CN105434402A - Sustained-release microcapsule with optimized release property - Google Patents
Sustained-release microcapsule with optimized release property Download PDFInfo
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- CN105434402A CN105434402A CN201511018988.5A CN201511018988A CN105434402A CN 105434402 A CN105434402 A CN 105434402A CN 201511018988 A CN201511018988 A CN 201511018988A CN 105434402 A CN105434402 A CN 105434402A
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- slow
- release
- core
- releasing microcapsule
- sustained
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- 238000013268 sustained release Methods 0.000 title abstract 8
- 239000012730 sustained-release form Substances 0.000 title abstract 8
- 239000000463 material Substances 0.000 claims abstract description 46
- 239000000203 mixture Substances 0.000 claims abstract description 28
- 150000003904 phospholipids Chemical class 0.000 claims abstract description 21
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 18
- 150000001413 amino acids Chemical class 0.000 claims abstract description 10
- 229930003231 vitamin Natural products 0.000 claims abstract description 9
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- 239000011782 vitamin Substances 0.000 claims abstract description 9
- 229940088594 vitamin Drugs 0.000 claims abstract description 9
- 150000003722 vitamin derivatives Chemical class 0.000 claims abstract description 9
- 239000008172 hydrogenated vegetable oil Substances 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 230000003578 releasing effect Effects 0.000 claims description 41
- 238000000034 method Methods 0.000 claims description 36
- UCMIRNVEIXFBKS-UHFFFAOYSA-N beta-alanine Chemical group NCCC(O)=O UCMIRNVEIXFBKS-UHFFFAOYSA-N 0.000 claims description 30
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- 238000000576 coating method Methods 0.000 claims description 18
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- WTJKGGKOPKCXLL-RRHRGVEJSA-N phosphatidylcholine Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@H](COP([O-])(=O)OCC[N+](C)(C)C)OC(=O)CCCCCCCC=CCCCCCCCC WTJKGGKOPKCXLL-RRHRGVEJSA-N 0.000 claims description 10
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- 238000001816 cooling Methods 0.000 claims description 6
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- PHIQHXFUZVPYII-ZCFIWIBFSA-N (R)-carnitine Chemical compound C[N+](C)(C)C[C@H](O)CC([O-])=O PHIQHXFUZVPYII-ZCFIWIBFSA-N 0.000 claims description 2
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 claims description 2
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- JLPULHDHAOZNQI-ZTIMHPMXSA-N 1-hexadecanoyl-2-(9Z,12Z-octadecadienoyl)-sn-glycero-3-phosphocholine Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@H](COP([O-])(=O)OCC[N+](C)(C)C)OC(=O)CCCCCCC\C=C/C\C=C/CCCCC JLPULHDHAOZNQI-ZTIMHPMXSA-N 0.000 description 2
- PZNPLUBHRSSFHT-RRHRGVEJSA-N 1-hexadecanoyl-2-octadecanoyl-sn-glycero-3-phosphocholine Chemical compound CCCCCCCCCCCCCCCCCC(=O)O[C@@H](COP([O-])(=O)OCC[N+](C)(C)C)COC(=O)CCCCCCCCCCCCCCC PZNPLUBHRSSFHT-RRHRGVEJSA-N 0.000 description 2
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- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- ODKSFYDXXFIFQN-BYPYZUCNSA-N L-arginine Chemical compound OC(=O)[C@@H](N)CCCN=C(N)N ODKSFYDXXFIFQN-BYPYZUCNSA-N 0.000 description 2
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- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 description 1
- IIZPXYDJLKNOIY-JXPKJXOSSA-N 1-palmitoyl-2-arachidonoyl-sn-glycero-3-phosphocholine Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@H](COP([O-])(=O)OCC[N+](C)(C)C)OC(=O)CCC\C=C/C\C=C/C\C=C/C\C=C/CCCCC IIZPXYDJLKNOIY-JXPKJXOSSA-N 0.000 description 1
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- 239000001856 Ethyl cellulose Substances 0.000 description 1
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 description 1
- 108010010803 Gelatin Proteins 0.000 description 1
- 241001597008 Nomeidae Species 0.000 description 1
- 108010073771 Soybean Proteins Proteins 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 229930003270 Vitamin B Chemical group 0.000 description 1
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- 239000001785 acacia senegal l. willd gum Substances 0.000 description 1
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- 238000009835 boiling Methods 0.000 description 1
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- 239000002775 capsule Substances 0.000 description 1
