CN111449960A - Nested capsule and preparation method thereof - Google Patents
Nested capsule and preparation method thereof Download PDFInfo
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- CN111449960A CN111449960A CN202010272667.2A CN202010272667A CN111449960A CN 111449960 A CN111449960 A CN 111449960A CN 202010272667 A CN202010272667 A CN 202010272667A CN 111449960 A CN111449960 A CN 111449960A
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- A61J3/00—Devices or methods specially adapted for bringing pharmaceutical products into particular physical or administering forms
- A61J3/07—Devices or methods specially adapted for bringing pharmaceutical products into particular physical or administering forms into the form of capsules or similar small containers for oral use
- A61J3/078—Devices or methods specially adapted for bringing pharmaceutical products into particular physical or administering forms into the form of capsules or similar small containers for oral use into the form of wafers or cachets
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Abstract
The application discloses a nested capsule and a preparation method thereof, wherein the preparation method of the nested capsule comprises the following steps: preparing O/W type emulsified contents; in the gel growth liquid, the gel layer is wrapped on the outer surface of the O/W type emulsion drop to form a sub-capsule; curing and drying the sub-capsules; nesting at least one transparent gel layer outside at least one sub-capsule by putting the at least one sub-capsule externally coated with the outer-layer emulsion into the gel growth liquid to form a nested capsule; and solidifying and drying the nested capsule, wherein the content is prepared from content emulsion, the content emulsion comprises 50-80% of oil phase, 20-50% of water phase, 0.5-3% of curing agent, 0.5-2% of co-emulsifier, 0.1-3% of surfactant and 0.05-5% of co-surfactant according to weight percentage, the gel growth solution comprises 0.1-3% of gelling agent, 0.1-3% of auxiliary colloid and 0.05-4% of gel growth auxiliary agent according to weight ratio, and the gelling agent is sodium alginate.
Description
Technical Field
The invention relates to the field of capsule manufacturing, in particular to a preparation method of a nested capsule.
Background
The traditional capsules are generally divided into two main categories, namely hard capsules (suitable for filling powder medicines) and soft capsules (suitable for oily liquid medicines such as fish oil, vitamin E, vitamin A and the like). The soft capsule is also called capsule, and is a round or oval preparation formed by sealing oil or liquid medicine or suspension which has no dissolving effect on gelatin or plant colloid in the soft capsule.
Compared with the traditional capsule, the soft capsule has the advantages of distinct characteristics, wide adaptability, extremely high transparency, good heat resistance, moisture resistance, sealing performance and toughness, and wide application in the industries of tobacco, food, medicine, cosmetics and the like. The soft capsule is divided into a seamed capsule and a seamless capsule according to different manufacturing processes, the seamed capsule mostly adopts gelatin or modified starch as a shell, a membrane is firstly prepared before the capsule is pressed, then core liquid is injected between two membranes through equipment and is pressed through a mould, and the joint of the two membranes has obvious indentation, so the seamed capsule is called. The seamless capsule, also called as dripping pill, is prepared by extruding the outer layer glue solution and the inner layer core solution through a group of concentric orifice holes by co-extrusion method (Didieye-Hartmann, Chinese patent publication No. CN 101203213A, CN 101203148A; Zhang wenhui, Chinese patent application publication No. CN101925403A), wrapping, dripping into oily cooling liquid, and solidifying to form seamless capsule.
The preparation of the multilayer capsule in the industry mostly adopts the principle of concentric circle coextrusion, each layer of core liquid and involucra is respectively extruded by a group of multiple concentric circle sharp holes to form nested package, for example, the three-layer capsule described in CN 107361392 is synchronously beaten by a phase-changeable grease layer component and a natural animal and plant glue layer component through three-channel concentric circle drippers, wherein, the innermost channel is added with a water-containing core liquid layer component, the outermost channel is added with a natural animal and plant glue layer component, the middle channel is added with a phase-changeable grease layer component, and three groups of feed liquids form three concentric spheres nested layer by layer in cooling liquid to fall under the action of liquid cohesion and are gradually cooled and solidified to form the complete inclusion three-layer capsule. The three-layer capsule described in the above CN 107361392 is actually a capsule with only the outermost layer of membrane, and the precision of the dripping device and the preparation and control of the core liquid and membrane material of each layer are very difficult to be achieved by adopting the concentric circle co-extrusion method to prepare the multi-layer capsule, and it is difficult to ensure that one layer does not fall off or deviate to one direction, thereby seriously affecting the mechanical strength, roundness and uniformity of the prepared capsule.
