CN103404955B - Preparation method and device for multilayered embedded particles - Google Patents
Preparation method and device for multilayered embedded particles Download PDFInfo
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- CN103404955B CN103404955B CN201310392791.2A CN201310392791A CN103404955B CN 103404955 B CN103404955 B CN 103404955B CN 201310392791 A CN201310392791 A CN 201310392791A CN 103404955 B CN103404955 B CN 103404955B
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Abstract
The invention provides a preparation method and device for multilayered embedded particles. The preparation method comprises the following steps of: dispersing active components into a protective colloidal solution to form an active component mixed suspension solution; processing the mixed suspension solution into liquid drops with the grain diameter in a range of 100-1000 microns; enabling second-layer embedding materials to be attached to the surfaces of the liquid drops and curing to obtain bead-shaped grains; and further drying the bead-shaped grains to obtain the multilayered embedded particles. The preparation method provided by the invention is simple in device and easy to operate. The multilayered embedded particles provided by the invention have high stability, narrow grain diameter distribution, good flowability and high mechanical strength, and can be widely applied to fields of tablets, hard capsules, diet supplementing foods, health-care foods, medicines and the like.
Description
Technical field
The present invention relates to preparation method and the equipment of a kind of multilayer embedding particulate (beadlets), more particularly, the invention provides and a kind of multilayer embedding is carried out to active component, with obtain high stable, narrow diameter distribution, good fluidity, microencapsulation particulate that mechanical strength is high method and prepare the equipment of this particulate.
Background technology
Microcapsules are embedded, seal the technology becoming a kind of solid particulate product in a kind of microencapsulation up for safekeeping solid, liquid or gaseous matter.Wrapped composition can be protected like this, make it the unsuitable environment facies with the external world and completely cut off, reach and keep original color, smell and taste, performance and biologically active to greatest extent, and prevent destruction and the loss of nutriment.Microcapsules technology is in fact a kind of packing technique, and quality and " packaging material " wall material, the embedding process of its effect are closely related, and determine the main performance of microcapsule product, as: dissolubility, slow release, mobility etc.
Usually, microencapsulation method many employings high temperature spray-drying method, fluidized bed coating etc. of food industry.The feature of these class methods is undertaken by following three steps:
Wall material is dispersed in its corresponding solvent;
Again core is dispersed in this dispersion;
By methods such as spraying dry, wall material is assembled, around core that heavy stain or wrap in has been disperseed.
The microcapsules membranous wall of such formation can only embed core by individual layer, and its product has segmental defect; Dry run temperature is higher, easily causes the loss of active component; Wall material is not high to the embedding rate of core, and unstable active components, product poor fluidity, distribution of particles are uneven, bad mechanical strength etc.The product of such preparation is still needed and to be processed, to reach certain mechanical strength by the method for chemistry or physics.
Summary of the invention
The present invention relates to preparation method and the equipment of a kind of multilayer embedding particulate, more particularly, the invention provides and a kind of double-layer embedment is carried out to active component, with obtain a kind of high stable, narrow diameter distribution, good fluidity, microencapsulation particulate that mechanical strength is high preparation method and prepare the equipment of this kind of particulate.
Multilayer embedding particulate prepared by method of the present invention, solves product Problems existing prepared by conventional microcapsule metallization processes, and multilayer embedding particulate of the present invention has following characteristics:
1. multilayer embedding, active component is not oxidizable, more stable;
2. product hardness is high, extremely strong anti-pressure ability, and can resist mechanical shearing;
3. narrow diameter distribution, mobility of particle is good, is easy to processing;
4. non-dusting mobility powder, makes batch mixing process easy, easy to operate;
5. active component release can also effectively be controlled;
6. implementation procedure equipment is simple, is easy to operation.
The preparation method of multilayer embedding particulate of the present invention, comprises the steps:
A) active component is scattered in the step forming active component suspension in protective colloid solution;
B) step suspension a) is formed the step of domain size distribution at 100 ~ 1000 μm of drops;
C) in step b) drop surface attachment second layer embedded material, after solidification the step of Beads; With
D) further that Beads is dry, obtain the step of multilayer embedding particulate.