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- 229920001525 carrageenan Polymers 0.000 description 1
- 229940113118 carrageenan Drugs 0.000 description 1
- 239000005018 casein Substances 0.000 description 1
- BECPQYXYKAMYBN-UHFFFAOYSA-N casein, tech. Chemical compound NCCCCC(C(O)=O)N=C(O)C(CC(O)=O)N=C(O)C(CCC(O)=N)N=C(O)C(CC(C)C)N=C(O)C(CCC(O)=O)N=C(O)C(CC(O)=O)N=C(O)C(CCC(O)=O)N=C(O)C(C(C)O)N=C(O)C(CCC(O)=N)N=C(O)C(CCC(O)=N)N=C(O)C(CCC(O)=N)N=C(O)C(CCC(O)=O)N=C(O)C(CCC(O)=O)N=C(O)C(COP(O)(O)=O)N=C(O)C(CCC(O)=N)N=C(O)C(N)CC1=CC=CC=C1 BECPQYXYKAMYBN-UHFFFAOYSA-N 0.000 description 1
- 235000021240 caseins Nutrition 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
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- 229920006184 cellulose methylcellulose Polymers 0.000 description 1
- 239000007766 cera flava Substances 0.000 description 1
- 238000013270 controlled release Methods 0.000 description 1
- MPVXINJRXRIDDB-VCDGYCQFSA-N dodecanoic acid;(2r,3r,4r,5s)-hexane-1,2,3,4,5,6-hexol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO.CCCCCCCCCCCC(O)=O MPVXINJRXRIDDB-VCDGYCQFSA-N 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
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- 239000003995 emulsifying agent Substances 0.000 description 1
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- 239000000706 filtrate Substances 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000008273 gelatin Substances 0.000 description 1
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- 239000008187 granular material Substances 0.000 description 1
- 235000010445 lecithin Nutrition 0.000 description 1
- 239000000787 lecithin Substances 0.000 description 1
- 229940067606 lecithin Drugs 0.000 description 1
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- 229920000609 methyl cellulose Polymers 0.000 description 1
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- 235000015112 vegetable and seed oil Nutrition 0.000 description 1
- 239000008158 vegetable oil Substances 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000001993 wax Substances 0.000 description 1
- -1 wet granulation Substances 0.000 description 1
- UHVMMEOXYDMDKI-JKYCWFKZSA-L zinc;1-(5-cyanopyridin-2-yl)-3-[(1s,2s)-2-(6-fluoro-2-hydroxy-3-propanoylphenyl)cyclopropyl]urea;diacetate Chemical compound [Zn+2].CC([O-])=O.CC([O-])=O.CCC(=O)C1=CC=C(F)C([C@H]2[C@H](C2)NC(=O)NC=2N=CC(=CC=2)C#N)=C1O UHVMMEOXYDMDKI-JKYCWFKZSA-L 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/48—Preparations in capsules, e.g. of gelatin, of chocolate
- A61K9/50—Microcapsules 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
- A61K9/5005—Wall or coating material
- A61K9/5015—Organic compounds, e.g. fats, sugars
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/185—Acids; Anhydrides, halides or salts thereof, e.g. sulfur acids, imidic, hydrazonic or hydroximic acids
- A61K31/19—Carboxylic acids, e.g. valproic acid
- A61K31/195—Carboxylic acids, e.g. valproic acid having an amino group
- A61K31/197—Carboxylic acids, e.g. valproic acid having an amino group the amino and the carboxyl groups being attached to the same acyclic carbon chain, e.g. gamma-aminobutyric acid [GABA], beta-alanine, epsilon-aminocaproic acid or pantothenic acid
- A61K31/198—Alpha-amino acids, e.g. alanine or edetic acid [EDTA]
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/33—Heterocyclic compounds
- A61K31/395—Heterocyclic compounds having nitrogen as a ring hetero atom, e.g. guanethidine or rifamycins
- A61K31/435—Heterocyclic compounds having nitrogen as a ring hetero atom, e.g. guanethidine or rifamycins having six-membered rings with one nitrogen as the only ring hetero atom
- A61K31/44—Non condensed pyridines; Hydrogenated derivatives thereof
- A61K31/455—Nicotinic acids, e.g. niacin; Derivatives thereof, e.g. esters, amides
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
- A61K47/06—Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite
- A61K47/24—Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite containing atoms other than carbon, hydrogen, oxygen, halogen, nitrogen or sulfur, e.g. cyclomethicone or phospholipids
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/0002—Galenical forms characterised by the drug release technique; Application systems commanded by energy
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/48—Preparations in capsules, e.g. of gelatin, of chocolate
- A61K9/50—Microcapsules 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
- A61K9/5089—Processes
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- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Public Health (AREA)
