CN101396068A - Carotenoid preparation and use thereof and feedstuff containing the preparation and preparation method thereof - Google Patents

Carotenoid preparation and use thereof and feedstuff containing the preparation and preparation method thereof Download PDF

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Publication number
CN101396068A
CN101396068A CNA2007101520268A CN200710152026A CN101396068A CN 101396068 A CN101396068 A CN 101396068A CN A2007101520268 A CNA2007101520268 A CN A2007101520268A CN 200710152026 A CN200710152026 A CN 200710152026A CN 101396068 A CN101396068 A CN 101396068A
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carotenoid
oil
feed
formulation
temperature
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CN101396068B (en
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邵斌
许新德
周迪
王燕峰
洪毅敏
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Zhejiang Medicine Co Ltd
Zhejiang Medicine Co Ltd Xinchang Pharmaceutical Factory
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Zhejiang Medicine Co Ltd Xinchang Pharmaceutical Factory
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Priority to CN2007101520268A priority Critical patent/CN101396068B/en
Priority to PCT/CN2008/000545 priority patent/WO2009039716A1/en
Priority to CL2008002231A priority patent/CL2008002231A1/en
Priority to NO20083794A priority patent/NO343960B1/en
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    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23DEDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
    • A23D9/00Other edible oils or fats, e.g. shortenings, cooking oils
    • A23D9/007Other edible oils or fats, e.g. shortenings, cooking oils characterised by ingredients other than fatty acid triglycerides
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23KFODDER
    • A23K20/00Accessory food factors for animal feeding-stuffs
    • A23K20/10Organic substances
    • A23K20/179Colouring agents, e.g. pigmenting or dyeing agents
    • 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
    • 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
    • A23L5/00Preparation or treatment of foods or foodstuffs, in general; Food or foodstuffs obtained thereby; Materials therefor
    • A23L5/40Colouring or decolouring of foods
    • A23L5/42Addition of dyes or pigments, e.g. in combination with optical brighteners
    • A23L5/43Addition of dyes or pigments, e.g. in combination with optical brighteners using naturally occurring organic dyes or pigments, their artificial duplicates or their derivatives
    • A23L5/44Addition of dyes or pigments, e.g. in combination with optical brighteners using naturally occurring organic dyes or pigments, their artificial duplicates or their derivatives using carotenoids or xanthophylls
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K47/00Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/06Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite
    • A61K47/08Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite containing oxygen, e.g. ethers, acetals, ketones, quinones, aldehydes, peroxides
    • A61K47/14Esters of carboxylic acids, e.g. fatty acid monoglycerides, medium-chain triglycerides, parabens or PEG fatty acid esters
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K47/00Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/44Oils, fats or waxes according to two or more groups of A61K47/02-A61K47/42; Natural or modified natural oils, fats or waxes, e.g. castor oil, polyethoxylated castor oil, montan wax, lignite, shellac, rosin, beeswax or lanolin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00Medicinal preparations characterised by special physical form
    • A61K9/10Dispersions; Emulsions

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Polymers & Plastics (AREA)
  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • General Health & Medical Sciences (AREA)
  • Animal Behavior & Ethology (AREA)
  • Veterinary Medicine (AREA)
  • Public Health (AREA)
  • Medicinal Chemistry (AREA)
  • Pharmacology & Pharmacy (AREA)
  • Epidemiology (AREA)
  • Zoology (AREA)
  • Animal Husbandry (AREA)
  • Dispersion Chemistry (AREA)
  • Nutrition Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Fodder In General (AREA)
  • Feed For Specific Animals (AREA)

Abstract

The invention provides a carotenoid preparation which relates to oil suspension, a feed which contains the carotenoid preparation, a method used for preparing the feed, and the use as additives of animal feed, food, cosmetics and/or medicines used for the carotenoid preparation. Effective compositions in the feed grains are uniformly distributed; furthermore, most of the effective compositions are distributed in the grains, thus reducing the surface oxidation loss; the carotenoid exists in a dissolved state, thus being beneficial for the absorption and utilization of animals; the animal tests also show that the coloring effect of the fish is extremely good after the feed grains are used for feeding the fish.

