A high oil content capsule formulation and a method of making the same

Abstract

The application provides a high-oil-content capsule preparation and a preparation method thereof, and relates to the technical field. The high-oil-content capsule preparation comprises the following raw materials in percentage by weight: oil microcapsule powder 20-80%, rice powder 1-42%, calcium hydrogen phosphate 2-12%, calcium silicate 1-6%, microcrystalline cellulose 1-21%, magnesium stearate 2-10% and silicon dioxide 1-10%. The application adopts calcium hydrogen phosphate, calcium silicate, magnesium stearate and silicon dioxide as the additives of the oil microcapsule powder, and through optimization of the ratio and the process, the oil capsule preparation with high content (50-80%) can be prepared, the production process will not cause the filling rod or the copper disc to be stuck, and the product loading is stable.

Description

TECHNICAL FIELD

[0001] The application relates to the technical field of capsule processes, in particular to a capsule preparation with high oil content and a preparation method thereof. BACKGROUND

[0002] Microcapsule refers to a micro container or wrapping with a polymer or inorganic wall. Microencapsulation is a technology of wrapping solid, liquid or gaseous active substances with materials. The microencapsulation technology can cover up the bad smell and odor of the wrapped substances, control the release speed and mode of the active substances, improve the matching degree of the active substances and the environment, reduce the incompatibility, and isolate oxygen, water and other factors affecting the stability of the active substances. The microencapsulation technology has been applied in many industrial fields for many years and there are many methods, such as pan coating process, spray drying, spray freezing, fluidized bed, sharp hole method, interfacial polymerization, in-situ polymerization and the like.

[0003] Powdered oil converts liquid oil into a flowable solid powder, which is beneficial for storage, transportation and use. The oil is wrapped by the film formed by the wall material, and the microcapsule forms a layer of protection for the oil in the core material, which can prevent the influence of oxygen, heat, light and other environmental and chemical substances on the oil, and prolong the storage period of the oil. Because the powdered oil has many advantages over the liquid oil, it is widely used in the fields of food and feed.

[0004] When producing capsules or tablets, if the addition amount of the oil / oil microcapsule powder or extract is too high, it is easy to stick to the filling rod or copper disc, and thus cannot be produced. Therefore, the addition amount of the oil / oil microcapsule powder or extract in the formula of the product is generally within 30%. SUMMARY

[0005] The application aims to provide a capsule preparation with high oil content, which has the advantage of high oil content (60-80%).

[0006] Another purpose of the application is to provide a preparation method of the capsule preparation with high oil content, which is simple and ingenious.

[0007] To solve the above technical problems, the application adopts the technical scheme of:

[0008] In one aspect, the application provides a capsule preparation with high oil content, which comprises the following raw materials in percentage by weight: oil microcapsule powder 20%-80%, rice powder 1%-42%, calcium hydrogen phosphate 2%-12%, calcium silicate 1%-6%, microcrystalline cellulose 1%-21%, magnesium stearate 2%-10% and silicon dioxide 1%-10%.

[0009] In another aspect, the present application provides a method for preparing a high oil content capsule preparation, comprising the following steps:

[0010] S1, the oil microcapsule powder, calcium silicate and silicon dioxide are sequentially put into a three-dimensional motion mixer, the total mixer speed is set to 10 rpm, the mixing time is 15 min, and the mixture is mixed until the color is uniform to obtain a premix;

[0011] S2, the premix, rice powder, calcium hydrogen phosphate, microcrystalline cellulose and magnesium stearate are put into a three-dimensional motion mixer, the total mixer speed is set to 10 rpm, the mixing time is 15 min, and the mixture is mixed until the color is uniform to obtain a mixture.

[0012] S3, the mixture is filled using a full-automatic capsule filling machine 0# mold, the production speed is 1100 particles / min, and the filling is debugged first. After the filling amount and the filling amount control range, the locking of the capsule, the appearance quality and the like meet the provisions, the formal production can be carried out. The filling amount is 420 mg / particle, the filling amount control range is 420 mg x (1±5%), and the disintegration time is ≤30 min.