- Medicinal Chemistry (AREA)
- Pharmacology & Pharmacy (AREA)
- Epidemiology (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Veterinary Medicine (AREA)
- Engineering & Computer Science (AREA)
- Bioinformatics & Cheminformatics (AREA)
- Biophysics (AREA)
- Molecular Biology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Medicinal Preparation (AREA)
- General Preparation And Processing Of Foods (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
The invention provides a sustained-release microcapsule with an optimized release property. The sustained-release microcapsule is prepared from the raw materials of a core material, a wall material and an auxiliary agent, and characterized in that the wall material is selected from hydrogenated vegetable oil; the auxiliary agent comprises phospholipid; a mixture of the wall material and the auxiliary agent serves as a release material. The sustained-release microcapsule provided by the invention has an excellent sustained-release effect and the dissolution rate of the core material is improved, so as to promote release of the core material, optimize the release dynamics, and achieve a continuous release effect. In addition, through addition of the special auxiliary agent, the wetting property and water dispersibility of the sustained-release microcapsule can be improved, so that the sustained-release microcapsule technology can well solve the problems that such poor properties as instability, high possibility of moisture absorption and bad smells are caused when an amino acid, a vitamin or other materials are applied to the core material, and the obtained sustained-release microcapsule, namely a basic sustained-release preparation, can be applied to foods, functional foods, dietary supplements and beverages.
Description
Technical field
The invention belongs to microencapsulation field, particularly relate to the microcapsule product of performance optimization.
Background technology
The slow releasing preparation product made by microcapsule technology, except the characteristic that can obtain stable, moistureproof, taste masking, controlled release, almost consistent with raw material on particle diameter, can solid beverage be made, or directly be added in liquid, make it be more conducive to absorption and eat.In addition, also tablet or capsule can be made neatly.Usual slow releasing preparation is little compared with ordinary preparation drug administration amount; take be easier to for making slow releasing tablet most medicine; but for the nutrient substance that some taking doses are large; as aminoacid, plant extract etc.; larger tablet and more taking dose reduce compliance, and people are more ready to be made into powder or the granule that can take after mixing it with water or can be made into suspension.
The method of microencapsulation has a lot, and conventional method comprises fluidized coating, wet granulation, spray congealing etc.Fluidized coating is suspended in high velocity air by core material particles, being atomized and being coated to particle surface, by dry or solidification, forming the clothing film of definite composition and thickness at particle surface by there being the coating solution of slow-releasing and controlled-releasing action.Wet granulation is mixed under high-speed stirred condition with coating solution core material particles, and then dry the method except desolventizing or cooling curing.Spray congealing is dissolved by core or is dispersed in the fat of fusing, and form droplet through atomization and fall into cooling chamber, fat solidifies formation fine particle.Described several formulation methods are each has something to recommend him, need to select optimal method according to preparation system.
In addition, encapsulating material is also the key factor determining microcapsule formulation quality.Encapsulating material should have certain intensity, and rub resistance, anti-extrusion, the performance such as heat-resisting, can not react with core, and therefore most encapsulating material is macromolecular material that is natural or synthesis.Main species has plant gum, as arabic gum, sodium alginate, carrageenan agar etc.; Next is starch and derivant thereof, as various types of Hu Jing, oligosaccharide; In addition gelatin, casein, soybean protein, multiple cellulose derivative (CMC, ethyl cellulose, methylcellulose etc.), wax (paraffin, Cera Flava etc.) is also had also to be all good encapsulating material.
