CN106666731A - Stable liposoluble nutrient microcapsules as well as preparation method and application thereof - Google Patents
Stable liposoluble nutrient microcapsules as well as preparation method and application thereof Download PDFInfo
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- CN106666731A CN106666731A CN201611242763.2A CN201611242763A CN106666731A CN 106666731 A CN106666731 A CN 106666731A CN 201611242763 A CN201611242763 A CN 201611242763A CN 106666731 A CN106666731 A CN 106666731A
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- starch
- microcapsule
- oil
- preparation
- oil phase
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- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 description 1
- ZAKOWWREFLAJOT-CEFNRUSXSA-N D-alpha-tocopherylacetate Chemical compound CC(=O)OC1=C(C)C(C)=C2O[C@@](CCC[C@H](C)CCC[C@H](C)CCCC(C)C)(C)CCC2=C1C ZAKOWWREFLAJOT-CEFNRUSXSA-N 0.000 description 1
- 244000068988 Glycine max Species 0.000 description 1
- 235000010469 Glycine max Nutrition 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000004166 Lanolin Substances 0.000 description 1
- 229920002774 Maltodextrin Polymers 0.000 description 1
- 239000005913 Maltodextrin Substances 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 239000005642 Oleic acid Substances 0.000 description 1
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 1
- 235000021314 Palmitic acid Nutrition 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 235000021355 Stearic acid Nutrition 0.000 description 1
- 229930006000 Sucrose Natural products 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- DTOSIQBPPRVQHS-PDBXOOCHSA-N alpha-linolenic acid Chemical compound CC\C=C/C\C=C/C\C=C/CCCCCCCC(O)=O DTOSIQBPPRVQHS-PDBXOOCHSA-N 0.000 description 1
- 235000020661 alpha-linolenic acid Nutrition 0.000 description 1
- 238000009360 aquaculture Methods 0.000 description 1
- 244000144974 aquaculture Species 0.000 description 1
- 150000001514 astaxanthins Chemical class 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 229940116226 behenic acid Drugs 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 150000001707 canthaxanthins Chemical class 0.000 description 1
- 235000014633 carbohydrates Nutrition 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 239000004203 carnauba wax Substances 0.000 description 1
- 210000004027 cell Anatomy 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000007385 chemical modification Methods 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- ZAKOWWREFLAJOT-UHFFFAOYSA-N d-alpha-Tocopheryl acetate Natural products CC(=O)OC1=C(C)C(C)=C2OC(CCCC(C)CCCC(C)CCCC(C)C)(C)CCC2=C1C ZAKOWWREFLAJOT-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- ZPWVASYFFYYZEW-UHFFFAOYSA-L dipotassium hydrogen phosphate Chemical compound [K+].[K+].OP([O-])([O-])=O ZPWVASYFFYYZEW-UHFFFAOYSA-L 0.000 description 1
- 229910000396 dipotassium phosphate Inorganic materials 0.000 description 1
- 229910000397 disodium phosphate Inorganic materials 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- OVBPIULPVIDEAO-LBPRGKRZSA-N folic acid Chemical compound C=1N=C2NC(N)=NC(=O)C2=NC=1CNC1=CC=C(C(=O)N[C@@H](CCC(O)=O)C(O)=O)C=C1 OVBPIULPVIDEAO-LBPRGKRZSA-N 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 210000003976 gap junction Anatomy 0.000 description 1
- 229940075507 glyceryl monostearate Drugs 0.000 description 1
- 230000012010 growth Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000036737 immune function Effects 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 1
- 239000012182 japan wax Substances 0.000 description 1
- 235000019388 lanolin Nutrition 0.000 description 1
- 229940039717 lanolin Drugs 0.000 description 1
- 229920005610 lignin Polymers 0.000 description 1
- 229960004488 linolenic acid Drugs 0.000 description 1
- KQQKGWQCNNTQJW-UHFFFAOYSA-N linolenic acid Natural products CC=CCCC=CCC=CCCCCCCCC(O)=O KQQKGWQCNNTQJW-UHFFFAOYSA-N 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 229940035034 maltodextrin Drugs 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 239000001788 mono and diglycerides of fatty acids Substances 0.000 description 1
- 230000021332 multicellular organism growth Effects 0.000 description 1
- WQEPLUUGTLDZJY-UHFFFAOYSA-N n-Pentadecanoic acid Natural products CCCCCCCCCCCCCCC(O)=O WQEPLUUGTLDZJY-UHFFFAOYSA-N 0.000 description 1
- 235000016709 nutrition Nutrition 0.000 description 1
- 230000035764 nutrition Effects 0.000 description 1
- 239000007764 o/w emulsion Substances 0.000 description 1
- UTOPWMOLSKOLTQ-UHFFFAOYSA-M octacosanoate Chemical compound CCCCCCCCCCCCCCCCCCCCCCCCCCCC([O-])=O UTOPWMOLSKOLTQ-UHFFFAOYSA-M 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
- 235000021313 oleic acid Nutrition 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 230000035479 physiological effects, processes and functions Effects 0.000 description 1
- 230000035790 physiological processes and functions Effects 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 235000020777 polyunsaturated fatty acids Nutrition 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 230000001850 reproductive effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000600 sorbitol Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000012177 spermaceti Substances 0.000 description 1
- 229940084106 spermaceti Drugs 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 239000001334 starch sodium octenyl succinate Substances 0.000 description 1
- 235000013826 starch sodium octenyl succinate Nutrition 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000005720 sucrose Substances 0.000 description 1
