CN108210569A - A kind of tea tree oil microcapsule and its granule - Google Patents

A kind of tea tree oil microcapsule and its granule Download PDF

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Publication number
CN108210569A
CN108210569A CN201810272986.6A CN201810272986A CN108210569A CN 108210569 A CN108210569 A CN 108210569A CN 201810272986 A CN201810272986 A CN 201810272986A CN 108210569 A CN108210569 A CN 108210569A
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tea
oil
tea tree
tree oil
oil microcapsule
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CN201810272986.6A
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CN108210569B (en
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徐建中
王红霞
贾新超
高伟
段志鹏
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Chenguang Biotech Group Co Ltd
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Chenguang Biotech Group Co Ltd
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/61Myrtaceae (Myrtle family), e.g. teatree or eucalyptus
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23KFODDER
    • A23K10/00Animal feeding-stuffs
    • A23K10/30Animal feeding-stuffs from material of plant origin, e.g. roots, seeds or hay; from material of fungal origin, e.g. mushrooms
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23KFODDER
    • A23K40/00Shaping or working-up of animal feeding-stuffs
    • A23K40/30Shaping or working-up of animal feeding-stuffs by encapsulating; by coating
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00Medicinal preparations characterised by special physical form
    • A61K9/48Preparations in capsules, e.g. of gelatin, of chocolate
    • A61K9/50Microcapsules having a gas, liquid or semi-solid filling; Solid microparticles or pellets surrounded by a distinct coating layer, e.g. coated microspheres, coated drug crystals
    • A61K9/5005Wall or coating material
    • A61K9/5015Organic compounds, e.g. fats, sugars
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00Medicinal preparations characterised by special physical form
    • A61K9/48Preparations in capsules, e.g. of gelatin, of chocolate
    • A61K9/50Microcapsules having a gas, liquid or semi-solid filling; Solid microparticles or pellets surrounded by a distinct coating layer, e.g. coated microspheres, coated drug crystals
    • A61K9/5005Wall or coating material
    • A61K9/5021Organic macromolecular compounds
    • A61K9/5036Polysaccharides, e.g. gums, alginate; Cyclodextrin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00Medicinal preparations characterised by special physical form
    • A61K9/48Preparations in capsules, e.g. of gelatin, of chocolate
    • A61K9/50Microcapsules having a gas, liquid or semi-solid filling; Solid microparticles or pellets surrounded by a distinct coating layer, e.g. coated microspheres, coated drug crystals
    • A61K9/5073Microcapsules having a gas, liquid or semi-solid filling; Solid microparticles or pellets surrounded by a distinct coating layer, e.g. coated microspheres, coated drug crystals having two or more different coatings optionally including drug-containing subcoatings

Abstract

The invention discloses a kind of tea tree oil microcapsule and its granules, belong to chemicals field, tea oil phosphatide complexes are emulsified with aqueous emulsion, homogeneous obtains tea tree oil microcapsule.The present invention can improve the stability of tea oil and embedding rate, improvement taste masking effect, have the advantages that simple for process, production cost is low, pollution is small, be suitble to industrialized production, can completely or partially substitute the antibiotic usage in feed or veterinary drug.

Description

A kind of tea tree oil microcapsule and its granule
Technical field
The present invention relates to microcapsules or microballoon or granule, especially a kind of microcapsules and its particle containing plants essential oil Agent belongs to chemicals field.
Background technology
The harm that antibiotic is brought increasingly is recognized now by whole world people, and this tradition of addition antibiotic solves dynamic The method of object disease can generate a series of safety problem and potential risk:As microbial population of animal intestinal tract is unbalance, medicament residue and anti- The various aspects negative effect such as pharmacological property threatens the quality safety of animal foods.