[0013] The roles of the raw materials of the present application are as follows:

[0014] Magnesium stearate: also known as magnesium octadecanoate, it has the dual properties of metal salt and stearic acid. The inherent fat properties of stearic acid, including lubricity and water repellency, are retained in magnesium stearate. Magnesium stearate is a white or milky white uniform powder with a large specific surface area, and has strong adsorption and hygroscopicity. Food-grade magnesium stearate can be used as a food processing aid, mainly as a lubricant, anti-sticking agent and flow aid for tablets and capsules.

[0015] Silicon dioxide: silicon dioxide is a white and loose powder. According to the Chinese Pharmacopoeia, silicon dioxide is mainly used as a flow aid and a suspending agent. The surface of the oil / oil microcapsule powder is rough, and the addition of silicon dioxide can reduce the friction between particles, increase the bulk and tap densities, and reduce the compression degree, thereby improving the flowability.

[0016] Anhydrous calcium hydrogen phosphate: anhydrous calcium hydrogen phosphate is a white, odorless and tasteless powder or crystal, which exists in the form of triclinic crystal. Anhydrous calcium hydrogen phosphate has good flowability and stability, low hygroscopicity, and cannot be hydrated to form dihydrate. It is used as a filler in tablets and hard capsules to increase the volume and aid molding.

[0017] Calcium silicate: Calcium silicate is a white to off-white crystalline or amorphous powder, defined as different proportions of calcium oxide and silicon dioxide, including tricalcium silicate and dicalcium silicate, divided into two kinds of anhydrous and hydrated. Calcium silicate is obtained by reacting freshly matured lime with synthetic silicon dioxide. Calcium silicate is a loose porous structure with high oil and water absorption value. The calcium silicate covers the surface of the oil / oil microcapsule powder to form a protective film, which isolates the effect of external moisture on the material, thereby playing a role in anti-blocking and flow aid, and improving its bulk density.

[0018] Microcrystalline cellulose: Microcrystalline cellulose is a straight-chain polysaccharide combined by β-1, 4 glucoside bond, which is a natural polymer composed of free-flowing cellulose crystals. Microcrystalline cellulose is insoluble in water, dilute acid and oil, and has the functions of adhesion, molding, etc. It has low degree of polymerization (between 15-375) and large specific surface area. Microcrystalline cellulose can also reduce the friction between material particles and improve the flowability of the material. It can be used as a filler to increase the volume and assist the molding.

[0019] Compared with the prior art, the embodiments of the present application have at least the following advantages or beneficial effects:

[0020] The present application uses calcium hydrogen phosphate, magnesium stearate and silicon dioxide as the additives of oil / oil microcapsule powder. Through optimization of the ratio and process, high content (60-80%) oil / oil capsule preparation can be prepared, and the filling rod or copper disc will not be stuck during production. BRIEF DESCRIPTION OF DRAWINGS

[0021] In order to more clearly illustrate the technical solutions of the embodiments of the present application, the following will briefly introduce the drawings needed to be used in the embodiments. It should be understood that the following drawings only show some embodiments of the present application, and therefore should not be regarded as a limitation on the scope. For those skilled in the art, other related drawings can also be obtained without creative labor.

[0022] Figure 1 The three-dimensional motion mixer used in the embodiments of the present application;

[0023] Figure 2 The full-automatic capsule filling machine used in the embodiments of the present application;

[0024] Figure 3 The capsule product real object diagram prepared by the embodiments of the present application. DETAILED DESCRIPTION

[0025] In order to make the purposes, technical solutions, and advantages of the embodiments of the present application clearer, the technical solutions in the embodiments of the present application will be clearly and completely described below. The specific conditions are not indicated in the embodiments, and the conventional conditions or the conditions suggested by the manufacturers are adopted. The reagents or instruments are not indicated by the manufacturers, and are all conventional products that can be purchased in the market.