- 239000003760 tallow Substances 0.000 description 1
- 229940042585 tocopherol acetate Drugs 0.000 description 1
- 125000002640 tocopherol group Chemical group 0.000 description 1
- 235000015112 vegetable and seed oil Nutrition 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
Landscapes
- Medicinal Preparation (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
The invention discloses a preparation method and an application of stable liposoluble nutrient microcapsules. The method comprises the steps as follows: 1) an oil phase is subjected to spray granulation by a fluidized bed, and microcapsules coated with starch granules are formed; 2) the temperature is increased to a dry temperature, an alkali solution is added to the fluidized bed by spraying, so that starch and grease on the surfaces of the microcapsules are gelatinized and saponified at the same time, a compact protective film is formed, and the stable liposoluble nutrient microcapsules are obtained, wherein the oil phase is a grease solution or a grease dispersion liquid containing liposoluble nutrients and an antioxidant. The preparation method performs gelatinization and saponification under the flow dry condition simultaneously, a formed dual protection film containing gelatinized starch and saponified grease is more compact, and the microcapsules are more stable.
Description
Technical field
The invention belongs to field of medicine and chemical technology, and in particular to a kind of preparation side of stable fat soluble nutrient microcapsule
Method.
Background technology
Fat soluble nutrient of the present invention is primarily referred to as fatsoluble vitamin and carotenoid.Vitamin be people and
Animal is the micro organic Auto-regulator of a class that maintain normal physiological function and must obtain from food, body growth,
Play an important role in metabolism, growth course；Carotenoid is the general name of the important natural pigment of a class, it is possible to increase dynamic
Thing reproductive capacity, immunologic function, with antioxidation, coloring and reinforcement cell and various physiology such as the ability that cell gap junction is exchanged
Function.Carotenoid and vitamin can not synthesize in vivo or synthetic quantity is not enough, it is often necessary to be fitted by food or feedstuff from the external world
Amount supply.
It is extremely sensitive to light, heat and oxygen because vitamin and carotenoid are in itself the highly unstable materials of a class,
Be not suitable for directly adding in feedstuff or food, therefore many research worker and company have developed respectively for stablizing these work
Property material method, such as WO2005/013708 announce use milk proem, carbohydrate, reducing sugar through cross-linking agents
Fatsoluble vitamin, the carotenoid dry powder of parcel, its vitamin, carotenoid include vitaminss, carotenoid
Class and polyunsaturated fatty acid etc..
A kind of stable vitamin and/or the microcapsule and its production method of carotenoid that US6328995 is introduced, should
Method is dispersed to 0.1%~20% one or more fatsoluble vitamiies and/or one or more carotenoid containing 2%
~40% at least one protein, 1%~30% at least one sugar, 0.2%~20% K2HPO4、Na2HPO4It is mixed
Compound, remaining composition for water system in after by spray drying technology be obtained；CN100527983C is mentioned and inhaled using Silicon stone
Adding sorbitol ester emulsifier during attached Vitamin E can improve the bioavailability of vitamin e acetate；CN101703243B is utilized
The maltodextrin and gelatin of special ratios as wall material, the mixture using glyceryl monostearate and sucrose ester as emulsifying agent,
The Vitamin E contained micro capsule for being highly soluble in water is obtained.
It is reported above to have respective advantage, the stability of active substance is also improve to a certain extent, but it is common
With deficiency be：1) can to some extent there is space and aperture on microcapsule or adsorbent surface, protective layer is inadequate
Densification, oxygen enters and touches vitamin, carotenoid along space and aperture in storage, transport and secondary processing process,
Easily there is side reaction and content to decline；2) microcapsule class product surface in embedding more or less has core residual, directly
Using the loss that certainly will cause this some vitamin, carotenoid.If added in premix material, affected by the course of processing,
As astaxanthin isoreactivity composition has 35%~48% loss [Ind.Aliment.Agric. (1987) 104:529-533；
Aquaculture Ind.Develop.Report(1991)91:34-51]；By vitamin A acetate dry powder application to milk powder system
For into after infantile nutrition strengthening model, after milk powder is stored 6 months under 40 DEG C, 75% damp condition, vitamin A acetate contains
Amount has 18%~25% decline；When the application of lycopene dry powder is to health product, after tabletting makes tablet, 40 DEG C,
After storing 6 months under 75% damp condition, lycopene content has 20%~32% decline；And the application of canthaxanthin dry powder is extremely
After feedstuff, after feedstuff accelerates January under 60 DEG C, 75% damp condition, the canthaxanthin content in feedstuff declines 15%~27%.Portion
Storage stability of the dry powder formulations not only in storage is divided still to can further improve, and it is in feedstuff, food and health care
Application stability in product also has larger room for promotion.