European Union just completely forbade in feed early in 2006 and adds antibiotic.With the food-safe attention of country, resist Raw element is increasingly restricted in husbandry sector, and the Ministry of Agriculture's the 6th standing meeting in 2015 is approved《National veterinary drug 5 years action schemes of (antimicrobial) comprehensive treatment》, governing project is proposed to abuse of antibiotics present situation;On September 1st, 2015, agricultural Portion issues first " prohibiting anti-enable ", forbid Lomefloxacin, Pefloxacin, Ofloxacin, 4 kinds of bulk pharmaceutical chemicals of Norfloxacin it is various Salt, ester and its various preparations use in food animal;Version in 2015《Chinese veterinary pharmacopoeia》The antibiotic that will have clearly disabled There are Arsanilic Acid, roxarsone, colistine sulfate, Bacitracin Zinc and colistine sulfate pre-mixing agent, olaquindox, and propose two The antibiotic such as disabling kitasamycin, virginiamycin are discussed after year.Chinese feed antibiotic-free is following inevitable development Direction.
Tea oil has the antimicrobial acivity of wide spectrum, is carried from the wood Myrtaceae Cajeputtree Leaf of port in a manner of distillation The Pure natural plant essential oil taken originates in Australia state, has the effect of characteristic perfume and antibacterial, anti-inflammatory, expelling parasite, mite killing, and with no dirt The characteristics of contaminating, be non-corrosive, permeability is strong.
Tea oil has very strong antiviral, antibacterium and inflammation-diminishing function, golden yellow to 10 kinds of contaminated bacterias common in fowl, poultry Color staphylococcus, bacillus subtilis, Escherichia coli, proteus, aspergillus niger, aspergillus flavus, saccharomyces cerevisiae, thermophilic lactic hammer The fungistatic effects such as bacterium, lactobacillus bulgaricus, abnormal Hansenula anomala are good, and alimentary canal and respiratory tract to animal can play guarantor Strong and therapeutic effect, can effectively replace are widely used in the antibiotics drug of aquaculture, and related drugs can also be coordinated to use work For therapeutic agent, the effect of enhancing drug effect is played.Tea oil uses the approval for obtaining U.S. FDA already, FEMA as food flavor Number for 3902, allow the forage plant extract used for the Ministry of Agriculture.It acts on livestock and poultry nonhazardous, without residual in animal products It stays, non-hazardous to human health, farm animal excrement is environmentally safe, is a kind of safe efficient, green natural plants essential oil Feed addictive.Since tea oil has unique fragrant strongly fragrant smell, it is directly appended to smell in feed and is difficult to cover, easily influence dynamic The appetite of object, and tea tree oil product is volatile, there are quality it is unstable the problems such as.
The current existing relevant report that tea oil is made to microcapsules, can improve the stability of tea oil can simultaneously cover because The special odor for volatilizing and generating, the preparation method for the tea tree oil microcapsule that patent document CN201310047112.8 is recorded are: Stabilizer and carboxymethyl chitosan are mixed into obtain solution I, emulsifier and tea oil add in and solution II obtained in chitosan aqueous solution, molten Liquid II is added in solution I, reacts to obtain multiple lime set, then curing agent is added to react to obtain tea oil microcapsule emulsion, centrifugation, washing precipitation, Tea tree oil microcapsule is obtained after freeze-drying.This method embedding rate is low, and processing step is complicated, is especially freeze-dried process, can not Realize large-scale industrial production.A kind of chitosan 6-OH bearing cyclodextrins that patent document CN201310685212.3 is recorded spread out Biology inclusion tea oil preparation method be:Chitosan 6-OH bearing cyclodextrin derivatives are dissolved in organic solvent, and molten A certain amount of polyvinylpyrrolidone is solved, stirring inclusion certain time after the two is mixed adds in precipitating reagent precipitation, and with having Solvent is washed, and obtains chitosan 6-OH bearing cyclodextrin derivatives inclusion tea tree oily product.But this method embedding rate is low, taste masking Effect is poor, and has used a variety of organic solvents in the process, and there are security risks.
Invention content
The technical problem to be solved in the invention is to provide a kind of tea tree oil microcapsule and its granule, can improve tea tree The stability and embedding rate of oil improve taste masking effect, have that simple for process, production cost is low, pollution is small, suitable industrialized production The advantages of, it can completely or partially substitute the antibiotic usage in feed or veterinary drug.
In order to solve the above technical problems, the technical solution adopted in the present invention is:
A kind of tea tree oil microcapsule is emulsified tea oil phosphatide complexes with aqueous emulsion, that homogeneous obtains tea oil is micro- Capsule.