Description

Carotenoid formulation and application thereof and comprise feed of said preparation and preparation method thereof
Technical field
The present invention relates to a kind of carotenoid novel form, specifically, the method that relates to the carotenoid formulation of oil suspension, the feed that comprises described carotenoid formulation, the described feed of preparation, and carotenoid formulation is as the purposes of the additive of animal feed, food, cosmetics and/or medicine.
Background technology
According to the existence of oxygen atom in the molecular structural formula whether, carotenoid can be divided into two big classes, be respectively carotenoid and lutein class, the former does not have the existence of oxygen atom in the molecular structural formula, as beta carotene, lycopene, then include hydroxyl or carbonyl in the latter's the structural formula or comprise this two kinds of oxygen-containing functional groups, such as canthaxanthin, lutein, astaxanthin, zeaxanthin etc.In the carotenoid of lutein class, if a hydroxyl in its molecular structural formula, it often demonstrates yellow, if having carbonyl in its molecular structural formula, then demonstrates redness.
Carotenoid is a kind of important material in feed industry, they not only participate in the physiological metabolism of animal body, and can also give animal trunk or various chromatic colour such as feather or globefish, give aesthetic feeling, be widely used in laying hen, fryer, egg duck industry such as lutein, zeaxanthin and canthaxanthin, these pigments can make the skin of fowl, the yolk of birds, beasts and eggs demonstrate charming yellow and redness respectively; And astaxanthin extensively is present in marine fishes such as some salmons, salmon and crab, the shrimps.Animal self can not be synthesized and must be obtained these carotenoid by ingest wild plant or algae, owing to these reasons, generally to add an amount of carotenoid in the feed in order to the carotenoid levels in the animal of replenishing suitability for industrialized production such as fish, the bird body, reach nutrition and painted purpose.
Two problems that tend to run into when adding carotenoid in feed are respectively: the stability problem of carotenoid and bioavailability problem.This is because carotenoid itself is a kind of very unsettled material, its solubility in water, in the grease is very little, and particularly to experience the expanded step of HTHP in the process of aquatic feeds at feed, these mal-conditions are unfavorable for the stable of carotenoid, are reported in commodity canthaxanthin formulation common in the feed process as Berset (Ind.Aliment.Agric. (1987) 104:529-533) and have 18% loss of effective components; Henken and Estermann (Aquaculture Ind.Develop.Report (1991) 91:34-51) is reported in the process of fish meal, and the extrusion step can cause the loss of synthesizing astaxanthin 25-48%.And the carotenoid formulation can have influence on its bioavilability in animal body greatly.So just require to find suitable carotenoid formulation, make it in the feed process, not only be easy to add, and can also keep stable, the more important thing is that the carotenoid that requires to add is easy to absorb the bioavailability height in animal body.
Many researchs of related genera carrotene all are in order to reach above-mentioned two purposes, begin most is that to develop warm water solvable, the carotenoid microcapsules particulate of good stability, add first and other batch mixes in man-hour at feed, after maturation process, carry out granulation process again, because required temperature is not very high during granulation, like this as long as the good stability of carotenoid microcapsules particulate, certain hear resistance is arranged, the loss of the active component in process still is smaller, at present those are not needed through the high-temperature high-pressure swelling step, and only need mix, the fowl feed of slaking and granulation step, beastly feed, replenish lutein, vitamin A, beta-carrotene, the general still suitable carotenoid microcapsules product of interpolation when mixing during canthaxanthin, these products mainly contain Lali Red, Lali Yellow, Carophyll Red etc. but to those aquatic feeds such as shrimp feed, fish meal, because in process, need expanding treatment process through HTHP, if just add carotenoid for example behind the microcapsule product of astaxanthin in early stage like this, be easy to cause the active ingredient considerable damage, so people develop cold water soluble astaxanthin microcapsule product and a kind of back spraying technology again, be exactly with feed behind extrusion, the astaxanthin microcapsules that are dissolved in cold water evenly are sprayed in the expanded good feed, so just avoided the destruction of HTHP, improved the processing retention rate of astaxanthin astaxanthin.