CN201280019199.1 reports the beadlet preparation method comprising carotenoid, by containing fat-soluble nutrients
The high-melting-point grease spraying condensation of element obtains beadlet, but the dosage form rigidity is not enough, fragile in the courses of processing such as follow-up tabletting
Damage, and the fat soluble nutrient shortage of surface of beads is effectively protected carrier, these can all cause fat soluble nutrient unstable.
CN201380011311.1 and CN201480062474.7 are then respectively by the way that fat soluble nutrient and emulsifying are protected
The mode of colloid or macromolecular material mixing extrusion is processed, but these dosage forms are formed without for the fat soluble nutrient on surface
Effect protection.
The content of the invention
For the not enough and defect that existing fat soluble nutrient preparation is present, the invention provides a kind of stable fat-soluble
The preparation method of nutrient microcapsule, the method is easy to operate, and obtained fat soluble nutrient microcapsule stability is more preferable.
A kind of preparation method of stable fat soluble nutrient microcapsule, comprises the steps：
1) oil phase containing ore materials is carried out into fluidized bed spray granulation, forms the microcapsule that surface is coated by starch grain；
2) baking temperature is warming up to, the spraying in fluid bed adds aqueous slkali, makes the starch and oils and fatss of surface of microcapsule same
Shi Fasheng gelatinizings and saponification, form fine and close protecting film, obtain stable fat-soluble nutrients cellulose capsule；
Described oil phase is the fat solution comprising the ore materials, fat soluble nutrient and antioxidant or oils and fatss point
Dispersion liquid；Described ore materials are one or more in silicon dioxide, Calcium Carbonate, calcium phosphate, magnesium carbonate or magnesium phosphate, Ore
Mass ratio of the material in oil phase is 10~30%.
The described fat solution comprising fat soluble nutrient and antioxidant refer at high temperature fat soluble nutrient and
Antioxidant is dissolved in oils and fatss, becomes solution；
The described oils and fatss dispersion liquid comprising fat soluble nutrient and antioxidant refers to fat soluble nutrient under room temperature, resists
Oxidant and oils and fatss mixed grinding, become dispersion liquid, or the organic solvent solution of fat soluble nutrient, antioxidant is sprayed
To in oils and fatss, nutrient is made with the precipitation of fine grained form, while removing solvent by heating up, become the nutrient after spraying crystallize
Dispersion liquid.
In the present invention, described fat soluble nutrient be beta-carotene, astaxanthin, lycopene, canthaxanthin, phylloxanthin,
Vitamin D3, retinyl acetate, Vitamin E, vitamin e derivative or their mixture；
Mass ratio of the described fat soluble nutrient in oil phase is 1~60%；
Oils and fatss in the oil phase are soybean oil, Semen Maydis oil, Oleum Arachidis hypogaeae semen, Oleum Cocois, Oleum sesami, olive oil, Petiolus Trachycarpi oil, dish
In seed oil, Testa oryzae oil, Oleum Helianthi, cupu oil, butter, Adeps Sus domestica, Adeps Bovis seu Bubali, herring oil, pilchard oil, haco oil, mineral oil
One or more；
Described antioxidant is tocopherol, ethoxyquin, BHT (2,6 di tert butyl 4 methyl phenol), BHA (butyl
BHA) or TBHQ (tert-butylhydroquinone) in one or more；
Mass ratio of the described antioxidant in oil phase is 0.1~5%；
Described starch is in potato starch, corn starch, waxy corn starch, pea starch or sweet potato starch
Kind；
Described alkali liquor is sodium hydroxide that mass concentration is 10~50% or the aqueous solution of potassium hydroxide；
Described baking temperature is 30~50 DEG C.
The mechanism of gelatinizing of the present invention and saponification is：
1) surface starch grain is run into after alkali liquor, and local can occur rapidly gelatinizing so that micellar structure is significantly destroyed, and forms paste
Shape liquid, enables the space that starch grain is formed when adsorbing to be partially filled with, and intercepting air effect strengthens；
2) while, the barish oils and fatss of surface of microcapsule after running into alkali liquor, equally can rapidly occur saponification so that solidifying
Solid point is improved, and intercepting air effect strengthens, and heat-resisting quantity is improved.
Oil phase mist projection granulating is carried out starch adsorption by the present invention, in fluidized drying condition after the completion of absorption, by spraying
Mode add alkali liquor, carry out saponification and gelatinizing under graininess, surface of microcapsule formed densification gelatinized starch/saponification
The duplicate protection film of oils and fatss, finally obtains stable fat soluble nutrient microcapsule.The microcapsule protecting film of indication of the present invention by
Starch and oils and fatss gelatinizing simultaneously and saponification are obtained, and protecting film is finer and close, stable.