CN 105377243B describes a hydrogel formed by hollow silica capsules containing water-insoluble substances, a stabilizing agent and a polymer blend and a capsule with a three-layer structure prepared by using polymers with proper hydrophobicity, wherein the three-layer capsule has a size of 50um to 3,000 um. The microcapsule is prepared by dispersing and dehydrating a poorly water-soluble substance, a stabilizer, and hollow silica in ethanol or hydrous ethanol in which a hydrophobic polymer is dissolved. However, more than three layers of capsules cannot be produced by this method, and it is difficult to produce capsules containing more than two sub-capsules.
Disclosure of Invention
It is an object of the present invention to provide a method for producing a nested capsule, wherein a multi-layer nested capsule, in particular, a nested capsule having three or more layers can be produced by the method for producing a nested capsule.
It is another object of the present invention to provide a method for preparing a nested capsule, wherein a capsule containing more than two sub-capsules can be prepared using the nested capsule preparation method.
Another object of the present invention is to provide a process for the preparation of nested capsules, wherein the nested capsules prepared by the process for the preparation of nested capsules have good roundness and uniformity.
To achieve at least one of the above objects, the present invention provides a method for preparing a nested capsule, wherein the method for preparing the nested capsule comprises the steps of:
preparing O/W emulsified contents, wherein the contents are prepared from contents emulsion, wherein the contents emulsion comprises 50-80% of oil phase, 20-50% of water phase, 0.5-3% of curing agent, 0.5-2% of co-emulsifier, 0.1-3% of surfactant and 0.05-5% of co-surfactant according to weight percentage;
wrapping a gel layer on the outer surface of the O/W type emulsion drop in a gel growth solution to form the sub-capsule, wherein the gel growth solution comprises 0.1-3 wt% of a gel agent, 0.1-3 wt% of an auxiliary colloid and 0.05-4 wt% of a gel growth auxiliary agent, and the gel agent is sodium alginate;
curing and drying the sub-capsules;
nesting at least one transparent gel layer outside at least one of the sub-capsules by throwing at least one of the sub-capsules externally coated with an outer layer emulsion into a gel growth liquid to form a nested capsule; and
curing and drying the nested capsules.
According to an embodiment of the present invention, preparing the emulsified contents is performed to include the steps of:
(a) dissolving the coemulsifier with the corresponding proportion in the deionized water with the proportion range;
(b) dissolving a curing agent and a surfactant in the deionized water solution;
(c) slowly adding the uniformly mixed fat-soluble solvent and functional ingredients into the deionized water solution in the step (b);
(d) stirring the deionized water solution in the dispersing step (c) to form a white emulsion of oil phase/water (O/W) phase type; and
(e) stirring is continued for 20min to 30min, and the solution is cooled to room temperature.
According to an embodiment of the present invention, in the step (e), the rotation speed of stirring is greater than or equal to 200 r/min.
According to an embodiment of the present invention, the viscosity of the emulsion is 2000 to 20000 cps.
According to an embodiment of the present invention, curing and drying the sub-capsules comprises the steps of: washing the prepared sub-capsules with deionized water to clean the surfaces, and transferring the sub-capsules into a divalent metal ion solution with the mass concentration of 0.5-20% for curing for 10 min-2 h;
and (3) washing the cured sub-capsules with deionized water to clean the surfaces of the sub-capsules, drying for 30 min-3 h, transferring the sub-capsules to a ventilation place for drying until the sub-capsules are completely transparent after the sub-capsules are dehydrated, cured and shaped and the surfaces of the sub-capsules have certain hardness, wherein the drying time is 1 h-12 h.
According to an embodiment of the present invention, the viscosity of the outer layer emulsion is 8000-20000 cps.
According to an embodiment of the invention, the outer layer emulsion comprises 50-80% of oil phase, 20-50% of water phase, 0.5-3% of curing agent, 1-3% of co-emulsifier, 0.1-3% of surfactant and 0.05-5% of co-surfactant according to weight percentage.
According to an embodiment of the present invention, the curing agent is a divalent or polyvalent metal ion, including: ca2+、Ba2+、Mg2+One or more of (a).
According to an embodiment of the invention, the method for preparing the nested capsule comprises the following steps:
nesting at least one transparent gel layer outside at least one nested capsule by putting the nested capsule coated with an outer layer emulsion into gel growth liquid to form a plurality of layers of nested capsules, wherein the gel growth liquid comprises 0.1-3% of gelling agent, 0.1-3% of auxiliary colloid and 0.05-4% of gel growth auxiliary agent in weight ratio; and
curing and drying the multi-layered wrapped nested capsules.
According to another aspect of the invention, there is provided a nested capsule, wherein the nested capsule is prepared by the method of preparing the nested capsule.
Further objects and advantages of the invention will be fully apparent from the ensuing description and understanding.
These and other objects, features and advantages of the present invention will become apparent from the following detailed description, and from the claims
Detailed Description
The preferred embodiments in the following description are given by way of example only, and other obvious variations will occur to those skilled in the art. The basic principles of the invention, as defined in the following description, may be applied to other embodiments, variations, modifications, equivalents, and other technical solutions without departing from the spirit and scope of the invention.