Several astaxanthin formulations that are suitable for this technology are arranged at present, as the Lali Pink of Xinchang pharmaceutical factory (ZMC), the Carophyll Pink of DSM etc., they all are the astaxanthin product of cold water solubles type, have good solubility and stability.But this technology has also been brought following problem: well-known, for the nutrition of strengthening fish with to the absorption of carotenoid, in fish meal, often to add a large amount of oil, this oil is the mixture of fish oil and vegetable oil, these oil add by the back spraying technology, just with the fish meal extrusion good after, again at a large amount of grease of its surface spraying, grease is lipophilic, the adding and the astaxanthin that will add subsequently is dissolved in the water, very difficulty just becomes in the feed granules of one deck grease that the astaxanthin that is dissolved in water will be sprayed on surface coverage equably like this, the resistance that the existence of hydrophobicity oil makes nano level astaxanthin soluble in water enter the feed granules inner duct on the particle surface greatly strengthens, so these astaxanthins can only be distributed in particle surface and can not enter its inside; And if dissolving is incomplete in water for astaxanthin, short grained existence can be blocked the feed granules inner passage, also can stop astaxanthin only to be adsorbed in the surface to the granule interior infiltration.If elder generation's spraying astaxanthin aqueous solution sprays grease again and also can run into similar problem, make grease in feed granules, be difficult to evenly distribute.
For above-mentioned reasons, the astaxanthin that adds by the back spraying technology often only is adsorbed in the feed granules surface and can not be scattered in its inside, and this can cause the loss of other kind of active component form such as oxidation.And, because the inhomogeneities that distributes can cause the nonrepeatability of product quality, give to raise to produce and bring certain trouble.
In order to address these problems, and consider in the production process of shrimp pellet, the operation of one spraying grease is arranged after the extrusion step, the adding of astaxanthin can be merged in this step and go, just earlier the astaxanthin crystal is made the form of high-quality oil suspension, again this oil suspension is mixed dispersing or dissolving in the grease that will add, in spraying grease process, added the astaxanthin of requirement simultaneously.
In U.S. Patent number 5,716,655, with 6,083, introduced a kind of preparation method of pellet in 541, wherein relate to the back spraying of active component, specifically, in normal pressure or vacuum environment, will be scattered in carotenoid micro mist in the oil exactly and be sprayed in the feed granules after expanded.But obvious defects of the method is: carotenoid is to be scattered in the oil with the micro mist state, and its particle diameter is bigger, and maximum can reach 20 μ m.As previously mentioned, so big particle is enough to block the passage of pellet inside, thereby stoped oil suspension further to permeate to granule interior, cause many carotenoid crystals directly to be adsorbed in the surface of pellet, this not only causes the skewness of active ingredient easily, significantly reduce the fuel load of product, product quality has nonrepeatability, and oxidative degradation also very easily takes place in these carotenoid that are in the feed granules surface, what is more important, from start to finish, exist because carotenoid is the crystalline state with micro mist, this will inevitably obtain quite low bioavailability in animal body, because organism is very low to the carotenoid absorption rate of crystalline state, think that the coloring effect that reaches desirable must add the more carotenoid crystals of volume, this also will cause great waste.
Defective at above these technology, a kind of new carotenoid oil suspension preparation is provided among the present invention, the particle diameter of carotenoid micro mist is enough little in this oil suspension, to such an extent as in follow-up operation, under lower temperature, just in spray oil, dissolve fully at an easy rate, thereby can be scattered in the duct, inside of feed granules equably, product fuel load height, steady quality.And in this oil suspension, added certain natural, not only helped the stability of carotenoid in the feed granules, and helped animal body absorbing it.
Summary of the invention
A kind of novel form carotenoid oil suspension that is applicable to carotenoid in the pellet has been described among the present invention, carotenoid can be combined in the adding step of grease in the feed preparation process and add, because the grain diameter of carotenoid is very little in this oil suspension, the temperature that raise a little before adding in feed granules can be dissolved fully, this helps carotenoid and permeates in the feed granules inner passage, thereby evenly distribute, reach higher fuel load, stable product quality and raising organism are to the purpose of Bioavailability of Carotenoids, and in oil suspension, added a certain amount of antioxidant, help reducing the oxidational losses of carotenoid and the raising of its bioavailability in animal body.
According to an aspect of the present invention, the invention provides a kind of carotenoid formulation of oil suspension, described preparation comprises having carotenoid, antioxidant and the edible oil and fat that average grain diameter is less than or equal to 10 μ m.
Wherein, described carotenoid comprises astaxanthin, lutein, zeaxanthin, beta carotene, alpha-carotene, kryptoxanthin, lycopene, canthaxanthin and limocitrin.The average grain diameter of carotenoid particle is 4~6 μ m in the described oil suspension.