Technical solution of the present invention further improvement lies in that:Tea oil phosphatide complexes are molten by tea oil, phosphatide and oil Property antioxidant is made;Aqueous emulsion is that disaccharide and wall material are dissolved in successively in 50~60 DEG C of water to be made.
Technical solution of the present invention further improvement lies in that:The preparation method of tea oil phosphatide complexes is by phosphatide, oil Soluble antioxidant and tea oil are added sequentially in non-polar organic solvent, are heated to 40~50 DEG C, stir vacuum after 2~3h It is dry.
Technical solution of the present invention further improvement lies in that:Non-polar organic solvent is n-hexane, petroleum ether, ether, three Any one of chloromethanes, the tea tree oil quality added in every milliliter of non-polar organic solvent are 0.5~2g, the HLB value of phosphatide It is 10~12.
Technical solution of the present invention further improvement lies in that:Oil-soluble inhibitor is tea polyphenols or vitamin E;Disaccharide is Any one of sucrose, lactose, maltose;Wall material is any one of Arabic gum, guar gum.
Technical solution of the present invention further improvement lies in that:The parts by weight of each ingredient are tea oil in tea tree oil microcapsule 1 part, phosphatidase 0 .5~1 part, 0.05~0.2 part of oil-soluble inhibitor, 4~5 parts of disaccharide, 3.5~4 parts of wall material, the weight of water is Tea oil, phosphatide, disaccharide, 1~1.5 times of total weight of wall material and oil-soluble inhibitor.
Technical solution of the present invention further improvement lies in that:It emulsifies as the high shear under the rotating speed of 8000~10000r/min Emulsification, the time of emulsification is 30~60min;Homogeneous is homogeneous 2~3 times under 20~60MPa high pressures.
Granule prepared by a kind of tea tree oil microcapsule, will obtain tea tree oil microcapsule after tea tree oil microcapsule mist projection granulating Granule enters embedding medium during mist projection granulating using spray granulator top spray, while it is 10~50 DEG C to control spraying inlet air temperature, is made After grain remaining starchiness is screened out with 60~200 mesh.
Technical solution of the present invention further improvement lies in that:The frequency of nozzle is 40~50hHz during mist projection granulating, and rotating speed is 2000~3000r/min;The embedding medium is any one of maltodextrin, cyclodextrin, cornstarch or several mixing;Tea It is 2~20 μm to set the tea oil Microcapsules Size in oil microcapsule granule.
By adopting the above-described technical solution, the technological progress that the present invention obtains is:
A kind of tea tree oil microcapsule and its granule provided by the invention can improve stability and the embedding of tea oil Rate improves taste masking effect, has the advantages that simple for process, production cost is low, pollution is small, suitable industrialized production, can all or Antibiotic usage in partial alternative feed or veterinary drug.
The tea tree oil microcapsule of the present invention is first prepared tea oil phosphatide complexes, can be increased using two layers of embedding techniques The stability of tea oil improves its bioavilability, then wraps up tea oil phosphatide complexes with wall material, makes it have good water Dissolubility obtains the tea tree oil microcapsule of two layers of embedding, and tea oil microcapsule granule is then on the basis of more than tea tree oil microcapsule On, third layer embedding is carried out with embedding medium mist projection granulating, obtained tea oil microcapsule granule stability is strong, is not easy to reveal, Embedding rate reaches more than 99%.Tea oil eliminates the overpowering odor of tea oil, efficiently masks it significantly after three layers of embedding Bad smell can also improve the appetite of animal.Microencapsulation simultaneously can effectively weaken the volatilization of tea oil, and active ingredient has obtained very Good protection since microcapsules have sustained release performance, can extend the action time of tea oil active ingredient, add suitable for feed Add agent or for animal pharmaceuticals preparation.
The raw material that the present invention selects is tea oil, phosphatide, disaccharide, wall material, oil-soluble inhibitor.Tea oil has suppression The effect of bacterium, anti-inflammatory, expelling parasite, mite killing, and have the characteristics that pollution-free, non-corrosive, permeability is strong, it is adapted as feed and adds Add agent or for animal pharmaceuticals preparation.Using oil-soluble inhibitor and phosphatide, the oxidation of tea oil can be prevented, increases tea tree When the HLB value of phosphatide is 10~12, the bioavilability and stability of tea oil can be greatly improved in the stability of oil.Using Disaccharide and wall material can embed tea oil well, reduce the volatilization of tea oil, simultaneously effective mask the smell of tea oil.