It will be understood by those skilled in the art that in the present disclosure, the terms "longitudinal," "lateral," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," and the like are used in an orientation or positional relationship indicated based on the orientation or positional relationship shown, which is for convenience in describing and simplifying the description, and do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus the terms should not be construed as limiting the invention.
A method of making a nested capsule according to a preferred embodiment of the present invention is described in detail below, wherein the method of making a nested capsule enables the production of multi-layered nested capsules, particularly nested capsules of three or more layers, and capsules containing two or more sub-capsules. The preparation method for preparing the nested capsule comprises the following steps:
(S1) preparing contents; the content is prepared from content emulsion, wherein the content emulsion comprises 50-80% of oil phase, 20-50% of water phase, 0.5-3% of curing agent, 0.5-2% of co-emulsifier, 0.1-3% of surfactant and 0.05-5% of co-surfactant according to weight percentage.
Preferably, the viscosity of the content emulsion is controlled to be 8000-18000 centipoises. Along with the increase of the proportion of the oil phase, the viscosity of the formed emulsion gradually rises, even the fluidity is gradually lost, which can generate certain influence on the dripping parameters at the later stage, so the attention and the control on the viscosity are required in the emulsification process of the contents,
the oil phase 50-80% comprises 0.01-30% of functional components and 20-50% of fat-soluble solvent. The functional component is a fragrant substance or a functional substance, and the fragrant substance is one of peppermint oil, sweet orange oil, citral, cedar wood oil, geraniol, furanone, rum ether, anethole, cinnamaldehyde, tobacco extract, tobacco essential oil, etc., or other substances capable of being used for flavoring; the functional substances are: fat-soluble vitamin C, vitamin E, astaxanthin, nicotinamide, lutein, tea polyphenol and other functional antioxidants.
The content emulsion prepared by the invention is oil-in-water emulsion, water-soluble components and fat-soluble components are added into the content, after the capsule is dried, the water in the content is fully dispersed to only leave an oil phase, the oil-soluble active components are dissolved in the fat-soluble solvent, and the water-soluble components are separated out to form precipitates. The content emulsion prepared by the invention is oil-in-water emulsion, and the higher the oil phase proportion is, the better the roundness of the dried capsule is, because the capsule is coated with an emulsion by reverse spheroidization of alginate, the water phase in the emulsion can be gradually lost and completely lost in the drying process of the capsule, and if the oil phase proportion is less than 60%, the situations of depression and shrinkage are easy to occur in the drying process. The preparation of the emulsion becomes more difficult along with the reduction of the proportion of the water phase, the solution is not completely emulsified, and the gel is easy to grow unevenly to generate liquid leakage in the dripping process, thereby reducing the quality of finished products; meanwhile, with the increase of the proportion of the oil phase, the viscosity of the formed emulsion gradually rises, even gradually loses the fluidity, and the viscosity is concerned and controlled in the emulsification process of the contents because the viscosity of the formed emulsion gradually rises, even gradually loses the fluidity, which has a certain influence on the later dripping parameters, and the preferable viscosity of the emulsion is controlled between 8000 and 18000 centipoises.
The fat-soluble solvent is as follows: MCT, olive oil, simethicone, triglyceride, paraffin oil, soybean oil, and rapeseed oil.
The curing agent is a divalent or polyvalent metal ion and comprises: ca2+、Ba2+、Mg2+One or more of (a).
It is worth one, divalent metal ion meets alginate and then produces gel, carries on the ball-shaped package to the latex, in the capsule gel growth process, divalent metal gradually permeates out the capsule surface from the gel and forms gel with the alginate solution, therefore the divalent metal ion concentration in the solution water phase increases, the capsule skin thickness increases the speed and increases.
The concentration of the curing agent accounts for 0.5-3% of the proportion of the emulsion, wherein 1-2% is more ideal, the growth speed of gel which is less than 0.5% is slower, the structure of the formed gel is not compact, and the surface of the capsule is not smooth; if the content of the divalent metal ions is more than 3 percent, a certain amount of divalent metal ions remain, and the capsules still have certain residue after elution, so that the conditions of uneven growth or turbidity in suspended contents after drying and the like are finally caused.
The auxiliary emulsifier is as follows: one or more of konjac gum, xanthan gum, guar gum, pectin, methyl cellulose, starch, dextrin, sucrose ester and sodium curtate. The vegetable gum is dissolved in the water phase, so that the viscosity of the water phase can be increased, the emulsification efficiency is improved, and the stability of the oil-in-water emulsion is improved. Meanwhile, the vegetable gum can be a membrane component of the capsule, and the colloid is dissipated from inside to outside along with the water phase in the drying process of the capsule and migrates to the membrane of the capsule to enter a membrane system, so the vegetable gum used as an emulsifying aid is an auxiliary way for characteristic composition and improvement of the membrane of the capsule.