Wherein, described edible oil and fat comprise vegetable oil and animal oil; Vegetable oil comprises soybean oil, sunflower oil, rapeseed oil, corn oil, peanut oil, olive oil, and animal oil comprises fish oil.
Wherein, described preparation also comprises antioxidant.Described antioxidant is selected from one or more components in natural VE, synthesising complex E, 2.6-BHT (BHT), the tert-butyl group hydroxyl anisole (BHA).The addition of described antioxidant is 1~10wt% of oil suspension weight.The addition of described antioxidant is 2~5wt% of oil suspension weight.
Wherein, described content of carotenoid is 10~30wt% of oil suspension weight.
According to a second aspect of the invention, the present invention also provides a kind of feed that comprises described carotenoid formulation, in the final particle of described feed content of carotenoid at the 15mg/kg dry between the 100mg/kg dry.The final average diameter of particles of described feed is about 9mm, and length is between 0.9~1.2mm.
According to a third aspect of the invention we, the invention provides a kind of method for preparing described feed, described method comprises the steps:
(1) carotenoid is mixed with edible oil and fat, grinding or ball milling, obtain oil suspension;
(2) this oil suspension is stirred, rising temperature for dissolving obtains transparent solution, obtains containing this carotenoid grain diameter the oil solution that is 0 μ m;
(3) under normal pressure or vacuum environment, above-mentioned oil solution is sprayed directly into the feed granules surface, obtains the feed of final particle.
Wherein, carotenoid and part vegetable oil are pre-mixed grinding, fully mix with remaining vegetable oil again after reaching the requirement fineness; Perhaps with carotenoid with grind again after all vegetable oil fully mixes.
The temperature of described rising temperature for dissolving is 30~70 ℃, and preferably, the temperature of described rising temperature for dissolving is 40~60 ℃; Under this temperature, be incubated 0.5~5hr, preferably, under this temperature, be incubated 0.5~2hr.
According to last aspect of the present invention, the present invention also provides the purposes of a kind of carotenoid formulation as the additive of animal feed, food, cosmetics and/or medicine.
In sum, particularly in the process of aquatic feeds,, have bigger loss at the feed of routine as adding carotenoid expanded before owing to will relate to the high temperature high pressure process process.After being scattered in water-soluble carotenoid dry powder in the water, by the back spraying technology this being scattered in carotenoid in the water is sprayed on the feed granules surface and can reduces the loss that brings active component owing to high temperature high pressure process, but because a process of adding grease by the back spraying method itself is arranged in this type of feed process, more loaded down with trivial details in the operation so on the one hand, live through two steps back spraying step, on the other hand, because the hydrophily and the hydrophobicity of twice back spraying substance are opposite fully, the moisture that is sprayed at the feed granules surface earlier will inevitably stop the transfer of the grease of second step spraying to granule interior, the grease that perhaps is sprayed on particle surface earlier more can influence the stability of product quality owing to hydrophobic effect stops follow-up sprinkling carotenoid soluble in water in feed granules surface and inner even distribution.In technology afterwards, by carotenoid such as astaxanthin crystal directly are dispersed in the grease that is used for the back spraying, back spray processing interpolation carotenoid in conjunction with grease can overcome above-mentioned defective, bring the loss of operational simplicity and minimizing carotenoid process, but because carotenoid is that form with crystal is adsorbed in the feed granules surface in the method, these may stop up the inner duct of feed granules than megacryst, cause active ingredient skewness therein, the more important thing is, the carotenoid that animal body is ingested exists with crystal state, this can reduce these Bioavailability of Carotenoids widely, causes coloring effect relatively poor.
Therefore, deficiency at above each technology, a kind of method of effectively adding carotenoid in pellet is disclosed among the present invention, make carotenoid before the spraying operation of back, keep dissolved state, can guarantee operational easy like this, stability that again can product quality, the more important thing is has good coloring effect in animal feeding.