Embedding medium preferably uses any one of maltodextrin, cyclodextrin, cornstarch or several during mist projection granulating of the present invention The mixing of kind.Maltodextrin, cyclodextrin, cornstarch are respectively provided with preferable viscosity, can be micro- by tea oil in mist projection granulating Capsule is well bonded to forms the particle that grain size is suitble to together.Maltodextrin can absorb the bad smell of tea oil simultaneously, Improve mouthfeel.Maltodextrin hygroscopicity itself is low, not easy to knot groups, can effectively facilitate formed product, and filming performance is good, can prevent tea Oil microcapsule particle deformation is set, ensures granule shape stable homogeneous, good water solubility is easily absorbed by the body, manufactured When granula is as feed addictive or animal formulation, can preferably it play a role.Cyclodextrin can improve the stability of tea oil, It can also be used to cover the bad smell of tea oil, have the function that make tea oil slow release when in use, extend tea oil Action time in animal body reduces and number is added in feed as feed addictive or is directly taken as animal formulation With number, medication efficiency is improved.Cornstarch has the characteristics that low viscosity during high concentration.When cornstarch and cyclodextrin cooperation make Used time, the particularly ratio of the two are 2:When 1, the viscosity of embedding medium can be improved, masks the bad smell of tea oil, and energy Raising system solid concentration reduces energy consumption, reduces production cost.
Embedding medium is entered using spray granulator top spray during mist projection granulating of the present invention, at the same control spraying inlet air temperature for 10~ 50 DEG C, the lotion after phosphatide complexes and aqueous emulsion double-layer embedment and maltodextrin, cyclodextrin or cornstarch can be made It is uniformly bonded together, rate of drying is fast, and the time is short, and temperature of charge is low, and tea oil is not easy oxygenolysis.Temperature is excessively high, then tea Tree oil is easily aoxidized;Temperature is too low, then lotion can not well be bonded with embedding medium, can not be granulated.After granulation with 60~ 200 mesh screen out remaining maltodextrin, cyclodextrin or cornstarch, ensure the grain size of tea oil micro-capsule granules to be formed Uniformly, without starchiness.
In the present invention parts by weight of each raw material be 1 part of tea oil, phosphatidase 0 .5~1 part, oil-soluble inhibitor 0.05~ 0.2 part, 4~5 parts of disaccharide, 3.5~4 parts of wall material, the weight of water is tea oil, phosphatide, disaccharide, wall material and oil-soluble inhibitor 1~1.5 times of total weight.Under matching herein, the phosphatide complexes emulsibility that tea oil is formed improves, with disaccharide, wall material shape Into aqueous emulsion conjugation it is high, while protect tea oil not oxidized, the lotion of formation easily embeds, embedding rate up to more than 99%, The tea tree oil microcapsule stay in grade of preparation efficiently masks the bad smell of tea oil, applied to animal feed additive The appetite of animal is greatly improved, the slow release of tea oil can be increased applied to animal formulation, extends tea oil active ingredient Action time makes drug effect preferably play a role.
The wall material that the present invention selects is Arabic gum or guar gum, and Arabic gum has good encystation performance, can have Effect cladding tea oil phosphatide complexes, do not react with tea oil phosphatide complexes, Arabic gum while or good shield Wafer can keep the smell of the substance in micro-capsule, prevent the bad smell of tea oil from evaporating and influencing the appetite of animal, When the quality of Arabic gum is 3.5~4 times of tea tree oil quality, taste masking effect is best.Guar gum is equal in hot water or cold water With good dispersibility, will not conglomeration, have good compatibility with anion, amphoteric ion and surfactant.Ah Draw primary glue and guar gum source sufficient, it is cheap, when it is used cooperatively with sucrose, lactose or maltose, can reduce Oil/water interfacial tension increases storage-stable.