The surfactant is one or more of Tween 20, Tween 60, Tween 40, Tween80, Tween 60, span 20, span 40, span 60, span 80, sucrose ester, sorbitol ester, soybean phospholipid, dodecane, sodium sulfate and the like, more preferably Tween80 and Tween 60, during emulsion preparation, a higher H L B value is more favorable for preparing a more uniform, stable and completely dispersed oil-in-water emulsion, but in the actual emulsification process, different types of contents, even mixtures, may need to be prepared with different types of surfactants, and even need to be matched for use to obtain a better emulsification effect.
Optionally, the co-surfactant is: one or more of ethanol, propylene glycol, glycerol, isopropanol, and n-butanol. The cosurfactant can change the surface activity and the hydrophilic-lipophilic balance of the surfactant, participate in forming micelles, adjust the polarity of water and oil, reduce the polarity of the water by using the water-soluble alcohol, and increase the polarity of the oil by using the oil-soluble alcohol, so that the phase state and the phase property of a system are influenced, and the emulsibility and the stability are improved. In addition, the toughness and brittleness of the capsule coating can be adjusted by the migration of propylene glycol and glycerol from inside to outside along with the loss of the water phase to the capsule coating entering the coating system in the drying process of the capsule.
The preparation method for preparing the nested capsule comprises the following steps: (S2) emulsifying the contents. Specifically, emulsifying the contents is carried out to include the steps of:
(a) melting the coemulsifier with the corresponding proportion in the deionized water with the proportion range;
(b) dissolving a curing agent and a surfactant in the deionized water solution;
(c) slowly adding the uniformly mixed fat-soluble solvent and functional ingredients into the deionized water solution in the step (b);
(d) stirring the deionized water solution in the dispersing step (c) to form a white emulsion of oil phase/water (O/W) phase type; and
(e) stirring is continued for 20min to 30min, and the solution is cooled to room temperature.
It is worth integrating that in said step (e) the rotation speed of the stirring is greater than or equal to 200r/min, preferably the stirrer rotation speed is greater than 1000 r/min. The viscosity of the emulsion is 2000-20000 centipoises, preferably 2000-10000 centipoises.
Correspondingly, in the step (a), when the deionized water with the corresponding proportion of the coemulsifier in the proportion range is melted, the coemulsifier is added into the deionized water according to the proportion range, the mixture is heated to 75 ℃ and stirred until the mixture is completely melted,
it is worth noting that the order of addition of the aqueous phase and the oil phase is important in the preparation of the emulsion, and in the O/W type emulsion, water is used as the continuous phase, and the oil phase is generally slowly added to the aqueous phase while stirring. The stirring speed influences the size of oil phase particles in the emulsion, and the diameter of the oil phase particles obtained by medium-speed stirring is larger than that of the oil phase particles obtained by high-speed stirring. Generally, the emulsion obtained by high-speed stirring is more uniform and stable, so that the later-stage emulsion gel growth process is more uniform and controllable.
The preparation method for preparing the nested capsule comprises the following steps: (S3) preparing the sub-capsules.
Specifically, a gel layer is wrapped on the outer surface of the O/W type emulsion drop in the gel growth liquid to form the sub-capsule.
The gel growth liquid comprises 0.1-3 wt% of gelling agent, 0.1-3 wt% of auxiliary colloid and 0.05-4 wt% of gel growth auxiliary agent;
the gel is sodium alginate, and comprises the following components: one or more of high G type sodium alginate and high M type sodium alginate in certain proportion. Divalent or polyvalent metal ions, e.g. Ca2+The gel formed by the high G type sodium alginate and the high M type sodium alginate has the characteristic of hardness and brittleness, and the gel formed by the high M type sodium alginate is flexible, so that the proportion of the high G type and the high M type can be adjusted according to the requirement of a product on the rubber characteristic in the actual product design.
The auxiliary colloid is as follows: one or more of konjac gum, xanthan gum, guar gum, pectin, methyl cellulose, starch, dextrin or other colloid substances with film-forming function. The addition of auxiliary colloids can change the characteristics of the capsule membrane, such as: brittleness, flexibility, disintegration, moisture resistance and the like, and the content gel growth liquid containing the auxiliary colloid does not generate gel at normal temperature, otherwise, the gel growth cannot be carried out.
The gel growth auxiliary agent comprises: one or more of PEG, glycerol and propylene glycol. The addition of the gel growth aid can change the flexibility of the capsule membrane.
