as claimed in claim 1, wherein the stabilizer is one or more of BHT, BHA, TBHQ, PG, sodium metabisulfite and EDTA-2 Na.
6. The composite vitamin nanoemulsion for veterinary use as claimed in claim 1, wherein the preservative is one or more of potassium sorbate, sodium sorbate and sodium benzoate.
7. The complex vitamin nanoemulsion for veterinary use according to any one of claims 1 to 6, wherein each 1L of the complex vitamin nanoemulsion for veterinary use consists of the following components: 5-10 parts of vitamin A acetate, 25-hydroxy vitamin D31-3 parts of vitamin D34-6 parts of vitamin E, 10-30 parts of vitamin E, 1-3 parts of ammonium sulfate hydrochloride, 0.02-1 part of riboflavin, 20-40 parts of nicotinamide and vitamin B61-2 parts of folic acid, 0.13-0.2 part of vitamin B120.01-0.02 part of emulsifier, 100-400 parts of auxiliary emulsifier, 150-400 parts of auxiliary emulsifier, 0.4-5 parts of stabilizer and 3-5 parts of preservative; pH6.0-7.0; the volume of the water for injection is up to 1L.
8. The vitamin complex nanoemulsion for veterinary use according to claim 7, wherein each 1L of the vitamin complex nanoemulsion for veterinary use consists of the following components: vitamin A acetate 8 parts, 25-hydroxy vitamin D32 parts of vitamin D34 parts of vitamin E, 10 parts of vitamin E, 2 parts of ammonium sulfate hydrochloride, 0.02 part of riboflavin, 20 parts of nicotinamide and vitamin B61 part, 0.2 part of folic acid and vitamin B120.012 part, OP-10100 part, 150 parts of propylene glycol, 0.1 part of BHT, 0.1 part of BHA, 0.3 part of EDTA-2Na, 4 parts of sodium metabisulfite and 4 parts of sodium benzoate; pH6.0-7.0; the volume of the water for injection is up to 1L.
9. The method for preparing the composite vitamin nanoemulsion for livestock of any one of claims 1 to 6, characterized in that the preparation method comprises the following steps:
s1, uniformly mixing an emulsifier and a co-emulsifier in proportion; then are sequentially mixed according to the proportionAdding vitamin A acetate and 25-hydroxy vitamin D3Vitamin D3Mixing vitamin E and ultrasonic wave uniformly until forming a clear and uniform light yellow transparent liquid for later use;
s2, sequentially dissolving the water-soluble vitamins, the stabilizer and the preservative in the water for injection according to the proportion, and stirring until the water-soluble vitamins, the stabilizer and the preservative are completely dissolved for later use;
s3, slowly adding the solution prepared in the step S1 into the solution obtained in the step S2 while stirring, fixing the volume with water for injection, and adjusting the pH value to 6.0-7.0 to obtain a compound vitamin primary emulsion; homogenizing the vitamin complex primary emulsion, and performing nanometer granulation to obtain nanometer emulsion with nanometer emulsion particle size of 20-30 nm; filtering the mixture by a folding filter element microporous membrane filter with the aperture of 0.22 mu m, filling nitrogen, and finally subpackaging by adopting an aseptic packaging process to obtain the composite vitamin nanoemulsion for livestock.
10. Use of the multi-vitamin nanoemulsion for veterinary use according to any one of claims 1 to 6 for improving the production performance of livestock.
CN202110375014.1A 2021-04-07 2021-04-07 Composite vitamin nanoemulsion for livestock and preparation method and application thereof Pending CN113040277A (en)

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