[0026] It should be noted that the embodiments in the present application and the features in the embodiments can be combined with each other without conflict. The present application will be described in detail below with reference to specific embodiments.

[0027] A high-oil-content capsule preparation, comprising the following raw materials in percentage by weight: oil microcapsule powder 20%-80%, rice powder 1%-42%, calcium hydrogen phosphate 2%-12%, calcium silicate 1%-6%, microcrystalline cellulose 1%-21%, magnesium stearate 2%-10%, and silicon dioxide 1%-10%.

[0028] In some embodiments of the present application, the high-oil-content capsule preparation comprises the following raw materials in percentage by weight: oil microcapsule powder 60%-80%, rice powder 1%-10%, calcium hydrogen phosphate 2%-6%, calcium silicate 1%-6%, microcrystalline cellulose 1%-6%, magnesium stearate 2%-7%, and silicon dioxide 2%-6%.

[0029] In some embodiments of the present application, the oil microcapsule powder is vitamin E powder, fish oil microcapsule powder, or lutein / lutein ester microcapsule powder.

[0030] In some embodiments of the present application, the content of VE in the vitamin E powder is 98%, and the total content of EPA and DHA in the fish oil microcapsule powder is 40%.

[0031] A preparation method of a high-oil-content capsule preparation, comprising the following steps:

[0032] S1, first mixing oil microcapsule powder, calcium silicate, and silicon dioxide until the color is uniform to obtain a premix;

[0033] S2, mixing the premix with other raw materials to obtain a mixture;

[0034] S3, filling the mixture into capsules.

[0035] In some embodiments of the present application, the mixing in the step S1 is specifically as follows: the oil microcapsule powder, the calcium silicate, and the silicon dioxide are sequentially put into a three-dimensional motion mixer, the rotation speed is set to 10 rpm, the mixing time is 15 min, and the premix is obtained by mixing until the color is uniform.

[0036] In some embodiments of the present application, the mixing in the above S2 step is specifically: the premix, rice powder, calcium hydrogen phosphate, microcrystalline cellulose and magnesium stearate are put into a three-dimensional motion mixer, the total mixer speed is set to 10 rpm, and the mixing time is 15 min; the mixture is obtained by mixing until the color is uniform.

[0037] In some embodiments of the present application, the capsule filling in the above S3 step is specifically: using a full-automatic capsule filling machine 0# mold to fill; the production speed is 1100 particles / min, the filling amount is 420 mg / particle, the mass of each particle is 420 mg x (1±5%), and the disintegration time is ≤30 min.

[0038] The features and performances of the present application are further described in detail below in combination with embodiments.

[0039] Embodiment 1

[0040] A high-oil-content capsule preparation is prepared by the following method:

[0041] A high-oil-content capsule preparation is prepared by the following method:

[0042] S1, preparing raw materials, weight percentage: vitamin E powder (VE content 98%) 60.00%, rice powder 10.00%, calcium hydrogen phosphate 6.00%, calcium silicate 6.00%, microcrystalline cellulose 6.00%, magnesium stearate 6.00% and silicon dioxide 6.00%;

[0043] S2, the oil microcapsule powder, calcium silicate and silicon dioxide are put into a three-dimensional motion mixer in order, as shown in Figure 1 , the total mixer speed is set to 10 rpm, the mixing time is 15 min, and the premix is obtained by mixing until the color is uniform;

[0044] S3, the premix, rice powder, calcium hydrogen phosphate, microcrystalline cellulose and magnesium stearate are put into a three-dimensional motion mixer, the total mixer speed is set to 10 rpm, the mixing time is 15 min, and the mixture is obtained by mixing until the color is uniform.

[0045] S4, the mixture is filled using a full-automatic capsule filling machine 0# mold, as shown in Figure 2 , the production speed is 1100 particles / min, and the filling process needs to be debugged first. After the filling amount and the filling amount control range, the locking of the capsule, the appearance quality and the like meet the regulations, formal production can be carried out. The filling amount is 420 mg / particle, and the capsule product is as shown in Figure 3 .