Below the present invention is carried out following specific descriptions:
In the present invention, earlier carotenoid is carried out ultramicro grinding by certain mode, its particle diameter is reached below the 10 μ m, be generally 4~6 μ m.Micro mist after again this being pulverized is well-dispersed in the vegetable oil, and this vegetable oil can be other oils that can buy on soybean oil, sunflower oil, rapeseed oil and other market.Also carotenoid crystals and part plant oil can be pre-mixed grinding, fully mix with remaining vegetable oil again after reaching the requirement fineness; Perhaps with carotenoid crystals with grind again after all plant oil fully mixes.Lapping mode can be for directly grinding or ball milling etc.Final oil suspension product has good flowing property, wherein the particle diameter of carotenoid requires to be generally 4~6 μ m, maximum is no more than 10 μ m, and this size distribution helps the excellent dissolution of particle in the subsequent technique, and particle size distribution is seen Fig. 1 in the typical carotenoid oil suspension.Carotenoid concentration is between 10~30wt%, and under the prerequisite that guarantees liquid fluidity, content of effective also can be higher.
In the present invention, in order to reduce the loss of carotenoid in processing and the storage process, in above-mentioned oil suspension, added a certain amount of antioxidant, can be natural VE, synthesising complex E, BHT, BHA or other kind and permit the antioxidant of use legally, preferential vitamin E class is because it helps animal body absorbing carotenoid.The addition of antioxidant for this reason the oil suspension total amount 1~10%, preferably 2~5%.
Carotenoid oil suspension is sprayed onto before the feed granules behind the extrusion, earlier part or all of oil suspension and the grease class (mixture of vegetable oil or fish oil or vegetable oil and fish oil) that will spray are mixed, and under condition of stirring rising temperature for dissolving, obtain transparent solution.The temperature that raises is between 30~70 ℃, preferred 40~60 ℃, under this temperature, be incubated 0.5~5hr, and preferred 0.5~2hr, in this process, any change can take place in content of carotenoid and content of isomer hardly.
Carotenoid in the above-mentioned grease can be sprayed directly into the feed granules surface together with grease under normal pressure or vacuum environment.Before spraying according to the needs of feed formula, can replenish or not replenish new grease class, these greases are the mixture of plant oil or fish oil class or vegetable oil and fish oil, temperature can drop to normal temperature, be to make carotenoid oil suspension in grease, keep the temperature of dissolved state in the time of also can keeping beginning, but generally speaking, carotenoid was to be in dissolved state before spraying, and its typical particle diameter in grease distributes and sees Fig. 2.
The composition of the feed among the present invention can carry out suitable adjustment according to actual needs, purpose is to satisfy the nutritional need of different animals, and parameters such as the outward appearance of feed granules, shape, size, weight and porosity also are to decide according to different object and the features of feeding of feeding.
As required, the carotenoid of interpolation can be the monomer of astaxanthin, canthaxanthin, lutein, zeaxanthin and other kind liposoluble vitamin or one or more mixture in them.To between the 100mg/kg dry, the addition of total grease is to add according to the growth of animal requirement to content of carotenoid at the 15mg/kg dry in the final feed particle.
The feed granules that obtains according to the present invention, active ingredient is evenly distributed therein, and the overwhelming majority is distributed in granule interior, has reduced the surface oxidation loss; Carotenoid exists with dissolved state, helps absorbing of animal body, and animal experiment shows that also to feed behind this kind feed granules the coloring effect of fish fine.
Technical characterstic of the present invention and advantage can well be embodied in embodiment subsequently, but this inventive method not only is confined to this embodiment.
Description of drawings
Fig. 1 represents the particle size distribution figure of the carotenoid of oil suspension;
The particle size distribution figure of Fig. 2 representation class carrotene before spraying.
The specific embodiment
Embodiment 1
The preparation of astaxanthin 20% oil suspension
(content: 97.2%) 2.2kg, natural VE 0.3kg and 5.0kg sunflower oil mix to take by weighing the pure product of astaxanthin, place grinding in ball grinder 1.5hr, get thick fluid after the taking-up, replenish the 2.5kg sunflower oil again, mix the mobile oil suspension of astaxanthin preferably.
Record by ultraviolet spectrophotometry that content astaxanthin is 21.2% in the oil suspension, record with the laser particle size distribution instrument that the particle average grain diameter is 4.68 μ m in the oil suspension.
