Capsule preparation method for removing peculiar smell of gelatin capsule shell

Abstract

The invention discloses a capsule preparation method for removing peculiar smell of a gelatin capsule shell, and relates to the technical field of capsule preparation products. Comprising the following steps: heating and mixing gelatin particles and purified water, adding a calcium phosphate compound, and filtering to obtain a first glue solution; adding a plasticizer into the first glue solution, stirring, controlling the viscosity, and degassing to obtain a second glue solution; and pressing the gelatin liquid into two half membranes by adopting a rotary mold pressing method, filling medicines, performing hot-pressing sealing, and drying and sterilizing the product to obtain the odorless gelatin capsule. The preparation method provided by the invention can efficiently remove the peculiar smell of the gelatin capsule shell.

Description

Technical Field

[0001] The present invention relates to the field of capsule preparation products, and particularly relates to a method for preparing capsules to remove the odor of gelatin capsule shells. Background Art

[0002] Gelatin is mainly made by extracting collagen from animal tissues such as bovine bones and pig skins, and may contain a small amount of residual grease. When gelatin is used to prepare edible capsules, oil-phase lubricants are also used in the production process. After steps such as sterilization of the hot-pressed capsules, temperature, pressure, light radiation, etc. will cause the proteins in the gelatin to denature and the oil-phase lubricants to decompose, releasing odoriferous gases such as sulfides and amines, resulting in poor odor of the edible capsules.

[0003] Currently developed plant-based capsules can improve the odor problem, but they may still have a slight sour or solvent odor of cellulose derivatives remaining, and the production cost is significantly higher than that of gelatin capsules.

[0004] Therefore, a preparation method is needed to remove the odor of the gelatin capsule shell. Summary of the Invention

[0005] The present invention is made in view of the above problems, and provides a method for preparing capsules to remove the odor of gelatin capsule shells.

[0006] The first aspect of the present invention provides a method for preparing capsules to remove the odor of gelatin capsule shells, comprising the following steps: heating and mixing gelatin particles with purified water, adding a calcium phosphate compound, filtering to obtain a first glue solution; adding a plasticizer to the first glue solution, stirring, controlling the viscosity and degassing to obtain a second glue solution; using a rotary molding method to press the glue into two half membranes, filling with drugs and then hot-pressing and sealing, and then drying and sterilizing the product to obtain odorless gelatin capsules.

[0007] In some embodiments of the present invention, the mass ratio of the gelatin particles to the purified water is (60 - 80):(70 - 100).

[0008] In some embodiments of the present invention, the calcium phosphate compound includes at least one of hydroxyapatite, dicalcium phosphate, and amorphous calcium phosphate.

[0009] In some embodiments of the present invention, the added mass of the plasticizer is 30 wt% - 70 wt% of the dry weight of the gelatin particles.

[0010] In some embodiments of the present invention, the plasticizer is a plasticizer mixed with glycerol, sorbitol, and polyethylene glycol in a mass ratio of 7:3:(0.1 - 0.5).

[0011] In some embodiments of the present invention, the viscosity is 3000 mPa·s - 5000 mPa·s.

[0012] In some embodiments of the present invention, the drying includes air-drying the semi-finished capsules in a rotating cage, and the rotating cage includes an oil-absorbing cloth soaked with a solvent.

[0013] In some embodiments of the present invention, the solvent is a mixed solvent of isopropyl alcohol and ethanol with a volume ratio of (3-5):2.

[0014] In some embodiments of the present invention, the air volume in the rotating cage is 2000 3 / h to 3500 m 3 / h.

[0015] In some embodiments of the present invention, the rotation speed of the rotating cage is 15 rpm to 20 rpm.

[0016] Beneficial effects that the present invention can achieve:

[0017] The present invention provides a method for preparing capsules to remove the odor of the gelatin capsule shell. Through physical adsorption and chemical bonding, the calcium phosphate compound effectively captures odor molecules such as residual sulfides and amines in the gelatin. Combining with the process design of high-efficiency solvent volatilization, air volume, and rotation speed in the rotating cage drying, the low-cost and high-efficiency removal of the odor of the gelatin capsule is achieved from both the material itself and the solvent removal operation. Detailed implementation manners

[0018] The following description is provided to enable those skilled in the art to fully understand the present invention and is not intended to limit the subject matter recited in the claims.