Ore materials are then as rigid filler material, it is ensured that the overall structure of microcapsule so as to meet instantaneous high-temperature, height
Pressure is difficult avalanche.
Also include in stability, oil phase described in the present invention to further improve fat soluble nutrient microcapsule
High melting point component.Using high melting point component, the freezing point of microcapsule inside oil phase is raised, fat soluble nutrient can be substantially reduced
Oxidized speed.
Described high melting point component is that freezing point is more than 30 DEG C, can be wax, hardening (hydrogenation or part hydrogenate) oil/grease
One or more in fat, higher fatty acids.
Described wax can be animal wax, the vegetable wax of animal wax, vegetable wax and synthetic wax or chemical modification, for example, eat
Grade paraffin, microwax, Cera Flava, candelilla wax, palm wax, montanate are cured, the oily wax of Fructus Oryzae Germinatus, spermaceti, lanolin wax, Xi Mende
Haze tallow, Sa Suoer waxes, Japan wax etc.；
Described hardening (hydrogenation or part hydrogenate) oil/grease fat can be the oils and fatss used in the oil phase, preferred hydrogen
Change the one kind in Petiolus Trachycarpi oil, cotmar and oil with hydrogenated soybean；
Described higher fatty acids are C16-C24Saturation or undersaturated fatty acid, for example palmitic acid, pearly-lustre fat acid,
Stearic acid, Oleic acid, linoleic acid, linolenic acid, arachidic acid, EPA (eicosapentaenoic acid), behenic acid, DHA (two dodecahexaenes
Acid), lignin acid etc.；
Mass ratio of the described high melting point component in oil phase is 30~70%.
Present invention also offers the fat soluble nutrient microcapsule that a kind of described preparation method is obtained.
Present invention also offers a kind of application of described fat soluble nutrient microcapsule, described fat soluble nutrient is micro-
Capsule is used to be processed into other dosage forms, and other dosage forms can be any dosage form outside microcapsule.Preferably, its described
Its dosage form is tablet, at this point it is possible to passing through tabletting method commonly used in the prior art obtains corresponding tablet.
Present invention also offers a kind of feedstuff, food (such as milk powder) or health product, comprising described microcapsule or its
Its dosage form is used as additive, at this point it is possible to improve the retention time of active component in these products, improves the storage life of product
Limit.
The gelatinizing and saponification process of the present invention is realized by adding aqueous slkali toward the microcapsule spraying in fluid bed, should
Process is not only capable of achieving the gelatinizing and saponification of surface starch grain and oils and fatss, while and having functions/drying concurrently.Therefore, as long as general alkali
After liquid spraying terminates, then stop 30~40 minutes or so in fluid bed, you can obtain stable fat soluble nutrient microcapsule.
Compared with prior art, it is an advantage of the current invention that：
1) by carrying out gelatinizing and saponification simultaneously under fluidised form drying condition, the gelatinized starch of formation and saponification oils and fatss it is double
Weight protecting film, protecting film is finer and close, and microcapsule is more stable；
2) high melting point component and ore materials are with the addition of, the heatproof of microcapsule, resistance to pressure is greatly improved.
Specific embodiment
The preparation of the retinyl acetate microcapsule of embodiment 1
At 60 DEG C, by 15 part by weight of vitamin A acetass, 1 weight portion ethoxyquin, 4 parts by weight Corn oil, 70 weight portions
Microwax mixed dissolution, adding 10 weight portion magnesium carbonate makes it be uniformly dispersed, and obtains oil phase.Oil phase is sprayed to and is covered with Ma Ling
Adsorb pelletize in the fluid bed of sweet potato starch granule, obtain the microcapsule that surface is coated by starch.
Temperature is set to 50 DEG C in fluid bed, and spraying adds the sodium hydrate aqueous solution that mass concentration is 40%, makes microcapsule
There is gelatinizing and saponification in the starch and oils and fatss on surface, spraying stays on 30 minutes after terminating in fluid bed simultaneously, obtain steady
Fixed retinyl acetate microcapsule.
The preparation of the retinyl acetate microcapsule of embodiment 2
It is at 60 DEG C, 15 part by weight of vitamin A acetass, 1 weight portion ethoxyquin, the oil mixing of 64 parts by weight Corn is molten
Solution, adds 20 weight parts of calcium carbonate, obtains oil phase.Oil phase is sprayed in the fluid bed for be covered with potato starch particle and is adsorbed
Pelletize, obtains the microcapsule that surface is coated by starch.
Temperature is set to 30 DEG C in fluid bed, and spraying adds the sodium hydroxide solution that mass concentration is 40%, makes microcapsule table
There is gelatinizing and saponification in the starch and oils and fatss in face, spraying stays on 40 minutes after terminating in fluid bed simultaneously, obtain dimension life
Plain A acetass microcapsule.