The dissolving of astaxanthin before the spraying
Getting above-mentioned astaxanthin oil suspension 8.0kg is that the grease class that 4800kg need add (is the mixture of fish oil and soybean salad oil with part, their ratio is 2:1) mix, being warming up to 60 ℃ of insulation 1.5hr under stirring state fully dissolves the astaxanthin particulate of suspension, get clear solution, compound lard 4800kg with remainder joins in the solution of above-mentioned astaxanthin again, stir, temperature drops to 40 ℃.Recording the blue or green crude granule particle diameter of solution Prawn with the laser particle size distribution instrument is 0 μ m, illustrates that astaxanthin is dissolved in the grease fully.
The salmon feed is sprayed
Get the oil solution 1200kg (astaxanthin-containing is about 0.2kg) of above-mentioned astaxanthin, spray under the vacuum environment in the half-finished pellet of 2800kg and remove (granulation of this feed and puffing process, but do not spray grease), the feed granules diameter is about 9mm, length between 0.9 to 1.2mm, every heavily about 350mg.This spraying process has continued about 1.0hr, and each particle surface color homogeneous of the feed that obtains, and also uniformity of granule interior color and outer surface color illustrate that astaxanthin fully is penetrated into granule interior with grease.
Feed is handled the back record with HPLC that content astaxanthin is the 50mg/kg dry in the final feed.
The salmon feeding trial
Get atlantic salmon 5000 tails after June, feed by normal feeding amount and above-mentionedly to add the pellet of astaxanthin and grease simultaneously by the back spraying method, take out 10 tail salmons wherein at set intervals at random, get respectively and survey wherein content astaxanthin with the HPLC method after its muscle of back is handled, get its mean value.
After recording 50 days, 100 days and 150 days as stated above, the content of astaxanthin is respectively 8.5mg/kg, 10.4mg/kg and 14.7mg/kg fresh weight in the atlantic salmon muscle, and bright-colored, coloring effect is obvious.
The comparative example 2
Press U.S.Pat.5,716,655 and U.S.Pat.6,083, the method that discloses in 541 makes the feed granules that content astaxanthin is the 50mg/kg dry, does not have antioxidants such as natural VE in its oil suspension, does not also pass through the abundant course of dissolution of heating before the grease spraying, because dissolved particles is not to the ponding in duct, feed granules inside, make not too homogeneous of the inner and outer surface color of feed granules.
The feed granules that obtains with the method carries out animal experiment by the method among the embodiment 1, after 50 days, 100 days and 150 days, the content of astaxanthin is respectively 5.9mg/kg, 8.8mg/kg and 11.5mg/kg fresh weight in the test atlantic salmon muscle, like this different phase salmon to the utilization rate of astaxanthin respectively than hanging down 30.6%, 15.4%, 21.8% among the embodiment 1.
Can find out significantly from embodiment 1 and comparative example 2 by advantage of the present invention: at first, special particle diameter is distributed with to be beneficial to before spraying and just can dissolves fully under lower temperature in the oil suspension; Secondly, astaxanthin dissolving before spraying fully just is difficult for blocking the inner duct of feed granules, make active ingredient can be evenly distributed on the surface of feed granules and inner, help the product quality stable homogeneous, and fish are improved greatly to the absorptivity of the astaxanthin of dissolved state; At last, the existence of antioxidant natural VE also helps growth of fish and absorbing astaxanthin in the oil suspension.And animal experiment shows that also to feed behind the feed granules of the present invention the coloring effect of fish fine.
Embodiment 3-6
The preparation process of oil suspension is listed in the table 1 among the embodiment 3-6:
The preparation of oil suspension among the table 1. embodiment 3-6
Embodiment 3 Embodiment 4 Embodiment 5 Embodiment 6
The carotenoid kind Lutein Canthaxanthin Beta carotene Zeaxanthin
Vegetable oil kind Sunflower oil Rapeseed oil Corn oil Peanut oil
The antioxidant kind BHT BHA Synthesising complex E Synthesising complex E
Carotenoid content in the oil suspension 10wt% 20wt% 30wt% 20wt%
Oxidation preventive content in the oil suspension 1% 2.5% 10% 5%
The carotenoid particle diameter distributes in the oil suspension 4μm 6μm 3μm 10μm
Rising temperature for dissolving temperature before the spraying 30 40℃ 70℃ 70℃
The rising temperature for dissolving time before the spraying 5hr 2hr 0.5hr 1.5hr
Carotenoid content in the final particle The 100mg/kg dry The 20mg/kg dry The 15mg/kg dry The 15mg/kg dry
The present invention is illustrated by top embodiment, still, should be appreciated that the present invention is not limited to particular example as described herein and embodiment.The purpose that comprises these particular example and embodiment here is to help those of skill in the art to put into practice the present invention.Any those of skill in the art are easy to be further improved without departing from the spirit and scope of the present invention and perfect, therefore the present invention only is subjected to the restriction of the content and the scope of claim of the present invention, and its intention contains all and is included in alternative and equivalent in the spirit and scope of the invention that is limited by claims.