The preparation of the sub-capsules comprises the following steps:
weighing the gel growth solution according to the range, slowly adding the gel growth solution into hot water at 75 ℃, stirring until the gel growth solution is completely dissolved, and cooling to room temperature for later use.
Dripping the prepared O/W type emulsion into the gel growth solution;
slowly stirring to form a layer of transparent gel layer on the surface of the emulsion to wrap the emulsion into spherical capsules, and gradually thickening the gel layer on the surface of the capsules along with the increase of the soaking time of the capsules in the gel growth solution until reaching the proper thickness.
Preferably, slight stirring can be performed during the gel growth of the contents to avoid the adhesion between the capsules during the gel growth. The particle size of the capsule is controlled by the aperture of the orifice aperture of the dropper, fine adjustment is carried out according to the viscosity of the emulsion and the proportion of the oil phase in the emulsion, and the dropper with a large aperture is selected to carry out adjustment and correction through a plurality of tests in the actual dropping process.
The thickness of the gel layer determines the pressure value after the capsule is dried to a large extent, the thickness can be 0.5 mm-5 mm, and the growth rate is accelerated along with the concentration of alginate in the gel growth liquid and the concentration of divalent metal ions in the emulsion. The thickness of the gel layer can be controlled by controlling the growth speed or the growth time, wherein the growth speed needs to be controlled by the concentration of alginate and Ca2+The concentration of (2) is controlled.
The preparation method for preparing the nested capsule comprises the following steps: (S4) curing and drying the sub-capsules.
Washing the prepared sub-capsules with deionized water to clean the surfaces, and transferring the sub-capsules into a divalent metal ion solution with the mass concentration of 0.5-20% for curing for 10 min-2 h;
and (2) cleaning the surface of the cured sub-capsule with deionized water, transferring the sub-capsule to a rotating cage for drying, wherein the drying time is 30 min-3 h, transferring the capsule to a ventilation position for drying after the capsule is dehydrated, cured and shaped and the surface has certain hardness, wherein in the drying process, the emulsion in the capsule is gradually lost along with water, only fat-soluble components are left and gradually become transparent until the capsule is completely transparent, and the drying time is 1 h-12 h.
The preparation method for preparing the nested capsule comprises the following steps: (S5) preparing an outer emulsion.
The preparation method of the outer layer emulsion is the same as that of the inner layer emulsion, but the emulsion needs to have certain viscosity, and the outer layer emulsion needs to be coated on the processed capsule for secondary gel growth when the capsule is subjected to secondary nesting of the outer layer, so that the emulsion with certain viscosity is favorable for being adhered to the surface of the capsule in the inner layer. The viscosity is increased by properly adding a thickening auxiliary emulsifier to 1-3%. Preferably, the viscosity is 8000 to 20000 centipoises.
The auxiliary emulsifier is as follows: including but not limited to one or more of xanthan gum, guar gum, methyl cellulose, starch, dextrin or other colloidal materials having a thickening function useful for assisting emulsification.
The preparation method for preparing the nested capsule comprises the following steps: (S6) nesting a transparent gel layer outside the sub-capsules by dropping the sub-capsules externally coated with the outer layer emulsion into the gel growth liquid.
And (S5) coating the surface of the dried sub-capsules obtained in the step (S4) with the prepared outer-layer emulsion, putting the outer-layer emulsion into the gel growth solution, slowly stirring, forming a transparent gel layer on the surface of the emulsion wrapping the capsules, wrapping the emulsion into spherical capsules, and nesting the sub-capsules.
(S7) curing and drying the nested capsules.
The curing and drying process of the nested capsules is the same as (S4), and the sub-capsules gradually appear as the emulsion in the capsules gradually becomes transparent as water is lost.
If more levels of nesting are to be performed, the steps (S5) to (S7) are repeated. Not only can a plurality of capsules be nested according to the same method, but also two or more capsules or other granular materials can be nested in a certain layer of capsules.
In one embodiment of the invention, the preparation method of the nested capsule is adopted to prepare a two-layer nested capsule, wherein the diameter of the outer layer of the two-layer nested capsule is 4-5 mm, the diameter of the inner layer of the two-layer nested capsule is 2-3 mm, the inner layer of the two-layer nested capsule tastes lemon, and the outer layer of the two-layer nested capsule tastes sweet orange. Firstly, preparing a lemon flavor content according to the steps, specifically, preparing the lemon flavor content from a content emulsion, wherein the content emulsion comprises the following oil-phase and water-phase substances in percentage by weight:
an oil phase of 70%, wherein the oil phase comprises
Fat-soluble lemon essence 20%
MCT 50%; and
an aqueous phase 30%, wherein the aqueous phase comprises:
subsequently, the contents were emulsified. Concretely, the xanthan gum is added into deionized water according to the proportion range, the mixture is heated to 75 ℃ and stirred until the mixture is completely melted, and then CaCl is sequentially added2Stirring, dissolving and insulating Tween80 and glycerol for later use; and uniformly mixing the lemon essence and MCT, slowly adding the lemon essence and MCT into the solution of the water phase to be used, stirring and dispersing simultaneously, gradually forming O/W type white emulsion with certain viscosity by the rotation speed of a stirrer being more than or equal to 200r/min, and continuously stirring for 20-30 min until the temperature of the emulsion is reduced to room temperature, thus finishing the preparation of the emulsion.