Phospholipid is the phospholipid extracted from vegetable oil, comprises concentrated phosphatide, powder phospholipid (deoiled phosphatides), lecithin and through structurally-modified above-mentioned phospholipid.In microencapsulated formulation, phospholipid, due to the character of its " parents ", how as emulsifying agent and surfactant, regulates the water oil balance of emulsion.
Summary of the invention
The object of this invention is to provide a kind of slow-releasing microcapsule of performance optimization, described slow-releasing microcapsule is prepared by raw material by core, wall material and auxiliary agent, and wherein said wall material is selected from hydrogenated vegetable oil; Described auxiliary agent comprises phospholipid; The mixture of wall material and auxiliary agent is as releasable material.
The present invention's object on the other hand, be the preparation method of the slow-releasing microcapsule providing above-mentioned optimization to discharge, described method is phospholipid as the application of short releasable material in microcapsule preparation, and its feature is just to prepare in the process of microcapsule, and use hydrogenated vegetable oil is wall material; In releasable material, add phospholipid simultaneously.
Above-mentioned slow-releasing microcapsule of the present invention has excellent slow release effect, improves the dissolution rate of core, thus promotes the release of core, and optimizes release dynamics, forms the effect of constant release.In addition, the interpolation of special auxiliary agent also increases wettability and the water dispersible of product.Therefore, slow-releasing microcapsule technology of the present invention is used to can be good at the undesirable property brought by raw material when solving the application of the core such as aminoacid or vitamin, as unstable, the easy moisture absorption, abnormal smells from the patient difference etc., gained basis slow releasing preparation can be applicable in food, functional food, dietary supplement and beverage.
Detailed description of the invention
The present invention comes from phospholipid in the understanding optimizing the novelty teabag in microencapsulated formulation release dynamics.Specifically, be that phospholipid is promoting the application in microcapsule release.
The result of above-mentioned application, the slow-releasing microcapsule that the present invention is provided a kind of release performance more superior, described slow-releasing microcapsule is prepared by raw material by core, wall material and auxiliary agent, and described wall material is selected from hydrogenated vegetable oil; Described auxiliary agent comprises phospholipid; The mixture of wall material and auxiliary agent is as releasable material.
In slow-releasing microcapsule of the present invention, the quality of described phospholipid is 0.5 ~ 10% of wall material amount.Preferably 1 ~ 6%, more preferably 2 ~ 5%.The selection of phospholipid, based on the common standard of this area, the mass ratio of preferred phosphatidylcholine (PC), phosphatidylinositols (PI) and PHOSPHATIDYL ETHANOLAMINE (PE) is the phospholipid prod of 1.8 ~ 2.5:0.9 ~ 1.1:1.2 ~ 2.0.The phospholipid prod of acetone insoluble matter >=55% also more preferably uses.
In slow-releasing microcapsule of the present invention, described wall material is the mixture that hydrogenated palm oil or itself and other hydrogenated vegetable oil form.The mass percentage of preferred hydrogenated palm oil is not less than the mixture of 60%.Wherein, other described hydrogenated vegetable oil is preferably selected from oil with hydrogenated soybean, hydrogenated sunflower oil, hydrogenated groundnut, cotmar, hydrogenated corn oil, and wherein 2 kinds or two or more mixture according to arbitrary proportion.
In slow-releasing microcapsule of the present invention, described core is selected from aminoacid or vitamin.Be preferably selected from Beta-alanine, α-alanine, arginine, L-carnitine, vitamin C and vitamin B group.Most preferably Beta-alanine.
Slow-releasing microcapsule of the present invention can adopt conventional method well-known to those skilled in the art, and these methods can be illustrated but are not limited to air suspension fluidized bed coating (Wurster), spraying dry, efficient wet granulation etc.
With the use of following several concrete slow-releasing microcapsule preparation method for illustration of these formulation methods.
One of embodiment, a kind of method preparing slow-releasing microcapsule acid supplement is the core (preferred Beta-alanine) that will pulverize, and is dispersed in the releasable material that heat melts; Atomization; Cooling.
Embodiment two, a kind of method preparing slow-releasing microcapsule chemical preparation first releasable material heat is melted, and be in molten condition to be atomized smoothly before ensureing atomization, adopts top spray or end pressure spray process, carry out coating to core in fluid bed.