[0019] The "range" disclosed in the present invention is defined in the form of a lower limit and an upper limit. A given range is defined by selecting a lower limit and an upper limit, and the selected lower limit and upper limit define the boundary of a specific range. The range defined in this way can include the end values or not include the end values, and can be combined arbitrarily, that is, any lower limit can be combined with any upper limit to form a range. For example, if ranges of 60-120 and 70-100 are listed for a specific parameter, ranges of 60-110 and 80-120 are also contemplated. In addition, if the minimum range values 1 and 2 are listed, and if the maximum range values 3, 4, and 5 are listed, the following ranges are all contemplated: 1-3, 1-4, 1-5, 2-3, 2-4, and 2-5. In the present invention, unless otherwise specified, the numerical range "a-b" represents an abbreviated representation of any real number combination between a and b, where a and b are both real numbers. For example, the numerical range "0-5" means that all real numbers between "0-5" have been fully listed herein, and "0-5" is only an abbreviated representation of these numerical combinations. Additionally, when stating that a certain parameter is an integer ≥2, it is equivalent to disclosing that the parameter is, for example, the integer 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, etc.

[0020] Unless otherwise specified, all embodiments and optional embodiments of the present invention can be combined with each other to form new technical solutions.

[0021] Unless otherwise specified, all technical features and optional technical features of the present invention can be combined with each other to form new technical solutions.

[0022] Unless otherwise specified, all steps of the present invention can be carried out sequentially or randomly, and preferably sequentially. For example, the method includes steps (a) and (b), which means that the method may include steps (a) and (b) carried out sequentially, or may include steps (b) and (a) carried out sequentially. For example, it is mentioned that the method may further include step (c), which means that step (c) can be added to the method in any order. For example, the method may include steps (a), (b) and (c), or may include steps (a), (c) and (b), or may include steps (c), (a) and (b), etc.

[0023] Gelatin is mainly made by extracting collagen from animal tissues such as bovine bones and pig skins, and may contain a small amount of residual grease. When gelatin is used to prepare edible capsules, an oil-phase lubricant is also used in the production process. After steps such as sterilization of the hot-pressed capsules, temperature, pressure, light radiation, etc. will cause the protein in the gelatin to denature and the oil-phase lubricant to decompose, releasing odoriferous gases such as sulfides and amines, resulting in poor smell of the edible capsules.

[0024] The currently developed plant-based capsules can improve the odor problem, but they may still have a slight sour or solvent smell of cellulose derivatives remaining, and the production cost is significantly higher than that of gelatin capsules.

[0025] Therefore, a preparation method is needed to remove the odor of the gelatin capsule shell.

[0026] In view of this, this solution proposes a capsule preparation method for removing the odor of the gelatin capsule shell, including the following steps:

[0027] S1: Heat and mix gelatin particles with purified water, add a calcium phosphate compound, and filter to obtain a first glue solution;

[0028] S2: Add a plasticizer to the first glue solution, stir, control the viscosity and degas to obtain a second glue solution;

[0029] S3: Adopt the rotary die pressing method to press the glue into two half membranes, fill with drugs and then hot press and seal, and then dry and sterilize the product to obtain a gelatin capsule without odor.

[0030] In some embodiments, the gelatin particles are mixed with purified water in proportion, and stirred and dissolved in a water bath at 40°C to 50°C to form a uniform glue solution.

[0031] In some embodiments, the calcium phosphate compound added is in the form of powder particles with a Dv50 particle size of 1 μm to 5 μm. In some embodiments, the calcium phosphate compound modified with carboxyl or amino groups has stronger surface chemical adsorption ability and better odor removal effect. In some embodiments, the stirring adsorption time after adding the calcium phosphate compound is 30 min to 60 min.

[0032] The calcium phosphate compound in this solution effectively captures odor molecules such as residual sulfides and amines in gelatin through physical adsorption and chemical bonding, and combines with process designs such as efficient volatile solvents, air volume, and rotation speed in rotary cage drying to achieve low-cost and efficient removal of the odor of gelatin capsules from both the material itself and the solvent removal operation.

[0033] In some embodiments, the mass ratio of the gelatin particles to the purified water is (60 - 80):(70 - 100). When the ratio of the gelatin particles to the purified water is within the above range, problems such as cloudy glue liquid or brittle capsules can be avoided, which is beneficial for subsequent filtration operations and is also beneficial for adapting to the plasticizer in this solution.