Preparing an outer emulsion.
The preparation proportion of the outer layer emulsion is as follows by weight percent:
oil phase: 75%, wherein the oil phase comprises:
fat-soluble sweet orange essence: 25 percent of
And MCT: 50 percent; and
water phase: 25%, wherein the aqueous phase comprises:
the preparation method of the outer layer emulsion is the same as that of the inner layer emulsion.
The emulsion wraps the gel layer in the gel growth solution to form the lemon flavor sub-capsule.
Preparing the gel growth solution in percentage:
dripping the prepared inner-layer emulsion into the gel growth liquid by a dropper, wherein the aperture of the dropper is 1.5mm, slowly stirring during dripping, forming a layer of transparent gel layer on the surface of emulsion liquid drops to wrap the emulsion into spherical capsules, and gradually thickening the gel layer on the surfaces of the capsules along with the increase of the soaking time of the capsules in the gel growth liquid until the capsules reach a proper thickness. The gel growth time in this example was 5 min.
Solidifying and drying the lemon flavor sub-capsules.
Cleaning the capsule with deionized water, transferring to 5% CaCl2And (2) curing in the solution for 30min, washing the cured capsule with deionized water to clean the surface, transferring the capsule to a rotating cage for drying, wherein the drying time is 30 min-3 h, transferring the capsule to a ventilation place for drying after the capsule is dehydrated, cured and shaped and the surface has certain hardness, and in the drying process, only fat-soluble components are left in the emulsion in the capsule along with the gradual loss of water and the emulsion becomes transparent gradually until the emulsion is completely transparent, so that the inner-layer capsule is obtained, and the drying time is 1 h-12 h.
Nested capsules were prepared.
And uniformly coating the surface of the dried sub-capsule with the prepared outer-layer emulsion, putting the outer-layer emulsion into the growth liquid and slowly stirring, forming a transparent gel layer on the surface of the emulsion coating the capsule to coat the emulsion into a spherical capsule, and nesting the inner-layer capsule.
Curing and drying the nested capsules.
The curing and drying method of the nested capsule is the same as that of the son capsule, the nested capsule becomes transparent gradually along with the dissipation of emulsion moisture in the capsule, the capsule embedded in the inner layer is gradually shown, and when the inner layer and the outer layer of the capsule are transparent, the involucra of the capsule is dried, so that the secondary nested capsule with the lemon flavor in the inner layer and the sweet orange flavor in the outer layer is obtained.
In a further embodiment of the invention, a three-stage nested capsule can be manufactured using the nested capsule manufacturing method.
Specifically, the diameter of the outer layer of the three-level nested capsule is 4-5 mm, olive oil is arranged between the outer layer and the middle layer, the diameter of the middle-level capsule is 3-4 mm, MCT and vitamin complex are used as active ingredients between the middle layer and the inner layer, the diameter of the inner-level capsule is 2-3 mm, and astaxanthin with MCT as a solvent is wrapped by the inner layer. The preparation method comprises the following steps:
(A1) emulsification of the contents
The inner layer emulsion is prepared from the following components in percentage by weight: :
oil phase: 70%, wherein the oil phase comprises:
astaxanthin extract: 0.5 percent
And MCT: 69.5 percent; and
water phase: 30%, wherein the aqueous phase comprises:
adding xanthan gum into deionized water according to the above ratio, heating to 75 deg.C, stirring to completely melt, and sequentially adding CaCl2Stirring, dissolving and cooling Tween80 and glycerol to room temperature for later use; and uniformly mixing the astaxanthin extract and MCT, slowly adding the mixture into the water phase solution to be used, stirring and dispersing at the same time, wherein the rotating speed of a stirrer is more than or equal to 200r/min, the water phase and the oil phase gradually form an O/W type white emulsion with certain viscosity, and continuously stirring for 20-30 min to finish the preparation of the inner-layer emulsion.
Preparing a middle layer emulsion according to the following weight percentage:
oil phase: 75%, wherein the oil phase comprises:
fat-soluble vitamins: 1 percent of
And MCT: 74 percent; and
water phase: 25 percent of
The preparation method of the middle layer emulsion is the same as that of the inner layer emulsion.