Protective colloid of the present invention is at least one in modified starch, natural plant gum, caseinate, gelatin.Step a) in the content of protective colloid do not limit, be adjust in right amount according to the carrying capacity of active component, the mass ratio of protective colloid and active component preferably adopts 0.01 ~ 80:1 in the present invention.
Described modified starch is the natural origin starch that octenyl succinic acid anhydride (OSA) processed, and comprises corn, waxy corn, cassava, barley, wheat etc.
Described natural plant gum is the edible colloid deriving from plant, comprises Arabic gum, xanthans, carragheen, agar, soybean protein glue etc.
Active component of the present invention is at least one in ω-3 biodiesel, ω-6 biodiesel, ω-9 biodiesel, liposoluble vitamin, carotenoid.Described carotenoid is any one or two kinds and two or more mixtures in beta carotene, lutein, zeaxanthin, lycopene, astaxanthin, kryptoxanthin, capsorubin, fucoxanthine, cantharides xanthin.Described liposoluble vitamin is vitamin A, vitamin D, vitamin E etc.Described functional grease comprises, the DHA fish oil of such as ω-3 class, algae oil, EPA, ALA etc., the CLA of ω-6 quasi-grease and glyceride thereof, sunflower oil, ARA, GLA etc., the camellia oil of ω-9 quasi-grease, olive wet goods.
Caseinate of the present invention is casein and light metal, as unit price sodium (Na
+) or bivalent calcium (Ca
2+) synthetics, as casein sodium, calcium caseinate etc. that the art personnel know.
Multilayer embedding particulate prepared by method of the present invention, in its preparation process, does not specially require and adds emulsifying agent.In order to make the better emulsification of the suspension of active ingredient, preparation process of the present invention a) in can add appropriate emulsifying agent, but whether adding of emulsifying agent obviously can not affect the multilayer embedding preparation efficiency of particulate and its effect.The mass ratio of emulsifying agent and active component adopts 0.1 ~ 20:1.Described emulsifying agent preferably adopts nonionic emulsifier, is to derive from food, medicine surfactant.Described nonionic emulsifier is preferably selected from one or more mixtures formed with arbitrary proportion in sucrose fatty ester, polyglyceryl fatty acid ester, sorbitol fatty acid ester, single double glyceride, phosphatide, and one or more more preferably in sucrose fatty ester, polyglyceryl fatty acid ester, sorbitol fatty acid ester, single bi-tristearin are with mixtures of arbitrary proportion composition.One or more mixtures formed with arbitrary proportion in sucrose fatty ester, polyglyceryl fatty acid ester, single double glyceride are most preferably adopted in the present invention.
Multilayer embedding particulate prepared by method of the present invention, in its preparation process, does not specially require and adds filler.Preparation method's step of the present invention a) in can add appropriate filler, play the effect of micrograined texture densification.Described filler is preferably selected from the starch derivatives such as maltodextrin, oligomeric maltose, corn syrup, glucose, sucrose, trehalose, lactose etc.
Multilayer embedding particulate prepared by the inventive method, in its preparation process, does not specially require and adds antioxidant.Preparation method of the present invention step a) in, appropriate antioxidant can be added, increase the antioxygenic property of product.Antioxidant can adopt this area to commonly use antioxidant, and its addition is that use amount is commonly used in this area.
The present invention also provides the multilayer embedding prepared by above-mentioned preparation method particulate.This multilayer embedding particulate is because active component is by double-layer embedment, and composition is not oxidizable, stable in properties, and the hardness of particulate is high, has extremely strong anti-pressure ability, can resist mechanical shearing; The particle diameter of particulate is between 40 ~ 150 orders, and narrow diameter distribution, mobility of particle is good, non-dusting mobility powder, makes batch mixing process easy, easy to operate in follow-up process.
Another object of the present invention is to provide a kind of equipment preparing multilayer embedding particulate, and described device comprises: shaping tower, atomizer, feed bin, conveying device, conveyance conduit and drying device; Described atomizer is arranged in shaping tower, and described conveying device is fixedly connected on the material outlet of bin bottom, and conveying device is connected with shaping tower inside by conveyance conduit; The particle outlet I being arranged on shaping tower bottom is connected with drying device.
Equipment of the present invention, described atomizer is centrifugal type atomizer, pressure atomizer or pulsed atomizer; Described drying device is boiling fluidised-bed drying machine or Vibratingfluidbeddrier.