Claims (18)

1, a kind of carotenoid formulation of oil suspension, described preparation comprise having carotenoid, antioxidant and the edible oil and fat that average grain diameter is less than or equal to 10 μ m.
2, carotenoid formulation as claimed in claim 1, described carotenoid comprises astaxanthin, lutein, zeaxanthin, beta carotene, alpha-carotene, kryptoxanthin, lycopene, canthaxanthin and limocitrin.
3, carotenoid formulation as claimed in claim 1, described edible oil and fat comprise vegetable oil and animal oil; Wherein, described vegetable oil comprises soybean oil, sunflower oil, rapeseed oil, corn oil, peanut oil, olive oil, and described animal oil comprises fish oil.
4, carotenoid formulation as claimed in claim 2, the average grain diameter of described carotenoid are 4~6 μ m.
5, carotenoid formulation as claimed in claim 1 also comprises antioxidant.
6, carotenoid formulation as claimed in claim 5, described antioxidant are selected from one or more components in natural VE, synthesising complex E, 2.6-BHT, the tert-butyl group hydroxyl anisole.
7, carotenoid formulation as claimed in claim 6, the addition of described antioxidant are 1~10wt% of oil suspension weight.
8, carotenoid formulation as claimed in claim 6, the addition of described antioxidant are 2~5wt% of oil suspension weight.
9, as the arbitrary described carotenoid formulation of claim 1~8, described content of carotenoid is 10~30wt% of oil suspension weight.
10, a kind of feed that comprises as the arbitrary described carotenoid formulation of claim 1~9, in the final particle of described feed content of carotenoid at the 15mg/kg dry between the 100mg/kg dry.
11, feed as claimed in claim 10, the final average diameter of particles of described feed is about 9mm, and length is between 0.9~1.2mm.
12, a kind of preparation is as the method for claim 10 or 11 described feeds, and described method comprises the steps:
(1) carotenoid is mixed with edible oil and fat, grinding or ball milling, obtain oil suspension;
(2) this oil suspension is stirred, rising temperature for dissolving obtains transparent solution, obtains containing this carotenoid grain diameter the oil solution that is 0 μ m;
(3) under normal pressure or vacuum environment, above-mentioned oil solution is sprayed directly into the feed granules surface, obtains the feed of final particle.
13, method as claimed in claim 12 is pre-mixed grinding with carotenoid and part vegetable oil, fully mixes with remaining vegetable oil after reaching the requirement fineness again; Perhaps with carotenoid with grind again after all vegetable oil fully mixes.
14, method as claimed in claim 12, the temperature of described rising temperature for dissolving are 30~70 ℃.
15, method as claimed in claim 14, the temperature of described rising temperature for dissolving are 40~60 ℃.
16, as claim 14 or 15 described methods, temperature retention time is 0.5~5hr under this temperature.
17, as claim 14 or 15 described methods, temperature retention time is 0.5~2hr under this temperature.
18, a kind of comprising as the purposes of the arbitrary described carotenoid formulation of claim 1~9 as the additive of animal feed, food, cosmetics and/or medicine.
CN2007101520268A 2007-09-27 2007-09-27 Carotenoid preparation and use thereof and feedstuff containing the preparation and preparation method thereof Active CN101396068B (en)

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PCT/CN2008/000545 WO2009039716A1 (en) 2007-09-27 2008-03-19 Carotenoid formulations and use thereof, and feeds containing the formulation and processes for the preparation of the feeds
CL2008002231A CL2008002231A1 (en) 2007-09-27 2008-07-30 Formulations of carotenoids and their use, and foods that contain the formulation and processes for the preparation of foods.
NO20083794A NO343960B1 (en) 2007-09-27 2008-09-03 Process for preparing a feed comprising a carotenoid formulation

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