The preparation proportion of the outer layer emulsion is as follows by weight percent:
oil phase: 75%, wherein the oil phase comprises:
olive oil: 75 percent; and
water phase: 25%, wherein the aqueous phase comprises:
the preparation method of the outer layer emulsion and the preparation method of the middle layer emulsion.
(A2) And preparing a gel growth solution.
The gel growth solution comprises the following components in percentage by weight:
dripping the prepared inner-layer emulsion into the gel growth liquid by a dropper, wherein the aperture of the dropper is 1.5mm, slowly stirring during dripping, forming a layer of transparent gel layer on the surface of emulsion liquid drops to wrap the emulsion into spherical capsules, and gradually thickening the gel layer on the surfaces of the capsules along with the increase of the soaking time of the capsules in the gel growth liquid until the capsules reach a proper thickness. The gel growth time for this example was 4 min.
(A3) Curing and drying the inner capsule
Cleaning the capsule with deionized water, transferring to 5% CaCl2And (2) curing in the solution for 30min, washing the cured capsule with deionized water to clean the surface, transferring the capsule to a rotating cage for drying, wherein the drying time is 30 min-3 h, transferring the capsule to a ventilation place for drying after the capsule is dehydrated, cured and shaped and the surface has certain hardness, and in the drying process, only fat-soluble components are left in the emulsion in the capsule along with the gradual loss of water and the emulsion becomes transparent gradually until the emulsion is completely transparent, so that the inner-layer capsule is obtained, and the drying time is 1 h-12 h.
(A4) Two-stage nested growth of capsules
And (3) uniformly coating the surface of the dried capsule with the middle-layer emulsion prepared in the step (A1), putting the middle-layer emulsion into the growth solution, slowly stirring, forming a transparent gel layer on the surface of the emulsion coating the capsule to coat the emulsion into a spherical capsule, and nesting the inner-layer capsule.
(A5) Curing and drying nested capsules
The curing and drying method of the nested capsule is the same as the step (A3), the capsule gradually becomes transparent along with the dissipation of the water in the emulsion in the capsule, the capsule embedded in the inner layer gradually appears, and the outer layer of the capsule is dried when the inner layer and the outer layer of the capsule are transparent.
(A6) Three-level nesting of capsules
And (3) uniformly coating the surface of the dried secondary nested capsule, putting the outer-layer emulsion prepared in the step (A1) into a growth solution, slowly stirring, forming a transparent gel layer on the surface of the emulsion coating the capsule to coat the secondary nested capsule, and simultaneously drying the capsule by using the same method in the step (A5) to obtain a tertiary nested capsule, wherein the diameter of the outer layer of the capsule is 4-5 mm, the diameter of the intermediate-layer capsule is 3-4 mm, the effective components of the tertiary nested capsule are MCT and vitamin complex, the diameter of the inner-layer capsule is 2-3 mm, and the tertiary nested capsule contains astaxanthin with MCT as a solvent.
In another embodiment of the invention, by adopting the preparation method of the nested capsule, a secondary nested capsule containing two small capsules in one capsule can be manufactured, the particle size of the outer capsule is 4-5 mm, the core liquid is salad oil in which powdered sugar is suspended, the diameter of the two inner capsules is 1-2 mm, the core liquid is MCT, and bifidobacterium powder is suspended. The preparation method comprises the following steps:
(B1) emulsification of the contents
The weight percentage of the inner layer microcapsule emulsion is as follows:
oil phase: 70%, wherein the oil phase comprises:
bifidobacterium powder: 0.05 percent
And MCT: 69.95 percent; and
water phase: 30%, wherein the aqueous phase comprises:
adding xanthan gum into deionized water according to the above ratio, heating to 75 deg.C, stirring to completely melt, and sequentially adding CaCl2Stirring, dissolving and cooling Tween80 and glycerol to room temperature for later use; adding bifidobacterium powder into salad oil, stirring and uniformly mixing, slowly adding the mixture into the solution of the water phase to be used, stirring and dispersing simultaneously, wherein the rotating speed of a stirrer is more than or equal to 200r/min, the water phase and the oil phase gradually form O/W type white emulsion with certain viscosity, and continuously stirring for 20-30 min to finish the preparation of the inner-layer emulsion.
The weight percentage of the prepared outer layer emulsion is as follows: :
oil phase: 75%, wherein the oil phase comprises:
salad oil: 70 percent of
Sugar powder: 5 percent; and
water phase: 25%, wherein the aqueous phase comprises:
the preparation method of the outer layer emulsion is the same as that of the inner layer emulsion.
(B2) And preparing a gel growth solution.
The weight percentage of the content gel growth solution is as follows:
the gel growth method of the inner layer microcapsule is the same as that of example 1 and example 2.
(B3) Curing and drying the inner capsule
The curing and drying methods of the inner layer microcapsules are the same as those of examples 1 and 2.