In a specific embodiment, the protective colloid solution being dispersed with active component forms the drop of emulsion through atomizer atomization formation uniform particle diameter through emulsifying; Second layer embedded material is stored in feed bin, and is sent in shaping tower by conveying device and conveyance conduit wind; The drop atomization at shaping tower is obtained Beads by the embedding of second layer embedded material, the rear separation of solidification; The particle outlet I of Beads through being arranged on shaping tower bottom is sent to drying device, and drying can obtain multilayer of the present invention embedding particulate.
Beneficial effect of the present invention:
In the preparation process of 1. multilayer of the present invention embedding particulate not with an organic solvent, technique environmental protection, no solvent residue, is more conducive to food security.
2. preparation technology of the present invention all carries out being not more than under the low temperature of 140 DEG C, and active component not easily loses in preparation process.
3. the multilayer embedding particulate that prepared by method of the present invention has release property effectively, and can be conducive to human body and absorb fast.
4. it is high that the multilayer that prepared by method of the present invention embeds particulate hardness, has extremely strong anti-pressure ability, not easily broken wall, the good stability of product, be easy to apply in food processing technology.
Accompanying drawing explanation
Fig. 1 is multilayer of the present invention embedding particle device;
Drawing reference numeral: 1, shaping tower, 2, atomizer, 3, feed bin, 4, conveying device, 5, drying device, 6, mozzle, 7, discharge duct, 8, conveyance conduit, 9, particle outlet I, 10, particle outlet II, 11, screen cloth
Detailed description of the invention
Following non-limiting example can make the present invention of those of ordinary skill in the art's comprehend, but does not limit the present invention in any way.
A preparation method for multilayer embedding particulate, comprises the steps:
A) active component is scattered in the step forming active component suspension in protective colloid solution;
B) step suspension a) is formed the step of domain size distribution at the drop of 100 ~ 1000 μm;
C) in step b) drop surface attachment second layer embedded material, after solidification the step of Beads; With
D) further that Beads is dry, obtain the step of multilayer embedding particulate.
The preparation method of above-mentioned multilayer embedding particulate is illustrated below in conjunction with the multilayer embedding particle device shown in accompanying drawing 1.
Described multilayer embedding particle device (Fig. 1) comprises shaping tower 1, atomizer 2, feed bin 3, conveying device 4 and drying device 5, wherein said atomizer 2 is arranged in shaping tower 1, described atomizer 2 is fixed with mozzle 6, mozzle 6 one end open and atomizer 2 nozzle upper surface compact siro spinning technology, it is outside that other end opening is positioned at shaping tower 1, and the protective colloid solution being dispersed with active component is formed after emulsion through emulsifying sends into atomizer 2 atomization formation drop by mozzle 6;
Described conveying device 4 is fixedly connected on bottom feed bin 3, conveying device 4 is connected with atomisation tower 1 inside by conveyance conduit 8, air is sent into by conveying device 4 side, the second layer embedded material stored in feed bin 3 is fed in shaping tower 1 by conveyance conduit 8 along with air, enter air in shaping tower 1 and part second layer embedded material enters in feed bin 3 by discharge duct 7, and second layer embedded material is separated in feed bin 3, the waste gas outlet of waste gas through being arranged on feed bin 3 top is discharged into outside;
Described conveying device 4 regulates by the control valve installed therein the amount being entered into the second layer embedded material in conveying device by the tapered outlet at bottom bottom feed bin 3.
In the specific implementation, while emulsion feeding atomizer 2 atomization of emulsifying, second layer embedded material wind sends into shaping tower 1, and parcel atomizer 2 is atomized the drop formed.Hot blast is blown into bottom shaping tower 1, and the particulate regulating air quantity and wind speed screening to be wrapped up by second layer embedded material and second layer embedded material, residue second layer embedded material enters in feed bin 3 with hot blast by discharge duct 7, be wrapped particulate (Beads) through being arranged on the particle outlet I 9 of shaping tower 1 bottom, enter into drying device 5, the particulate that drying completes sends outside through particle outlet II 10, is multilayer of the present invention embedding particulate.Be provided with screen cloth 11 bottom shaping tower 1, first through screen cloth 11 when hot blast is blown into shaping tower 1, avoid Beads to fall into hot air duct.