It is tea polyphenols or vitamin E that the present invention, which selects oil-soluble inhibitor, has stronger oxidation resistance, while tea Polyphenol or vitamin E sheet can be dissolved in tea oil well as oil-soluble, oxidation resistant so as to play the role of, each The tea polyphenols or vitamin E of 0.05~0.2 part of addition in part tea oil, it will be able to protect tea oil in the process for preparing microcapsules In it is not oxidized, tea polyphenols or vitamin E are all the active ingredient extracted from natural plant extracts, safe and healthy.
In the rotating speed of 8000~10000r/min when the present invention is emulsified by controlling tea oil phosphatide complexes with aqueous emulsion Lower high shear, and homogeneous 2~3 times under 20~60MPa high pressures, at the same when controlling mist projection granulating nozzle frequency 40~ 50Hz, rotating speed is in 2000~3000r/min, in addition the rationally grain size of control raw material, ensure that the grain sizes of each microcapsules 2~ 20 μm, there is good dispersibility and dissolubility, embedding rate to be up to 99%, disclosure satisfy that as feed addictive and for animal The requirement of medicament.
Tea tree oil microcapsule and its granule prepared by the present invention can all or part of substitute antibiotics use, applied to feeding During material, animal immunizing power can be effectively improved, there is disease-resistant, heat resistanceheat resistant, resisting stress, can effectively improve animal survival rate and Output capacity promotes growth;It is used to prevent applied to animal pharmaceuticals preparation or treats digestive system, respiratory disease.
Specific embodiment
Here is certain specific embodiments of the invention, to be described in further detail.
A kind of tea tree oil microcapsule and its granule are emulsified tea oil phosphatide complexes with aqueous emulsion, homogeneous obtains To tea tree oil microcapsule.Tea oil microcapsule granule will be obtained after tea tree oil microcapsule mist projection granulating.Tea oil phosphatide is compound Object is made by tea oil, phosphatide and oil-soluble inhibitor;Aqueous emulsion be disaccharide and wall material are dissolved in the water successively it is obtained. The parts by weight of raw material be 1 part of tea oil, phosphatidase 0 .5~1 part, 0.05~0.2 part of oil-soluble inhibitor, 4~5 parts of disaccharide, 3.5~4 parts of wall material, the weight of water are the 1~1.5 of the total weight of tea oil, phosphatide, disaccharide, wall material and oil-soluble inhibitor Times.
Preparation method includes the following steps:
A. it is organic molten phosphatide, oil-soluble inhibitor and tea oil that HLB value is 10~12 to be added sequentially to nonpolarity In agent, the tea tree oil quality added in every milliliter of non-polar organic solvent is 0.5~2g, is heated to 40~50 DEG C, stirs 2~3h After be dried in vacuo, tea oil phosphatide complexes are made;Oil-soluble inhibitor is preferably tea polyphenols or vitamin E, and nonpolarity has Solvent is preferably any one of n-hexane, petroleum ether, ether, chloroform.
B. disaccharide and wall material are added sequentially to dissolve in 50~60 DEG C of water, aqueous emulsion are made, in 8000~10000r/ High-shear emulsifying under the rotating speed of min, adds tea oil phosphatide complexes, continues high-shear emulsifying 30~60min, 20~ Double-layer embedment lotion (tea tree oil microcapsule) is made in homogeneous 2~3 times under 60MPa high pressures;Disaccharide be preferably sucrose, lactose or One kind in maltose, wall material are preferably one kind in Arabic gum or guar gum.
C. double-layer embedment lotion (tea tree oil microcapsule) is added in spray granulator, spraying inlet air temperature is 10~50 DEG C, while top spray embedding medium carries out a step granulation, and the frequency of best nozzle is 40~50Hz during mist projection granulating, rotating speed for 2000~ 3000r/min, it is 2~20 μm that can control the Microcapsules Size inside embedding medium, and embedding medium is preferably maltodextrin, ring paste Any one of essence, cornstarch or several mixing, screen out remaining starchiness with 60~200 mesh after granulation, obtain To tea oil microcapsule granule.