[0046] The production process of the product of the present embodiment is smooth, the filling amount is stable (±3.9%) and meets the requirements, the filling rod is not sticky, and the copper disc is not sticky. The disintegration time is 17 min.

[0047] Example 2

[0048] A high oil content capsule preparation is prepared by the following method:

[0049] S1, prepare raw materials, weight percentage: vitamin E powder (VE content 98%) 80.00%, rice powder: 1.00%, calcium hydrogen phosphate 2.00%, calcium silicate: 3.00%, microcrystalline cellulose: 1.00%, magnesium stearate 7.00% and silicon dioxide 6.00%;

[0050] S2, the oil microcapsule powder, calcium silicate and silicon dioxide are sequentially put into a three-dimensional motion mixer, the total mixer speed is set to 10 rpm, the mixing time is 15 min, and the mixture is mixed until the color is uniform to obtain a premix;

[0051] S3, the premix, rice powder, calcium hydrogen phosphate, microcrystalline cellulose, magnesium stearate are put into a three-dimensional motion mixer, the total mixer speed is set to 10 rpm, the mixing time is 15 min, and the mixture is mixed until the color is uniform to obtain a mixture.

[0052] S4, the mixture is filled using a full-automatic capsule filling machine 0# mold, the production speed is 1100 particles / min, and the filling is debugged first. After the filling amount and the filling amount control range, the locking of the capsule, the appearance quality and the like meet the regulations, formal production can be carried out. The filling process has a filling amount of 420 mg / particle.

[0053] The product production process of this embodiment is smooth, the filling amount is stable (±5.0%) and meets the requirements, does not stick to the filling rod and does not stick to the copper disc. The disintegration time is 15 min.

[0054] Example 3

[0055] A high oil content capsule preparation is prepared by the following method:

[0056] S1, prepare raw materials, weight percentage: vitamin E powder (VE content 98%) 80.00%, rice powder: 1.00%, calcium hydrogen phosphate 2.00%, calcium silicate: 3.00%, microcrystalline cellulose: 1.00%, magnesium stearate 7.00% and silicon dioxide 6.00%;

[0057] S2, the oil microcapsule powder, calcium silicate and silicon dioxide are sequentially put into a three-dimensional motion mixer, the total mixer speed is set to 10 rpm, the mixing time is 15 min, and the mixture is mixed until the color is uniform to obtain a premix;

[0058] S3, the premix, rice powder, calcium hydrogen phosphate, microcrystalline cellulose, magnesium stearate are put into a three-dimensional motion mixer, the total mixer speed is set to 10 rpm, the mixing time is 15 min, and the mixture is mixed until the color is uniform to obtain a mixture.

[0059] S4, the mixture is filled with a full-automatic capsule filling machine 0# mold, the production speed is 1100 particles / min, and the filling needs to be debugged first. After the filling amount and the filling amount control range, the locking of the capsule, the appearance quality and the like meet the provisions, formal production can be carried out. The filling amount is 420 mg / particle.

[0060] The production process of the product of the example is smooth, the filling amount is stable (±3.2%) and meets the requirements, the filling rod is not sticky, and the copper disc is not sticky. The disintegration time is 15 min.

[0061] Example 4

[0062] A high-oil-content capsule preparation is prepared by the following method:

[0063] A high-oil-content capsule preparation is prepared by the following method:

[0064] S1, prepare raw materials, the weight percentage: vitamin E powder (VE content 98%) 30.00%, rice powder 22.00%, calcium hydrogen phosphate 30.00%, calcium silicate 3.00%, microcrystalline cellulose 5.00%, magnesium stearate 5.00% and silicon dioxide 5.00%;

[0065] S2, the oil microcapsule powder, calcium silicate and silicon dioxide are sequentially put into a three-dimensional motion mixer, the total mixer speed is set to 10 rpm, the mixing time is 15 min, and the color is uniformly mixed to obtain a premix;

[0066] S3, the premix, rice powder, calcium hydrogen phosphate, microcrystalline cellulose, magnesium stearate are put into a three-dimensional motion mixer, the total mixer speed is set to 10 rpm, the mixing time is 15 min, and the color is uniformly mixed to obtain a mixture.