Described top spray technique is: inlet temperature 45 ~ 73 DEG C, and air quantity 20 ~ 50m3/h makes Beta-alanine be in good fluidized state, atomizing pressure 0.1 ~ 0.3MPa, flow velocity 3 ~ 20ml/min, and in order to prevent adhesion, flow velocity progressively will be increased to proper level.
Pressure spray process of the described end is: inlet temperature 45 ~ 73 DEG C, air quantity 20 ~ 50m3/h, regulate mozzle lower end and distribution grid spacing, Beta-alanine is made to be in good fluidized state, atomizing pressure 0.1 ~ 0.3MPa, flow velocity 3 ~ 20ml/min, in order to prevent adhesion, flow velocity progressively will be increased to proper level.
Embodiment three, a kind of method preparing slow-releasing microcapsule chemical preparation, comprises the steps:
Releasable material and core are placed in the high speed agitator being furnished with jacket heat-preservation system, are warming up to 45 ~ 73 DEG C, and stir with 1000 ~ 2000RPM rotating speed, and the releasable material of fusing is coated on core surfaces with what stir, reduce rotating speed and lower the temperature, cooling curing.
Slow-releasing microcapsule of the present invention, prepares preferably by following method, and meanwhile, the method also can be understood as the optimal technical scheme of slow-releasing microcapsule preparation method of the present invention, comprises the steps:
(1) heat melts wall material, and heat stirs under melting temperature and adds auxiliary agent, Homogeneous phase mixing; Then by gained mixture rapid drawdown temperature to 0 ~ 5 DEG C, and mixture is made to keep at least 24 hours at such a temperature;
(2) heat melts the mixture of step (1) gained, with it for releasable material prepares slow-releasing microcapsule.
More specifically, the preparation method of described slow-releasing microcapsule comprises the steps:
(1) heat melts wall material, and heat stirs under melting temperature and adds auxiliary agent, Homogeneous phase mixing; Then by mixture rapid drawdown temperature to 0 ~ 5 DEG C, and mixture is made to keep at least 24 hours at such a temperature;
(2) heat melts the mixture of step (1) gained, with it for releasable material prepares slow-releasing microcapsule;
(3) core (aminoacid or vitamin) is crushed to 100 ~ 120 orders, and prepares slow-releasing microcapsule with one of following step:
A. the core after pulverizing is dispersed in the releasable material that heat melts, atomization, cooling;
B. by the aminoacid of pulverizing or vitamin, adopt top spray technique fluidized bed coating, described top spray technique is: inlet temperature 45 ~ 73 DEG C, air quantity 20 ~ 50m
3/ h, makes core (aminoacid or vitamin) be in good fluidized state, atomizing pressure 0.1 ~ 0.3MPa, flow velocity 3 ~ 20ml/min.In order to prevent adhesion, flow velocity is progressively increased to proper level;
C. by the aminoacid of pulverizing or vitamin, adopt end pressure spray process fluidized bed coating, pressure spray process of the described end is: inlet temperature 45 ~ 73 DEG C, air quantity 20 ~ 50m
3/ h, regulates mozzle lower end and distribution grid spacing, makes core (aminoacid or vitamin) be in good fluidized state, atomizing pressure 0.1 ~ 0.3MPa, flow velocity 7 ~ 25ml/min.In order to prevent adhesion, flow velocity is progressively increased to proper level.
The heat that in the present invention, many places are addressed is melted, and according to the usual understanding of this area, is solid-state material, as wall material, becomes molten condition under namely making room temperature by heating.Required temperature can set according to the fusing point of concrete material, and those skilled in the art should select without doubt and implement.
In addition, in the present invention, have more addressed rapid drawdown temperature, conventional temperature method of controlling can be used, make the ambient temperature residing for mixture remain on temperature required scope.In detailed description of the invention, mixture heat being melted gained at temperature, as in 0-5 DEG C of refrigerator-freezer, is placed more than 24 hours.
With following non-limiting example, the present invention will be further described, so that the present invention of those of ordinary skill in the art's comprehend, but should not be construed as any type of restriction of the present invention.If no special instructions, the measuring method of following parameter is adopted in the application.
Release of the present invention, its assay method is: USP < 711 > DISSOLUTIO, adopt Apparatus2, rotating speed 50rpm, carries out 0.1N hydrochloric acid solution by DELAYED-RELEASEDOSAGEFORMS method B and tests with the release in pH6.8 phosphate buffer.