Embodiment 1
110g casein sodium, 890g sucrose are placed in 2000ml water, are warming up to 60 DEG C, be stirred to and mix and dissolve, obtain protective colloid solution.Then be slowly added in described protective colloid solution by 1000g fish oil (EPA/DHA:18/12), stir, gained suspension is homogeneous twice under 40MPa pressure, obtains emulsion; Emulsion is sent into centrifugal atomizer atomization, send into the edible corn starch (powdery) in feed bin to wind in atomisation tower simultaneously, parcel atomized drop; Collect the particulate that is wrapped cornstarch and screen out remaining starch and obtain Beads, grain diameter is at 40 order ~ 120 orders, and this particle is less than 5.0% at the fluidizing fluid-bed moisture that is dried to further, obtain 1890g particle of fish oil, in particulate, the mass percentage of Omega3 is 12%, and the bulk density of particulate is 0.63g/ml.
Embodiment 2
400g Arabic gum, 390g corn syrup are placed in 980ml water, are warming up to 55 DEG C, be stirred to and mix and dissolve, obtain protective colloid solution; By 50g mixed tocopherol, 160g lutein crystal, (lutein mass percentage is 80%, from Dalian Innobioactives Co., Ltd.
) slowly add in described protective colloid solution.And pass through emulsifying homogeneous 2 times, homogenization pressure 60Mpa.Above-mentioned emulsion is sent into centrifugal atomizer atomization, send into food-grade modified starch (silica addition is 5%) to wind in atomisation tower simultaneously, and wrap up atomized drop.Collect and wrapped up the wet granular of modified starch, then screen out remaining starch and obtain Beads, this particle at 20 order ~ 140 orders, and is wherein dried to moisture 3.0% at vibra fluidized bed drying by particle diameter further, obtains 935g lutein particulate (lutein content is 10.4%).Microparticle flow properties is good, bulk density 0.59g/ml.
Embodiment 3
870g modified starch is placed in 1000ml water, is warming up to 63 DEG C, be stirred to and mix and dissolve, obtain protective colloid solution; 1405g vitamin E (vitamin E mass percentage is 98%) is slowly added in above-mentioned protective colloid solution and is uniformly dispersed.And pass through emulsifying homogeneous 2 times, homogenization pressure 50Mpa.Above-mentioned emulsion is sent into the atomization of pulsed atomizer, atomized drop falls into the fluid bed that food-grade corn starch is housed simultaneously.Then collect wet granular, and screen out remaining starch and obtain Beads, this particle at 20 order ~ 140 orders, and is dried to moisture 3.5% by particle diameter further in ebullated dryer, obtains 1995g vitamin E particulate (content of vitamin E is 50%).Microparticle flow properties is good, bulk density 0.61g/ml.
Claims (5)
1. a preparation method for multilayer embedding particulate, is characterized in that, comprise the steps:
A) active component is scattered in the step forming active component suspension in protective colloid solution;
B) step suspension a) is formed the step of domain size distribution at 100 ~ 1000 μm of drops;
C) in step b) drop surface attachment second layer embedded material, after solidification the step of Beads; With
D) further that Beads is dry, obtain the step of multilayer embedding particulate;
Wherein: described protective colloid is at least one in modified starch, natural plant gum, caseinate, gelatin; Described second layer embedded material is at least one in silica, starch, dextrin, compound sugar, modified starch, calcium silicates, tricalcium phosphate, calcium carbonate, cellulose;
Described modified starch is the natural origin starch of octenyl succinic acid anhydride process; Described natural plant gum is Arabic gum, xanthans, carragheen, agar, soybean protein glue;
The preparation equipment of preparation multilayer embedding particulate comprises: shaping tower, atomizer, feed bin, conveying device, conveyance conduit and drying device; Described atomizer is arranged in shaping tower, and described conveying device is fixedly connected on the material outlet of bin bottom, and conveying device is connected with shaping tower inside by conveyance conduit; The particle outlet I being arranged on shaping tower bottom is connected with drying device;
The protective colloid solution being dispersed with active component forms the drop of emulsion through atomizer atomization formation uniform particle diameter through emulsifying; Second layer embedded material is stored in feed bin, and is sent in shaping tower by conveying device and conveyance conduit wind; The drop atomization at shaping tower is obtained Beads by the embedding of second layer embedded material, the rear separation of solidification; The particle outlet I of Beads through being arranged on shaping tower bottom is sent to drying device; Wherein, hot blast is blown into from shaping tower bottom, and the particulate regulating air quantity and wind speed screening to be wrapped up by second layer embedded material and second layer embedded material, residue second layer embedded material enters in feed bin with hot blast by discharge duct, Beads, through being arranged on the particle outlet I of shaping tower bottom, enters into drying device.