[0034] In some embodiments, the calcium phosphate compound includes at least one of hydroxyapatite, dicalcium phosphate, and amorphous calcium phosphate. The calcium phosphate compound needs to meet the requirements of "GB 1886.3 - 2016" (China) for impurities (arsenic ≤ 3 ppm, lead ≤ 4 ppm). In some embodiments, the calcium phosphate compound is preferably hydroxyapatite or amorphous calcium phosphate, and the raw material cost of the calcium phosphate compound does not exceed 5% of the total cost of the capsule raw materials.

[0035] In some embodiments, the added mass of the plasticizer is 30 wt% to 70 wt% of the dry weight of the gelatin particles. The plasticizer is used to enhance the flexibility of the capsule.

[0036] In some embodiments, the plasticizer is a plasticizer mixed with glycerol, sorbitol, and polyethylene glycol in a mass ratio of 7:3:(0.1 - 0.5). The ternary plasticizer compounding reduces the glycerol migration rate, stabilizes the colloidal structure through a hydrogen bond network, controls the water content of the capsule, and significantly optimizes the flexibility and low-temperature anti-brittleness.

[0037] In some embodiments, the viscosity is 3000 mPa·s to 5000 mPa·s. When the viscosity of the glue liquid is within this range, the defective sealing rate of the capsule can be significantly reduced, and the water content is appropriate, which is beneficial for improving the drying efficiency.

[0038] In some embodiments, the drying includes air-drying the semi-finished capsules in a rotary cage, and the rotary cage includes an oil-absorbing cloth soaked with a solvent. The oil-absorbing cloth can be non-woven fabric, polypropylene fiber cloth, cotton cloth, etc.

[0039] In some embodiments, the solvent is a mixed solvent of isopropyl alcohol and ethanol with a volume ratio of (3 to 5):2. The mixed solvent reduces the surface tension of the mixed solution, accelerates penetration, volatilizes rapidly, and carries small-molecule odor substances out.

[0040] In some embodiments, the air volume in the rotating cage is 2000 3 / h to 3500 m 3 / h.

[0041] In some embodiments, the rotation speed of the rotating cage is 15 rpm to 20 rpm. By setting the process parameters of the rotating cage to cooperate with the solvent, the drying time can be shortened by about 30%.

[0042] The technical solutions of the present invention will be further described in detail below in conjunction with specific embodiments. It should be understood that the following specific embodiments are only used to explain the present invention and are not used to limit the present invention.

[0043] Example 1

[0044] Mix 75 g of gelatin particles with 85 g of purified water, stir and dissolve in a 45°C water bath. Add 35 g of hydroxyapatite (particle size Dv50 is 3 μm) to the above-mentioned glue solution, stir and adsorb for 40 minutes. After filtering out the hydroxyapatite, the first glue solution is obtained;

[0045] Add a plasticizer (glycerol, sorbitol, polyethylene glycol mixed in a mass ratio of 7:3:0.3) to the first glue solution. The addition amount of the plasticizer is 50 wt% of the dry weight of the gelatin particles. After stirring evenly, control the viscosity of the glue solution to 4000 mPa·s and perform degassing treatment to obtain the second glue solution;

[0046] Use the rotary molding method to press the glue solution into two half membranes, fill with drugs, seal by hot pressing, and place in a rotating cage for air drying. Place a non-woven oil-absorbing cloth soaked with a mixed solvent of isopropyl alcohol and ethanol with a volume ratio of 3:2 in the rotating cage. Set the air volume in the rotating cage to 2500 m 3 / h, the rotation speed is 18 rpm, and then perform sterilization treatment to obtain odorless gelatin capsules.

[0047] Example 2

[0048] Mix 70 g of gelatin particles with 70 g of purified water, stir and dissolve in a 50°C water bath. Add 38 g of dicalcium phosphate (particle size Dv50 is 5 μm), stir and adsorb for 30 minutes. After filtering, the first glue solution is obtained;

[0049] Add a plasticizer (mass ratio of glycerol:sorbitol:polyethylene glycol = 7:3:0.5) to the first glue solution. The addition amount is 38 wt% of the dry weight of the gelatin. Adjust the viscosity of the glue solution to 3500 mPa·s and perform degassing treatment to obtain the second glue solution;

[0050] Rotary die pressing for film formation, hot pressing and sealing after filling with drugs. Place an oil absorbent cloth with V isopropanol:V ethanol = 4:1 in the rotating cage, with an air volume of 3000 m 3 / h, a rotation speed of 20 rpm, and then perform sterilization treatment to obtain odorless gelatin capsules.