The grain size of tea oil microcapsule granule obtained is 75~250 μm after mist projection granulating, for three layers of embedding structure, outside Portion is embedding medium, and inside is double-layer embedment lotion (tea tree oil microcapsule), and double-layer embedment lotion (tea tree oil microcapsule) is by grain size It is formed for 2~20 μm of tea tree oil microcapsules, the outer layer covers of tea tree oil microcapsule have aqueous emulsion, and the inside is that tea oil phosphatide is answered Object is closed, the phosphatide in tea oil phosphatide complexes is considered as the first coating to tea oil.
Embodiment 1
A kind of tea tree oil microcapsule and its granule are emulsified tea oil phosphatide complexes with aqueous emulsion, homogeneous obtains To tea tree oil microcapsule.Tea oil microcapsule granule will be obtained after tea tree oil microcapsule mist projection granulating.Tea oil phosphatide is compound Object is made by tea oil, phosphatide and oil-soluble inhibitor;Aqueous emulsion be disaccharide and wall material are dissolved in the water successively it is obtained.
Preparation method includes the following steps:
A. phosphatide, 1g vitamin Es and 20g tea oils that 10g HLB values are 10 are added sequentially in 20ml n-hexanes, added Heat is dried in vacuo to 40 DEG C after stirring 2h, and tea oil phosphatide complexes are made;
B. 100g sucrose, 70g guar gums are added sequentially to dissolve in 60 DEG C of 191g water, aqueous emulsion is made, High-shear emulsifying under the rotating speed of 8000r/min adds tea oil phosphatide complexes, continues high-shear emulsifying 30min, 20MPa Double-layer embedment lotion (tea tree oil microcapsule) is made in homogeneous 2 times under high pressure;
C. double-layer embedment lotion (tea tree oil microcapsule) is added in spray granulator, spraying inlet air temperature is 50 DEG C, together When top spray maltodextrin carry out a step granulation, the frequency of nozzle is 40Hz, rotating speed 2000r/min during mist projection granulating, is granulated knot 60 mesh of Shu Houyong screens out remaining starchiness, tea oil microcapsule granule.
The embedding rate of tea tree oil microcapsule is 99%.The grain size of tea oil microcapsule granule is 250 μm, the micro- glue of tea oil The grain size of microcapsules is 2~20 μm in capsule granule.
Embodiment 2
A kind of tea tree oil microcapsule and its granule are emulsified tea oil phosphatide complexes with aqueous emulsion, homogeneous obtains To tea tree oil microcapsule.Tea oil microcapsule granule will be obtained after tea tree oil microcapsule mist projection granulating.Tea oil phosphatide is compound Object is made by tea oil, phosphatide and oil-soluble inhibitor;Aqueous emulsion be disaccharide and wall material are dissolved in the water successively it is obtained. Preparation method includes the following steps:
A. phosphatide, 0.2kg tea polyphenols and 1kg tea oils that 1kg HLB values are 12 are added sequentially in 2L petroleum ethers, added Heat is dried in vacuo to 50 DEG C after stirring 3h, and tea oil phosphatide complexes are made;
B. 4kg lactose, 3.75kg Arabic gums are added sequentially to dissolve in 50 DEG C of 25kg water, aqueous emulsion is made, High-shear emulsifying under the rotating speed of 10000r/min adds tea oil phosphatide complexes, continues high-shear emulsifying 60min, 60MPa Double-layer embedment lotion (tea tree oil microcapsule) is made in homogeneous 3 times under high pressure;
C. double-layer embedment lotion (tea tree oil microcapsule) is added in spray granulator, spraying inlet air temperature is 30 DEG C, together When top spray cornstarch and cyclodextrin carry out a step granulation, the mass ratio of cornstarch and cyclodextrin is 2:1, maltodextrin and ring The mass ratio of dextrin is 1:1, the frequency of nozzle is 50Hz, rotating speed 3000r/min during mist projection granulating, with 200 after granulation Mesh screens out remaining starchiness, obtains tea tree oil microcapsule.
The embedding rate of tea tree oil microcapsule is 99%.The grain size of tea oil microcapsule granule is 75 μm, the micro- glue of tea oil The grain size of microcapsules is 2~20 μm in capsule granule.