2. preparation method according to claim 1, is characterized in that, described active component is at least one in ω-3 biodiesel, ω-6 biodiesel, ω-9 biodiesel, liposoluble vitamin, carotenoid.
3. prepare an equipment for multilayer embedding particulate, it is characterized in that, described equipment comprises: shaping tower, atomizer, feed bin, conveying device, conveyance conduit and drying device; Described atomizer is arranged in shaping tower, and described conveying device is fixedly connected on the material outlet of bin bottom, and conveying device is connected with shaping tower inside by conveyance conduit; The particle outlet I being arranged on shaping tower bottom is connected with drying device; Hot blast is blown into from shaping tower bottom.
4. equipment according to claim 3, is characterized in that, described atomizer is centrifugal type atomizer, pressure atomizer or pulsed atomizer.
5. equipment according to claim 3, is characterized in that, described drying device is boiling fluidised-bed drying machine or Vibratingfluidbeddrier.
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| EP3363532B1 (en) * | 2015-10-12 | 2020-11-25 | Zhejiang Medicine Co., Ltd. Xinchang Pharmaceutical Factory | Method for granulating, forming, and drying fat soluble nutrient microcapsule particles |
| CN106035739B (en) * | 2016-05-23 | 2019-05-17 | 中国农业大学 | A kind of method that LBL self-assembly solidifies linseed oil and its compounds grease |
| 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 |
| CN107549801B (en) * | 2017-08-24 | 2020-11-13 | 福格森（武汉）生物科技股份有限公司 | Multilayer embedded solid lipid calcium particle |
| CN108576817B (en) * | 2018-03-23 | 2021-07-02 | 河南科技大学 | Preparation method of slow-release type anthocyanin microcapsules |
| CN109090613A (en) * | 2018-07-13 | 2018-12-28 | 大连医诺生物股份有限公司 | A kind of conjugated linoleic acid glyceride microcapsule powder and preparation method thereof |
| CN109602952B (en) * | 2018-12-27 | 2021-05-18 | 上海北陆医药科技有限公司 | Long-acting slow-release cell scaffold and preparation method and application thereof |
| CN110584109A (en) * | 2019-07-26 | 2019-12-20 | 山东天音生物科技有限公司 | Lutein embedded with animal fat and preparation method and application thereof |
| CN111631334A (en) * | 2020-06-15 | 2020-09-08 | 中国海洋大学 | Multi-layer emulsion-based acidic multifunctional fish oil beverage and preparation method thereof |
| CN112189846B (en) * | 2020-10-30 | 2022-06-10 | 大连医诺生物股份有限公司 | High-oil-loading pressure-resistant particle preparation and preparation method thereof |
| CN112753778A (en) * | 2020-12-31 | 2021-05-07 | 大连臻鼎科技有限责任公司 | High-stability grease particle product and preparation method thereof |
| CN113016864B (en) * | 2021-04-20 | 2023-11-28 | 甘肃农业大学 | Preparation method of jerky preservative |
| CN115251396A (en) * | 2022-09-01 | 2022-11-01 | 江苏恒康生物科技有限公司 | Dispersing carrier, probiotic double-layer microcapsule, and preparation method and application thereof |
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| EP0530277B1 (en) * | 1990-05-15 | 1994-08-10 | Danochemo A/S | Process for preparing microcapsules containing a flavourant embedded in a matrix material and products prepared by using the process |
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| CN101015342A (en) * | 2007-02-08 | 2007-08-15 | 上海交通大学 | Preparation method of lycopersicin microcapsule |
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Address after: 116600 Dalian medical science and Technology Development Zone, Liaoning 49, Dalian Patentee after: Dalian promise biological Limited by Share Ltd Address before: 116600 No. 49 Development Zone, Jinzhou New District, Liaoning, Dalian Patentee before: Dalian Innobioactives Co., Ltd. |