The assay method of surface active ingredient of the present invention is: 5g microcapsule product to be measured joins in conical flask, add 50ml pure water wherein, turn after shaking 20s and filter, repeated washing once, merging filtrate, revolve steaming and remove pure water, the dry weight of remaining solid and the mass ratio of microcapsule product to be measured are the content of surface active ingredient, represent with percentage ratio.
Embodiment 1
By 450 hydrogenated palm oil heating and meltings, after 1400gL-arginine is pulverized, be placed in fluid bed and adopt top spray technique to carry out coating.Fluid bed inlet temperature 45 DEG C, air quantity 50m
3/ h, atomizing pressure 0.1MPa, flow velocity 3ml/min, operating time 120min, obtain slow release product A, its L-essence ammonia histidine content is 75.8%, and its surface active ingredient content is 9.0%, and its release of the 1st, 2,3,4,5,6,8 hour (pH6.8 phosphate buffer) is respectively 13.1%, 20.3%, 25.2%, 29.2%, 33.1%, 37.9% and 40.2%.
Embodiment 2
By 400g hydrogenated palm oil, 100g oil with hydrogenated soybean, 2.5g concentrated phosphatide (content ratio of PC, PI, PE is 1.8:0.9:1.9) heating and melting, abrupt temperature drop to 4 DEG C, for subsequent use after keeping 24h, after 1400gL-arginine is pulverized, be placed in fluid bed and adopt top spray technique to carry out coating.Fluid bed inlet temperature 73 DEG C, air quantity 20m
3/ h, atomizing pressure 0.3MPa, flow velocity 20ml/min, operating time 120min, obtain slow release product B, its L-essence ammonia histidine content is 72.2%, and its surface active ingredient content is 11.5%, and its release of the 1st, 2,3,4,5,6,8 hour (pH6.8 phosphate buffer) is respectively 25.5%, 45.9%, 60.8%, 72.1%, 77.2%, 80.7% and 87.4%.
Embodiment 3
By 300g hydrogenated palm oil, 200g hydrogenated corn oil, 25g soybean phospholipid (content ratio of PC, PI, PE is 2.5:1.1:2.0) heating and melting, by 1400g Beta-alanine, is placed in fluid bed and adopts top spray technique to carry out coating.Fluid bed inlet temperature 55 DEG C, air quantity 40m
3/ h, atomizing pressure 0.2MPa, flow velocity 12ml/min, operating time 120min, obtain slow release product C, its Beta-alanine content is 73.2%, and its surface active ingredient content is 14.5%, and its release of the 1st, 2,3,4,5,6,8 hour (pH6.8 phosphate buffer) is respectively 33.2%, 55.1%, 64.8%, 70.1%, 75.9%, 80.7% and 84.7%.
Embodiment 4
By 420g hydrogenated palm oil, 80g hydrogenated sunflower oil, 10g sunflower phospholipid (content ratio of PC, PI, PE is 2:1.1:1.2) heating and melting, abrupt temperature drop to 3 DEG C, for subsequent use after keeping 24h, after 1400g Beta-alanine is pulverized, be placed in fluid bed and adopt end pressure spray process to carry out coating.Fluid bed inlet temperature 73 DEG C, air quantity 20m
3/ h, atomizing pressure 0.2MPa, flow velocity 10ml/min, operating time 120min, obtain slow release product D, its Beta-alanine content is 71.9%, and its surface active ingredient content is 16.2%, and its release of the 1st, 2,3,4,5,6,8 hour (pH6.8 phosphate buffer) is respectively 42.7%, 59.9%, 65.1%, 72.2%, 76.3%, 88.0% and 90.6%.
Embodiment 5
By 450g hydrogenated palm oil, 50g cotmar, 50g Powdered Soy Lecithin (content ratio of PC, PI, PE is 2.1:1:2.1) heating and melting, abrupt temperature drop to 5 DEG C, for subsequent use after keeping 24h, 820g Beta-alanine is placed in fluid bed and adopts top spray technique to carry out coating.Fluid bed inlet temperature 58 DEG C, air quantity 19m
3/ h, atomizing pressure 0.3MPa, flow velocity 20ml/min, operating time 120min, obtain slow release product E, its Beta-alanine content is 61.2%, and its surface active ingredient content is 13.8%, and its release of the 1st, 2,3,4,5,6,8 hour (pH6.8 phosphate buffer) is respectively 27.2%, 42.9%, 59.2%, 70.1%, 73.9%, 78.2% and 84.6%.