Embodiment 3
A kind of tea tree oil microcapsule and its granule are emulsified tea oil phosphatide complexes with aqueous emulsion, homogeneous obtains To tea tree oil microcapsule.Tea oil microcapsule granule will be obtained after tea tree oil microcapsule mist projection granulating.Tea oil phosphatide is compound Object is made by tea oil, phosphatide and oil-soluble inhibitor;Aqueous emulsion be disaccharide and wall material are dissolved in the water successively it is obtained. Preparation method includes the following steps:
A. phosphatide, 2.5kg vitamin Es and 25kg tea oils that 25kg HLB values are 11 are added sequentially to 12.5L trichlorines In methane, 45 DEG C are heated to, is dried in vacuo after stirring 2.5h, tea oil phosphatide complexes are made;
B. 112.5kg maltose, 100kg Arabic gums are added sequentially to dissolve in 60 DEG C of 397.5 water, water and milk is made Agent, the high-shear emulsifying under the rotating speed of 10000r/min add tea oil phosphatide complexes, continue high-shear emulsifying 45min, Double-layer embedment lotion (tea tree oil microcapsule) is made in homogeneous 3 times under 40MPa high pressures;
C. double-layer embedment lotion (tea tree oil microcapsule) is added in spray granulator, spraying inlet air temperature is 10 DEG C, together When top spray cornstarch carry out a step granulation, the frequency of nozzle is 40Hz, rotating speed 2000r/min during mist projection granulating, is granulated knot 100 mesh of Shu Houyong screens out remaining starchiness, obtains tea tree oil microcapsule.
The embedding rate of tea tree oil microcapsule is 99%.The grain size of tea oil microcapsule granule is 150 μm, the micro- glue of tea oil The grain size of microcapsules is 2~20 μm in capsule granule.
In order to preferably verify the using effect of the present invention, inventor has carried out contrast test.
(1) promote growth of animal, the experiment for improving immunity applied to feed
Uniform 300 piggys of weight size (about 5Kg) are divided into six groups, wherein control group 1~3 is using conventional Forage feed, conventional feed formula is corn 25%, red dog flour 10%, wheat bran 30%, rapeseed cake 15%, cottonseed cake 15%, silkworm chrysalis 5%.Invention group is fed to be added in the conventional feed identical with control group using the tea tree oil microcapsule in embodiment, is invented Group 1, which is added to using the tea tree oil microcapsule in embodiment 1 in conventional feed, feeds, and invention group 2 is using the tea tree in embodiment 2 Oil microcapsule, which is added in conventional feed, feeds, and invention group 3 is added to conventional feed using the tea tree oil microcapsule in embodiment 3 Middle nursing, the additive amount of tea tree oil microcapsule are the 5% of conventional feed weight.Specific testing result as shown in Table 1 below, pig Average weight be pig after raising three months average weight, feed intake be to raise the average feed intake of three middle of the month daily.
Table 1
It is fed after can be seen that the tea tree oil microcapsule that the present invention is added in pannage according to result in table 1, with conventional feeding Material is fed and is compared, and the feed intake and weight of porkling significantly increase, and incidence is substantially reduced.
(2) experiment of antibiotic usage is replaced applied to veterinary drug
The laying hen 50 for suffering from influenza being born 120~140 days is chosen, flu symptom shows as spirit and declines, coughs, adopting Appetite declines, yellowish green excrement, laying rate is drawn to decline.Above-mentioned 50 chickens are randomly divided into control group and invention group, it is every group 10, right According to group 1 be conventional feed, conventional feed formula be corn 55%, wheat bran 20%, soya-bean cake 7%, cottonseed cake 5%, rape cake 5%, Fish meal 5%, bone meal 2%, shellfish powder 1%.Control group 2 is that ampicillin antibiolics is added in conventional feed, is fed in three times It supports, each drug additive amount is the 0.05% of conventional feed weight.Invention group is adds the tea in embodiment in conventional feed It sets oil microcapsule granule to feed, invention group 1 is fed for the tea oil microcapsule granule added in conventional feed in embodiment 1 It supports, invention group 2 is fed for the tea oil microcapsule granule added in conventional feed in embodiment 2, and invention group 3 is in routine The tea oil microcapsule granule added in feed in embodiment 3 is fed, and is fed in three times, tea oil when only feeding for the first time The additive amount of microcapsule granule is the 10% of conventional feed weight, second and third secondary nursing is conventional feed.Observation chicken daily Situation, as a result as shown in Table 2 below.