(B4) Two-stage nested growth of capsules
And (3) uniformly coating the surfaces of two dried capsules obtained in the step (1) with the outer-layer emulsion, putting the outer-layer emulsion into the growth liquid, slowly stirring, forming a transparent gel layer on the surface of the emulsion coating the capsules, coating the emulsion into spherical capsules, and simultaneously nesting the two small capsules.
(B5) Curing and drying nested capsules
The curing and drying methods of the nested capsules were the same as examples 1 and 2. And (3) drying to obtain a secondary nested capsule containing two small capsules in one capsule, wherein the core liquid of the outer layer is salad oil in which powdered sugar is suspended, the core liquid of the two capsules of the inner layer is MCT in which bifidobacterium powder is suspended.
It will be appreciated by persons skilled in the art that the embodiments of the invention described above and shown in the drawings are given by way of example only and are not limiting of the invention. The objects of the invention have been fully and effectively accomplished. The functional and structural principles of the present invention have been shown and described in the examples, and any variations or modifications of the embodiments of the present invention may be made without departing from the principles.
Claims (10)
1. A method for making a nested capsule, wherein the method for making the nested capsule comprises the steps of:
preparing O/W emulsified contents, wherein the contents are prepared from contents emulsion, wherein the contents emulsion comprises 50-80% of oil phase, 20-50% of water phase, 0.5-3% of curing agent, 0.5-2% of co-emulsifier, 0.1-3% of surfactant and 0.05-5% of co-surfactant according to weight percentage;
wrapping a gel layer on the outer surface of the O/W type emulsion drop in a gel growth solution to form the sub-capsule, wherein the gel growth solution comprises 0.1-3 wt% of a gel agent, 0.1-3 wt% of an auxiliary colloid and 0.05-4 wt% of a gel growth auxiliary agent, and the gel agent is sodium alginate;
curing and drying the sub-capsules;
nesting at least one transparent gel layer outside at least one of the sub-capsules by throwing at least one of the sub-capsules externally coated with an outer layer emulsion into a gel growth liquid to form a nested capsule; and
curing and drying the nested capsules.
2. The method of making nested capsules of claim 1, wherein the preparation of emulsified contents is carried out comprising the steps of:
(a) dissolving the coemulsifier with the corresponding proportion in the deionized water with the proportion range;
(b) dissolving a curing agent and a surfactant in the deionized water solution;
(c) slowly adding the uniformly mixed fat-soluble solvent and functional ingredients into the deionized water solution in the step (b);
(d) stirring the deionized water solution in the dispersing step (c) to form a white emulsion of oil phase/water (O/W) phase type; and
(e) stirring is continued for 20min to 30min, and the solution is cooled to room temperature.
3. The method for preparing a nested capsule of claim 2, wherein in step (e), the rotation speed of stirring is greater than or equal to 200 r/min.
4. The method for preparing the nested capsule of claim 2, wherein the emulsion viscosity is in the range of 2000 to 20000 cps.
5. The method of making a nested capsule of claim 1, wherein curing and drying the sub-capsule comprises the steps of: washing the prepared sub-capsules with deionized water to clean the surfaces, and transferring the sub-capsules into a divalent metal ion solution with the mass concentration of 0.5-20% for curing for 10 min-2 h;
and (3) washing the cured sub-capsules with deionized water to clean the surfaces of the sub-capsules, drying for 30 min-3 h, transferring the sub-capsules to a ventilation place for drying until the sub-capsules are completely transparent after the sub-capsules are dehydrated, cured and shaped and the surfaces of the sub-capsules have certain hardness, wherein the drying time is 1 h-12 h.
6. The method for preparing the nested capsule of claim 1, wherein the viscosity of the outer emulsion is 8000 to 20000 cps.
7. The method for preparing the nested capsule of claim 6, wherein the outer emulsion comprises 50-80% of oil phase, 20-50% of water phase, 0.5-3% of curing agent, 1-3% of co-emulsifier, 0.1-3% of surfactant and 0.05-5% of co-surfactant by weight percentage.
8. The method of making the nested capsule of claim 1, wherein the curing agent is a divalent or polyvalent metal ion comprising: ca2+、Ba2+、Mg2+One or more of (a).
9. The method of making nested capsules of claim 1, wherein the method of making nested capsules comprises the steps of:
nesting at least one transparent gel layer outside at least one nested capsule by putting the nested capsule coated with an outer layer emulsion into gel growth liquid to form a plurality of layers of nested capsules, wherein the gel growth liquid comprises 0.1-3% of gelling agent, 0.1-3% of auxiliary colloid and 0.05-4% of gel growth auxiliary agent in weight ratio; and
curing and drying the multi-layered wrapped nested capsules.
10. A nested capsule, wherein the nested capsule is prepared by the process for preparing a nested capsule as claimed in claims 1 to 9.
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