The preparation of the retinyl acetate microcapsule of embodiment 3
At 60 DEG C, by 15 part by weight of vitamin A acetass, 1 weight portion ethoxyquin, 14 parts by weight Corn oil, 60 weight
Part microwax mixed dissolution, adds 10 weight parts of calcium carbonate, obtains oil phase.Oil phase is sprayed to and is covered with potato starch particle
Fluid bed in adsorb pelletize, obtain the microcapsule that surface is coated by starch.
Temperature is set to 50 DEG C in fluid bed, and spraying adds the sodium hydroxide solution that mass concentration is 40%, makes microcapsule table
There is gelatinizing and saponification in the starch and oils and fatss in face, spraying stays on 40 minutes after terminating in fluid bed, discharges, and obtains simultaneously
Retinyl acetate microcapsule.
The preparation of the retinyl acetate microcapsule of embodiment 4
It is at 60 DEG C, 15 part by weight of vitamin A acetass, 1 weight portion ethoxyquin, the oil mixing of 74 parts by weight Corn is molten
Solution, adding 10 weight portion magnesium carbonate makes it be uniformly dispersed, and obtains oil phase.Oil phase is sprayed to and is covered with potato starch particle
Adsorb pelletize in fluid bed, obtain the microcapsule that surface is coated by starch.
Temperature is set to 50 DEG C in fluid bed, and spraying adds the sodium hydroxide solution that mass concentration is 40%, makes microcapsule table
There is gelatinizing and saponification in the starch and oils and fatss in face, spraying stays on 40 minutes after terminating in fluid bed, discharges, and obtains simultaneously
Retinyl acetate microcapsule.
The preparation of the beta-carotene microcapsule of embodiment 5
At 25 DEG C, by the beta Carotene preparation of 10 weight portion 10%, 0.1 weight portion BHT, 45 wt parts of olive oil, 14.9 weights
Amount part Cera Flava, 30 weight parts of calcium carbonate mixed grindings so as to be uniformly dispersed, obtain dispersion liquid oil phase.Oil phase is sprayed to and is covered with
Adsorb pelletize in the fluid bed of sweet potato starch granule, obtain the microcapsule that surface is coated by starch.
Temperature is set to 40 DEG C in fluid bed, and spraying adds the sodium hydroxide solution that mass concentration is 50%, makes microcapsule table
There is gelatinizing and saponification in the starch and oils and fatss in face, spraying stays on 40 minutes after terminating in fluid bed, discharges, and obtains simultaneously
Stable beta-carotene microcapsule.
The preparation of the Vitamin E of embodiment 6
At 40 DEG C, by 55 part by weight of vitamin E, 5 weight portion TBHQ, 20 parts by weight of soybean oil, 10 weight portion food stage stones
Wax mixed dissolution, adding 10 parts by weight of silica makes it be uniformly dispersed, and obtains oil phase.Oil phase is sprayed to and is covered with Semen Maydiss shallow lake
Adsorb pelletize in the fluid bed of powder particles, obtain the microcapsule that surface is coated by starch.
Temperature is set to 40 DEG C in fluid bed, and spraying adds the potassium hydroxide solution that mass concentration is 10%, makes microcapsule table
There is gelatinizing and saponification in the starch and oils and fatss in face, obtain stable Vitamin E contained micro capsule simultaneously.
The preparation of the astaxanthin microcapsule of embodiment 7
At 25 DEG C, by 5 weight portion astaxanthins, 5 weight portion phylloxanthins, 0.5 weight portion tocopherol, 10 weight portion Oleum Arachidis hypogaeae semen,
38 weight portion Oleum Cocois, 9.5 weight portion Oleum sesami, 22 wt parts Candelilla Wax, 10 parts by weight of phosphoric acid calcium mixed grindings so as to point
Dissipate uniform, obtain dispersion liquid oil phase.Oil phase is sprayed to be covered with the fluid bed of waxy corn starch and wheat starch granule and is adsorbed
Pelletize, obtains the microcapsule that surface is coated by starch.
Temperature is set to 30 DEG C in fluid bed, and spraying adds the sodium hydroxide solution that mass concentration is 35%, makes microcapsule table
There is gelatinizing and saponification in the starch and oils and fatss in face, spraying stays on 35 minutes after terminating in fluid bed, discharges, and obtains simultaneously
Stable astaxanthin microcapsule.
The preparation of the canthaxanthin microcapsule of embodiment 8
At 40 DEG C, the dichloromethane solution of 5 weight portion canthaxanthins is added to containing 3 weight portion BHA, 20 weight portion Petiolus Trachycarpis
In oil, 10 weight portion Oleum Brassicae campestriss, 27 weight portion Testa oryzae oil, the mixed liquor of 20 weight portion behenic acids, separate out canthaxanthin, by solvent
After reclaiming completely, then 15 parts by weight of phosphoric acid magnesium are added, carry out mixed grinding so as to be uniformly dispersed, obtain dispersion liquid oil phase.By oil
Mutually it is sprayed to be covered with the fluid bed of barley starch and naked barley starch granuless and adsorbs pelletize, obtains micro- glue that surface is coated by starch
Capsule.