[0067] S4, the mixture is filled with a full-automatic capsule filling machine 0# mold, the production speed is 1100 particles / min, and the filling needs to be debugged first. After the filling amount and the filling amount control range, the locking of the capsule, the appearance quality and the like meet the provisions, formal production can be carried out. The filling amount is 420 mg / particle.

[0068] The production process of the product of the example is smooth, the filling amount is stable (±4.7%) and meets the requirements, the filling rod is not sticky, and the copper disc is not sticky. The disintegration time is 12 min.

[0069] Example 5

[0070] A high-oil-content capsule preparation is prepared by the following method:

[0071] A high-oil-content capsule preparation is prepared by the following method:

[0072] S1, preparing raw materials, weight percentage: vitamin E powder (VE content 98%) 85.00%, rice flour 1.00%, calcium hydrogen phosphate 3.00%, calcium silicate 4%, microcrystalline cellulose 2%, magnesium stearate 2.00% and silicon dioxide 3.00%;

[0073] S2, the oil microcapsule powder, calcium silicate and silicon dioxide are sequentially put into a three-dimensional motion mixer, the total mixer speed is set to 10 rpm, the mixing time is 15 min, and the mixture is mixed until the color is uniform to obtain a premix;

[0074] S3, the premix, rice flour, calcium hydrogen phosphate, microcrystalline cellulose and magnesium stearate are put into a three-dimensional motion mixer, the total mixer speed is set to 10 rpm, the mixing time is 15 min, and the mixture is mixed until the color is uniform to obtain a mixture.

[0075] S4, the mixture is filled using a full-automatic capsule filling machine 0# mold, the product in this embodiment has a high vitamin E powder addition amount, the production process is not smooth, the loading amount difference fluctuates greatly by 8.7%, the material sticks to the filling rod, and the copper disc is stuck. Trial production failed.

[0076] Comparative Example 1

[0077] S1, preparing raw materials, weight percentage: vitamin E powder (VE content 98%) 85.00%, rice flour 1.00%, calcium hydrogen phosphate 3.00%, calcium silicate 4%, microcrystalline cellulose 2%, magnesium stearate 2.00% and silicon dioxide 3.00%;

[0078] S2, the vitamin E powder, calcium silicate and silicon dioxide are first added to the equipment, the total mixer speed is set to 10 rpm, the mixing time is 15 min, and the mixture is mixed until the color is uniform to obtain a premix;

[0079] S3, the premix, rice flour, microcrystalline cellulose and magnesium stearate are put into a three-dimensional motion mixer, the total mixer speed is set to 10 rpm, the mixing time is 15 min, and the mixture is mixed until the color is uniform to obtain a mixture.

[0080] S4, the mixture is filled using a full-automatic capsule filling machine 0# mold, the product in this embodiment has a high vitamin E powder addition amount, the production process is not smooth, the loading amount difference fluctuates greatly by 8.7%, the material sticks to the filling rod, and the copper disc is stuck. Trial production failed.

[0081] Comparative Example 2

[0082] S1, prepare raw materials, weight percentage: vitamin E powder (VE content 98%) 50.00%, rice flour 40.00%, calcium hydrogen phosphate 4.00%, calcium silicate 0.00%, microcrystalline cellulose 2.00%, magnesium stearate 2.00% and silicon dioxide 2.00%;

[0083] S2, first add vitamin E powder and silicon dioxide into the equipment, set the total mixer speed to 10 rpm, mixing time 15 min, mix until the color is uniform, get the premix;

[0084] S3, put the premix, rice flour, calcium hydrogen phosphate, microcrystalline cellulose, magnesium stearate into the three-dimensional motion mixer, set the total mixer speed to 10 rpm, mixing time 15 min, mix until the color is uniform to get the mixture.