Table 2
It is fed after can be seen that the tea oil microcapsule granule that the present invention is added in chicken feed according to result in table 2, chicken Feed intake and laying rate significantly increase, treatment influenza it is with obvious effects.Compared with adding antibiont drug control group, illness subtracts Light degree is not much different, but the had good sustained release effect of the present invention, need to only add within one day primary, you can achieve the purpose that treatment, and add Added with antibiotic drug control group needs addition in one day three times, can be only achieved with the same effect of the present invention, the present invention is by natural plants Extract is prepared, natural health, and not as caused by antibiotics, microbial population of animal intestinal tract is unbalance, medicament residue and anti- The negative effects such as pharmacological property.

Claims (9)

1. a kind of tea tree oil microcapsule, it is characterised in that:Preparation method is to carry out tea oil phosphatide complexes with aqueous emulsion Emulsification, homogeneous obtain tea tree oil microcapsule.
2. a kind of tea tree oil microcapsule according to claim 1, it is characterised in that:Tea oil phosphatide complexes are by tea tree Oil, phosphatide and oil-soluble inhibitor are made;Aqueous emulsion is that disaccharide and wall material are dissolved in successively in 50~60 DEG C of water to be made.
3. a kind of tea tree oil microcapsule according to claim 2, it is characterised in that:The preparation side of tea oil phosphatide complexes Method is heated to 40~50 DEG C, stirs for phosphatide, oil-soluble inhibitor and tea oil are added sequentially in non-polar organic solvent It is dried in vacuo after mixing 2~3h.
4. a kind of tea tree oil microcapsule according to claim 3, it is characterised in that:Non-polar organic solvent for n-hexane, Any one of petroleum ether, ether, chloroform, the tea tree oil quality added in every milliliter of non-polar organic solvent for 0.5~ 2g, the HLB value of phosphatide is 10~12.
5. a kind of tea tree oil microcapsule according to claim 2, it is characterised in that:Oil-soluble inhibitor for tea polyphenols or Vitamin E;Disaccharide is any one of sucrose, lactose, maltose;Wall material is Arabic gum or guar gum.
6. a kind of tea tree oil microcapsule according to claim 2, it is characterised in that:The weight of each ingredient in tea tree oil microcapsule Amount number be 1 part of tea oil, phosphatidase 0 .5~1 part, 0.05~0.2 part of oil-soluble inhibitor, 4~5 parts of disaccharide, wall material 3.5~ 4 parts, the weight of water is 1~1.5 times of the total weight of tea oil, phosphatide, disaccharide, wall material and oil-soluble inhibitor.
7. a kind of tea tree oil microcapsule according to claim 1, it is characterised in that:It emulsifies as in 8000~10000r/min Rotating speed under high-shear emulsifying, time of emulsification is 30~60min;Homogeneous is homogeneous 2~3 times under 20~60MPa high pressures.
8. the granule prepared using a kind of tea tree oil microcapsule described in claim 1~7, it is characterised in that:By tea oil It obtains tea oil microcapsule granule after microcapsules mist projection granulating, embedding medium is entered using spray granulator top spray during mist projection granulating, It is 10~50 DEG C to control spraying inlet air temperature simultaneously, and remaining starchiness is screened out with 60~200 mesh after granulation.
9. granule prepared by a kind of tea tree oil microcapsule according to claim 8, it is characterised in that:It is sprayed during mist projection granulating The frequency of head is 40~50Hz, and rotating speed is 2000~3000r/min;The embedding medium is maltodextrin, cyclodextrin, cornstarch Any one of or several mixing;Tea oil Microcapsules Size in tea oil microcapsule granule is 2~20 μm.
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109362792A (en) * 2018-11-06 2019-02-22 广西必要科技有限公司 A kind of agricultural synergist and preparation method thereof and application method
CN114190481A (en) * 2021-11-15 2022-03-18 北京生泰尔科技股份有限公司 Coated thymol for livestock and preparation method thereof

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