Temperature is set to 35 DEG C in fluid bed, and spraying adds the sodium hydroxide solution that mass concentration is 40%, makes microcapsule table
There is gelatinizing and saponification in the starch and oils and fatss in face, spraying stays on 45 minutes after terminating in fluid bed, discharges, and obtains simultaneously
Stable canthaxanthin microcapsule.
The preparation of the lycopene microcapsule of embodiment 9
At 50 DEG C, by 20 weight portion lycopenes, 2 weight portion BHT, 5 weight portion Oleum Helianthis, 11 weight portion mineral oil,
50 weight portion Cera Flava mixed dissolutions, adding 11.8 parts by weight of silica makes it be uniformly dispersed, and obtains oil phase.Oil phase is sprayed
Adsorb pelletize to being covered with the fluid bed of sorghum starch granule, obtain the microcapsule that surface is coated by starch.
Temperature is set to 50 DEG C in fluid bed, and spraying adds the potassium hydroxide solution that mass concentration is 35%, makes microcapsule table
There is gelatinizing and saponification in the starch and oils and fatss in face, spraying stays on 43 minutes after terminating in fluid bed, discharges, and obtains simultaneously
Stable lycopene microcapsule.
The preparation of the Vitamin D3 microcapsule of embodiment 10
At 25 DEG C, by 10 part by weight of vitamin D3,1 weight portion astaxanthin, 0.8 weight portion ethoxyquin, 10 weight portions flower
Oil generation, 20 weight portion herring oils, 20.6 weight portion butter, 18 weight portion Cera Flavas, 10 parts by weight of phosphoric acid magnesium mixed grindings so as to point
Dissipate uniform, obtain dispersion liquid oil phase.Oil phase is sprayed to be covered with to adsorb in the fluid bed of bean starch and wheat starch granule and is made
Grain, obtains the microcapsule that surface is coated by starch.
Temperature is set to 50 DEG C in fluid bed, and spraying adds the sodium hydroxide solution that mass concentration is 10%, makes microcapsule table
There is gelatinizing and saponification in the starch and oils and fatss in face, spraying stays on 40 minutes after terminating in fluid bed, discharges, and obtains simultaneously
Stable Vitamin D3 microcapsule.
The preparation of the Xanthophyll micro-capsule of embodiment 11
At 40 DEG C, by the xanthophyll preparation of 14.6 weight portion 10%, 0.5 weight portion tocopherol, 50 weight portion haco oils, 8.7
Weight portion higher fatty acids, 3 weight portion Cera Flavas, 25 weight portion magnesium carbonate mixed grindings so as to be uniformly dispersed, obtain dispersion liquid oil
Phase.Oil phase is sprayed to be covered with the fluid bed of tapioca granule and adsorbs pelletize, obtain the microcapsule that surface is coated by starch.
Temperature is set to 35 DEG C in fluid bed, and spraying adds the potassium hydroxide solution that mass concentration is 40%, makes microcapsule table
There is gelatinizing and saponification in the starch and oils and fatss in face, spraying stays on 46 minutes after terminating in fluid bed, discharges, and obtains simultaneously
Stable Xanthophyll micro-capsule.
The preparation of the vitamin e succinate microcapsule of embodiment 12
At 40 DEG C, the dichloromethane solution of 8 part by weight of vitamin E succinates is added to containing 3 weight portion TBHQ, 15 weights
In amount part Petiolus Trachycarpi oil, 10 weight portion butter, 21 weight portion Adeps Bovis seu Bubali, the mixed liquor of 20 weight portion behenic acids, 15 weight portions are added
Magnesium phosphate, separates out vitamin e succinate, by solvent recovery it is complete after, then add 9 parts by weight of phosphoric acid calcium, carry out mixing and grind
Mill so as to be uniformly dispersed, obtain dispersion liquid oil phase.Oil phase is sprayed to the fluid bed for being covered with sweet potato starch and naked barley starch granuless
Middle absorption pelletize, obtains the microcapsule that surface is coated by starch.
Temperature is set to 30 DEG C in fluid bed, and spraying adds the sodium hydroxide solution that mass concentration is 50%, makes microcapsule table
There is gelatinizing and saponification in the starch and oils and fatss in face, obtain stable vitamin e succinate microcapsule simultaneously.
The preparation of the retinyl acetate microcapsule of comparative example 1
At 60 DEG C, by the melting of 15 part by weight of vitamin A acetass, 85 weight portions containing 1 weight portion ethoxyquin are added drop-wise to
In the aqueous solution of starch sodium octenyl succinate, emulsifying is carried out, in being then sprayed to the fluid bed for being covered with potato starch particle
Absorption pelletize, obtains the Vitamin E contained micro capsule that surface is coated by starch.