Embodiment 6
By 450g hydrogenated palm oil, 50g hydrogenated sunflower oil, 30g soybean phospholipid (content ratio of PC, PI, PE is 2.0:1:2.1) heating and melting, abrupt temperature drop to 4 DEG C, for subsequent use after keeping 24h, 900g Beta-alanine is placed in fluid bed and adopts top spray technique to carry out coating.Fluid bed inlet temperature 56 DEG C, air quantity 17m
3/ h, atomizing pressure 0.2MPa, flow velocity 15ml/min, operating time 110min, obtain slow release product F, its Beta-alanine content is 63.2%, and its surface active ingredient content is 14.6%, and its release of the 1st, 2,3,4,5,6,8 hour (pH6.8 phosphate buffer) is respectively 28.7%, 44.9%, 57.5%, 69.3%, 73.5%, 77.8% and 83.9%.
Embodiment 7
By 325g hydrogenated palm oil, 175g hydrogenated groundnut, 75g Powdered Soy Lecithin (content ratio of PC, PI, PE is 2.2:1.1:1.5) heating and melting, abrupt temperature drop to 5 DEG C, for subsequent use after keeping 24h, the L-arginine that 1350g pulverizes is placed in fluid bed and adopts end pressure spray process to carry out coating.Fluid bed inlet temperature 45 DEG C, air quantity 50m
3/ h, atomizing pressure 0.1MPa, flow velocity 3ml/min, operating time 120min, obtain slow release product G, its L-arginine content is 70.8%, and its surface active ingredient content is 20.0%, and 1, the release (pH6.8 phosphate buffer) of 2 and 3 hours is respectively 40.2%, 70.5% and 100%.
Embodiment 8
By 325g hydrogenated palm oil, 100g hydrogenated corn oil, 75g cotmar, 20g anhydrous sorbitol laurate heating and melting, abrupt temperature drop to 5 DEG C, for subsequent use after keeping 24h, 1350g vitamin B3 is placed in fluid bed and adopts end pressure spray process to carry out coating.Fluid bed inlet temperature 55 DEG C, air quantity 38m
3/ h, atomizing pressure 0.3MPa, flow velocity 20ml/min, operating time 120min, obtain slow release product H, its vitamin B3 content is 69.9%, and its surface active ingredient content is 9.8%, and its release of the 1st, 2,3,4,5,6,8 hour (pH6.8 phosphate buffer) is respectively 13.9%, 21.8%, 30.5%, 34.9%, 37.8%, 40.2% and 43.7%.
Embodiment 9
By 500g hydrogenated corn oil, 5g sunflower powder phospholipid (content ratio of PC, PI, PE is 2.2:1:2.0) heating and melting, abrupt temperature drop to 5 DEG C, for subsequent use after keeping 24h, 1400g vitamin B3 is placed in above-mentioned solution be stirred to formed stablize homogeneous phase solution, and by atomizer spray be the microcapsule forming bead in the cold air of 10 degrees Celsius to temperature by mixture, air quantity 260m
3/ h, atomizing pressure 0.2MPa, flow velocity 10ml/min, beadlet is detained boiling in cold air, operating time, 20min was to free flowing powder, obtained slow release product I, the content 72.5% of its ascorbic acid, its surface active ingredient content is 17.5%, and its release of the 1st, 2,3,4,5,6,8 hour (pH6.8 buffer) is respectively 30.2%, 40.9%, 49.1%, 55.3%, 59.3%, 62.5% and 68.6%.
Claims (10)
1. optimize the slow-releasing microcapsule of release, be prepared by raw material by core, wall material and auxiliary agent, it is characterized in that, described wall material is selected from hydrogenated vegetable oil; Described auxiliary agent comprises phospholipid; The mixture of wall material and auxiliary agent is as releasable material.
2. slow-releasing microcapsule according to claim 1, is characterized in that, the quality of described phospholipid is 0.5 ~ 10% of wall material amount.