[0085] S4, fill the mixture using the full-automatic capsule filling machine 0# mold, this comparative example does not contain calcium silicate, resulting in an unsmooth production process, the loading amount difference fluctuates greatly by 9.1%, the material sticks to the filling rod, and the trial production fails.

[0086] Comparative Example 3

[0087] S1, prepare raw materials, weight percentage: vitamin E powder (VE content 98%) 50.00%, rice flour 40.00%, calcium hydrogen phosphate 4.00%, calcium silicate 2.00%, microcrystalline cellulose 2.00%, magnesium stearate 2.00% and silicon dioxide 0.00%;

[0088] S2, first add vitamin E powder and silicon dioxide into the equipment, set the total mixer speed to 10 rpm, mixing time 15 min, mix until the color is uniform, get the premix;

[0089] S3, put the premix, rice flour, calcium hydrogen phosphate, microcrystalline cellulose, magnesium stearate into the three-dimensional motion mixer, set the total mixer speed to 10 rpm, mixing time 15 min, mix until the color is uniform to get the mixture.

[0090] S4, fill the mixture using the full-automatic capsule filling machine 0# mold, this comparative example does not contain calcium silicate, resulting in an unsmooth production process, the loading amount difference fluctuates greatly by 9.1%, the material sticks to the filling rod, and the trial production fails.

[0091] The above-described embodiments are part of the embodiments of the present application, not all. The detailed description of the embodiments of the present application is not intended to limit the scope of the claimed application, but only represents selected embodiments of the present application. Based on the embodiments in the present application, all other embodiments obtained by those of ordinary skill in the art without creative labor are within the scope of protection of the present application.

Claims

1. A high oil content encapsulated formulation characterized in that, The oil and fat microcapsule powder is made of the following raw materials in percentage by weight: oil and fat microcapsule powder 60%-80%, rice powder 1%-10%, calcium hydrogen phosphate 2%-6%, calcium silicate 1%-6%, microcrystalline cellulose 1%-6%, magnesium stearate 2%-7%, and silicon dioxide 2%-6%. The oil and fat microcapsule powder is vitamin E powder, fish oil microcapsule powder, or lutein / lutein ester microcapsule powder.

2. A high oil content capsule formulation according to claim 1, characterised in that, The content of VE in the vitamin E powder is 98%, and the total content of EPA and DHA in the fish oil microcapsule powder is 40%.

3. A process for the preparation of a high oil content encapsulated formulation as claimed in any one of claims 1-2, characterized in that, The method comprises the following steps: S1, first mix the oil and fat microcapsule powder, calcium silicate, and silicon dioxide until the color is uniform to obtain a premix; S2, mix the premix with other raw materials to obtain a mixture; S3, fill the mixture into capsules.

4. A process for the preparation of a high oil content encapsulated formulation according to claim 3, characterised in that, The mixing in the S1 step is specifically as follows: the oil and fat microcapsule powder, calcium silicate, and silicon dioxide are sequentially put into a three-dimensional motion mixer, the rotation speed is set to 10 rpm, the mixing time is 15 min, and the premix is obtained after mixing until the color is uniform.

5. A process for the preparation of a high oil content encapsulated formulation according to claim 3, characterized in that, The mixing in the S2 step is specifically as follows: the premix, rice powder, calcium hydrogen phosphate, microcrystalline cellulose, and magnesium stearate are put into a three-dimensional motion mixer, the total mixing rotation speed is set to 10 rpm, the mixing time is 15 min, and the mixture is obtained after mixing until the color is uniform.

6. A process for the preparation of a high oil content encapsulated formulation according to claim 3, characterized in that, The capsule filling in the S3 step is specifically as follows: a full-automatic capsule filling machine 0# mold is used for filling, the production speed is 1100 capsules / min, the filling amount is 420 mg / capsule, the mass of each capsule is 420 mg×(1±5%), and the disintegration time is ≤30 min.

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