The preparation of the lycopene microcapsule of comparative example 2
At 50 DEG C, 20 weight portion lycopenes are dissolved in into 1000 pbw acetones containing 2 weight portion BHT, then Deca
To in the aqueous solution of 80 parts of gelatin, by long-time emulsification pretreatment, acetone is removed completely, form oil-in-water emulsion, most
It is sprayed to afterwards to be covered with the fluid bed of sorghum starch granule and adsorbs pelletize, obtains surface by the micro- glue of lycopene that starch is coated
Capsule.
The retinyl acetate microcapsule product stability test of embodiment 13
The retinyl acetate microcapsule that embodiment 1~4 is prepared carries out stability contrast with comparative example 1, tests
Method is as follows：By two kinds of microcapsules respectively with the additional aluminium foil bag sealing of plastic bag, 40 ± 2 DEG C of temperature, humidity 75% ± 5% are placed in
Stability experiment under the conditions of, under the test period of 1,2,3,6 months detect liquid content (external standard method).As a result it is as follows：
As can be seen from the above table, the stability of the retinyl acetate microcapsule that embodiment 1-4 is prepared is better than contrast
The retinyl acetate microcapsule that the conventional method of example 1 is prepared.
Retinyl acetate microcapsule product stability test in the tablet of embodiment 14
The retinyl acetate microcapsule that embodiment 1~4 and comparative example 1 are prepared is respectively adopted into same method
Processing obtains corresponding tablet, and the addition of microcapsule product is 15ug/g, then carries out stability contrast to two kinds of tablets,
Method of testing is as follows：Two kinds of tablets are sealed respectively with paper bag, 40 ± 2 DEG C of temperature, the stability reality of humidity 75% ± 5% is placed in
Under the conditions of testing, liquid content (external standard method) is detected under the test period of 1,2,3,6 months.As a result it is as follows：
As can be seen from the above table, in tablets the stability of the retinyl acetate tablet of embodiment 1-4 also superior to contrast
Example 1.
The lycopene microcapsule product stability of embodiment 15 is tested
The lycopene microcapsule that embodiment 9 is prepared carries out stability contrast with comparative example 2, and method of testing is such as
Under：By two kinds of microcapsules respectively with the sealing of plastic bag additional aluminium foil bag, it is placed in 40 ± 2 DEG C of temperature, humidity 75% ± 5% is stablized
Property experiment condition under, under the test period of 1,2,3,6 months detect liquid content (external standard method).As a result it is as follows：
As can be seen from the above table, the stability of the lycopene microcapsule of embodiment 9 is better than comparative example 2.
Lycopene microcapsule product stability test in the tablet of embodiment 16
The lycopene microcapsule that embodiment 9 is prepared is respectively adopted same method processing and obtains with comparative example 2
Corresponding tablet, the addition of microcapsule product is 300 μ g/g, then carries out stability contrast, test side to two kinds of tablets
Method is as follows：Two kinds of tablets are sealed respectively with paper bag, 40 ± 2 DEG C of temperature, the stability experiment condition of humidity 75% ± 5% is placed in
Under, liquid content (external standard method) is detected under the test period of 1,2,3,6 months.As a result it is as follows：
As can be seen from the above table, in tablets the stability of the lycopene tablet of embodiment 9 is better than comparative example 2.
Claims (10)
1. a kind of preparation method of stable fat soluble nutrient microcapsule, it is characterised in that comprise the steps：
1) oil phase containing ore materials is carried out into fluidized bed spray granulation, forms the microcapsule that surface is coated by starch grain；
2) baking temperature is warming up to, the spraying in fluid bed adds aqueous slkali, the starch and oils and fatss for making surface of microcapsule is sent out simultaneously
Raw gelatinizing and saponification, form fine and close protecting film, obtain stable fat soluble nutrient microcapsule；
Described oil phase is the fat solution comprising the ore materials, fat soluble nutrient and antioxidant or oils and fatss dispersion
Liquid.
2. preparation method according to claim 1, it is characterised in that described fat soluble nutrient is beta-carotene, shrimp
Blue or green element, lycopene, canthaxanthin, phylloxanthin, vitamin D3, retinyl acetate, Vitamin E, in vitamin e derivative
One or more；Mass ratio of the described fat soluble nutrient in oil phase is 1~60%；
Described antioxidant is one or more in tocopherol, ethoxyquin, BHT, BHA or TBHQ；Described antioxidation
Mass ratio of the agent in oil phase is 0.1~5%.