3. slow-releasing microcapsule according to claim 1, is characterized in that, in described phospholipid, the mass ratio of phosphatidylcholine, phosphatidylinositols, PHOSPHATIDYL ETHANOLAMINE is 1.8 ~ 2.5:0.9 ~ 1.1:1.2 ~ 2.0.
4. slow-releasing microcapsule according to claim 1, is characterized in that, described wall material is the mixture that hydrogenated palm oil or itself and other hydrogenated vegetable oil form.
5. slow-releasing microcapsule according to claim 4, is characterized in that, in described mixture, the mass percentage of hydrogenated palm oil is not less than 60%.
6. slow-releasing microcapsule according to claim 1, is characterized in that, described core is selected from aminoacid or vitamin.
7. slow-releasing microcapsule according to claim 6, is characterized in that, described core is selected from Beta-alanine, α-alanine, arginine, L-carnitine, vitamin C and vitamin B complex.
8. slow-releasing microcapsule according to claim 7, is characterized in that, described core is Beta-alanine.
9. slow-releasing microcapsule according to claim 1, prepared by following method:
(1) heat melts wall material, and heat stirs under melting temperature and adds auxiliary agent, Homogeneous phase mixing; Then by gained mixture rapid drawdown temperature to 0 ~ 5 DEG C, keep at least 24 hours;
(2) heat melts the mixture of step (1) gained, with it for releasable material prepares slow-releasing microcapsule.
10. slow-releasing microcapsule according to claim 9, prepared by following method:
(1) heat melts wall material, and heat stirs under melting temperature and adds auxiliary agent, Homogeneous phase mixing; Then by mixture rapid drawdown temperature to 0 ~ 5 DEG C, keep at least 24 hours;
(2) heat melts the mixture of step (1) gained, with it for releasable material prepares slow-releasing microcapsule;
(3) core is crushed to 100 ~ 120 orders, and prepares slow-releasing microcapsule with one of following step:
A. the core after pulverizing is dispersed in the releasable material that heat melts, atomization, cooling;
B. the core pulverized is adopted top spray technique fluidized bed coating, described top spray technological parameter comprises: inlet temperature 45 ~ 73 DEG C, air quantity 20 ~ 50m
3/ h, makes core be in good fluidized state, atomizing pressure 0.1 ~ 0.3MPa, flow velocity 3 ~ 20ml/min;
C. the core pulverized is adopted end pressure spray process fluidized bed coating, pressure spray process of the described end is: inlet temperature 45 ~ 73 DEG C, air quantity 20 ~ 50m
3/ h, regulates mozzle lower end and distribution grid spacing, makes core be in good fluidized state, atomizing pressure 0.1 ~ 0.3MPa, flow velocity 7 ~ 25ml/min.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2017114339A1 (en) * | 2015-12-30 | 2017-07-06 | 大连医诺生物有限公司 | Microencapsulation of β-alanine |
| 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 |
| CN107998224A (en) * | 2017-12-29 | 2018-05-08 | 武汉市天辰生物科技有限公司 | A kind of aquatic products anti virus herb slow-releasing granules and preparation method |
| CN109820836A (en) * | 2019-03-22 | 2019-05-31 | 大连医诺生物股份有限公司 | Levorotation carnitine sustained-release microcapsule powder and preparation method thereof |
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| EP3955909B1 (en) * | 2019-04-19 | 2023-11-22 | Sila S.P.A. | Granular product based on arginine |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2017114339A1 (en) * | 2015-12-30 | 2017-07-06 | 大连医诺生物有限公司 | Microencapsulation of β-alanine |
| US10555909B2 (en) | 2015-12-30 | 2020-02-11 | Innobio Corporation Limited | Microencapsulation of B-alanine |
| 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 |
| CN107811298B (en) * | 2017-12-01 | 2021-02-19 | 浙江新和成股份有限公司 | Water-soluble nutrient microcapsule and preparation method thereof |
| CN107998224A (en) * | 2017-12-29 | 2018-05-08 | 武汉市天辰生物科技有限公司 | A kind of aquatic products anti virus herb slow-releasing granules and preparation method |
| CN109820836A (en) * | 2019-03-22 | 2019-05-31 | 大连医诺生物股份有限公司 | Levorotation carnitine sustained-release microcapsule powder and preparation method thereof |
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