3. preparation method according to claim 1, it is characterised in that the oils and fatss in the oil phase be soybean oil, Semen Maydis oil,
Oleum Arachidis hypogaeae semen, Oleum Cocois, Oleum sesami, olive oil, Petiolus Trachycarpi oil, Oleum Brassicae campestriss, Testa oryzae oil, Oleum Helianthi, cupu oil, butter, Adeps Sus domestica, cattle
One or more in oil, herring oil, pilchard oil, haco oil, mineral oil；
Described ore materials are one or more in silicon dioxide, Calcium Carbonate, calcium phosphate, magnesium carbonate or magnesium phosphate, Ore
Mass ratio of the material in oil phase is 10~30%.
4. preparation method according to claim 1, it is characterised in that described baking temperature is 30~50 DEG C.
5. preparation method according to claim 1, it is characterised in that described starch be potato starch, corn starch,
It is waxy corn starch, wheaten starch, barley starch, naked barley starch, rice starch, sorghum starch, sweet potato starch, tapioca, red
One or more in sweet potato starch or bean starch.
6. preparation method according to claim 1, it is characterised in that described alkali liquor is 10~50% for mass concentration
The aqueous solution of sodium hydroxide or potassium hydroxide.
7. the preparation method according to any one of claim 1~6, it is characterised in that Gao Rong is also included in described oil phase
Point component；
Described high melting point component be preferably freezing point more than the one kind in 30 DEG C of wax, fixed oil/fat, higher fatty acids or
Various, the mass ratio of described high melting point component in oil phase is 30~70%.
8. the fat soluble nutrient microcapsule that a kind of preparation method as described in any one of claim 1~7 is obtained.
9. a kind of application of fat soluble nutrient microcapsule as claimed in claim 8, it is characterised in that described fat-soluble battalion
Supporting element microcapsule is used to be processed into other dosage forms；
Other described dosage forms are preferably tablet.
10. a kind of feedstuff, food or health product, it is characterised in that comprising microcapsule or claim described in claim 8
Other dosage forms described in 9 are used as additive.
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| CN107811298A (en) * | 2017-12-01 | 2018-03-20 | 浙江新和成股份有限公司 | A kind of water-soluble nutrients microcapsules and preparation method thereof |
| CN108813527A (en) * | 2018-04-11 | 2018-11-16 | 华南理工大学 | A kind of flavouring of astaxanthin-containing and preparation method thereof |
| CN109517080A (en) * | 2018-11-06 | 2019-03-26 | 浙江大学 | Starch octenyl succinate anhydride, fat soluble nutrient microcapsules and preparation method and application |
| CN109700025A (en) * | 2018-12-14 | 2019-05-03 | 晨光生物科技集团股份有限公司 | A kind of preparation method and its oil suspending agent of lycopene oil suspending agent |
| CN110810848A (en) * | 2019-12-03 | 2020-02-21 | 东北农业大学 | Preparation method of microcapsule with high vitamin E utilization rate |
| CN114468175A (en) * | 2022-02-28 | 2022-05-13 | 山东阜力康动物营养有限公司 | Laying hen vitamin premixed feed and preparation method thereof |
| CN114948772A (en) * | 2022-04-29 | 2022-08-30 | 可莱尼化妆品科技有限公司 | Astaxanthin nanocapsule and preparation method and application thereof |
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| CN107594597B (en) * | 2017-07-31 | 2020-05-12 | 浙江新和成股份有限公司 | Fat-soluble nutrient microcapsule and preparation method thereof |
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| CN110810848A (en) * | 2019-12-03 | 2020-02-21 | 东北农业大学 | Preparation method of microcapsule with high vitamin E utilization rate |
| CN114468175A (en) * | 2022-02-28 | 2022-05-13 | 山东阜力康动物营养有限公司 | Laying hen vitamin premixed feed and preparation method thereof |
| CN114948772A (en) * | 2022-04-29 | 2022-08-30 | 可莱尼化妆品科技有限公司 | Astaxanthin nanocapsule and preparation method and application thereof |
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Effective date of registration: 20190128 Address after: 312500 West Road 418 Qixing Street, Xinchang County, Shaoxing City, Zhejiang Province Applicant after: Zhejiang Xinhecheng Co., Ltd. Applicant after: Ningbo University of Technology Address before: 312500 Xinchang provincial high tech Industrial Park, Xinchang, Shaoxing, China (Mei Zhu) Applicant before: Zhejiang Xinweipu Additive Co.,Ltd. Applicant before: Zhejiang Xinhecheng Co., Ltd. Applicant before: Ningbo University of Technology |
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Effective date of registration: 20200819 Address after: 312500, No. 418, West Avenue, Qixing street, Xinchang County, Shaoxing, Zhejiang Co-patentee after: Ningbo University of Technology Patentee after: ZHEJIANG NHU Co.,Ltd. Co-patentee after: Xinchang XinHeCheng vitamin Co., Ltd Address before: No. 418, West Road, Qixing street, Xinchang County, Shaoxing City, Zhejiang Province Co-patentee before: Ningbo University of Technology Patentee before: ZHEJIANG NHU Co.,Ltd. |