[0051] Example 3

[0052] Mix 80 g of gelatin particles with 90 g of purified water, dissolve in a 40°C water bath, add 53 g of dicalcium phosphate (particle size Dv50 is 10 μm), adsorb for 60 minutes, and filter to obtain the first gelatin solution;

[0053] Add a plasticizer (mass ratio of glycerol:sorbitol = 6:4), with an addition amount of 55 wt%, adjust the viscosity to 5000 mPa·s, and perform degassing treatment to obtain the second gelatin solution;

[0054] The solvent in the rotating cage is pure ethanol, with an air volume of 2000 m 3 / h, a rotation speed of 15 rpm, and then perform sterilization treatment to obtain odorless gelatin capsules.

[0055] Example 4

[0056] The ratio of gelatin to purified water is 4:5 (80 g:100 g), add 85 g of amorphous calcium phosphate (particle size Dv50 is 5 μm), adsorb for 50 minutes, and filter to obtain the first gelatin solution;

[0057] The mass ratio of the plasticizer is glycerol:sorbitol:polyethylene glycol = 8:2:0.2, with an addition amount of 50 wt%, a viscosity of 4500 mPa·s, and perform degassing treatment to obtain the second gelatin solution;

[0058] The solvent in the rotating cage is V isopropanol:V ethanol = 3:2, with an air volume of 2800 m 3 / h, a rotation speed of 18 rpm, and then perform sterilization treatment to obtain odorless gelatin capsules.

[0059] Example 5

[0060] The air volume in the rotating cage is increased to 3500 m 3 / h, and other parameters are the same as in Example 1.

[0061] Example 6

[0062] The solvent in the rotating cage is changed to acetone:ethanol = 1:1 (volume ratio), and other references are made to Example 1.

[0063] Comparative Example 1

[0064] Omit the step of adding hydroxyapatite, and directly add a plasticizer to the gelatin solution, and other references are made to Example 1.

[0065] Comparative Example 2

[0066] The plasticizer used was only glycerol (added amount was 50 wt% of the dry weight of the gelatin particles), and the others were referred to Example 1.

[0067] Comparative Example 3

[0068] Instead of using a rotary cage dryer, a rotary dehumidification dryer was used, and the others were referred to Example 1.

[0069] Performance test:

[0070] The odor removal rate, drying duration, hardness, elasticity, and friability of the gelatin capsules obtained in the examples and comparative examples were measured, and the results were recorded in Table 1.

[0071] 1. Odor removal rate

[0072] Using a laboratory olfactometer SC300 Portable Olfactometer, the odor of the gelatin particles and the finished capsules was measured to determine the odor concentration (OU / m 3 ), and the odor removal rate was calculated.

[0073] 2. Drying duration

[0074] The time for the capsules after hot pressing to be dried in a rotary cage was directly recorded.

[0075] 3. Hardness

[0076] The hardness of the capsules was tested using a CHT-01 capsule elasticity and hardness tester, and the value was directly recorded.

[0077] 4. Friability

[0078] Take 50 samples and immediately place them one by one into a glass tube standing upright on a wooden board (with a thickness of 2 cm). The inner diameter of the glass tube is 26 mm, the length is 200 mm, and a cylindrical weight (made of polytetrafluoroethylene, with a diameter of 22 mm) weighing 20 g is freely dropped from the mouth of the glass tube to check whether the capsules are broken. The degree of breakage is divided into four levels: 0, 1, 2, and 3. Level 0 means no breakage, and level 3 means obvious breakage.

[0079] Record the above test results in Table 1.

[0080] Table 1: Characterization test results of Examples 1-2 and Comparative Examples 1-4

[0081] Odd smell removal rate / % Drying duration / h Hardness / N Friability / level Example 1 95 2.5 50 0 Example 2 92 3.5 48 1 Example 3 90 4.5 55 0 Example 4 93 4.5 52 1 Example 5 94 3.0 50 0 Example 6 88 2.5 48 2 Comparative example 1 60 4.0 45 2 Comparative example 2 85 4.5 40 2 Comparative example 3 70 5.5 50 1

[0082] It can be confirmed from the results in Table 1 that the odor component removal rates of Examples 1-4 using hydroxyapatite / calcium phosphate adsorbents are relatively high. In Comparative Example 1, no adsorbent was added, and the removal rate decreased significantly. In Example 6, acetone was used, which has high volatility but weak adsorption ability, and the removal rate decreased slightly.

[0083] The drying of Comparative Example 3 lacked solvent evaporation assistance, had a lower removal rate, and the longest drying time

[0084] The mixed plasticizers of glycerol, sorbitol, and polyethylene glycol (Examples 1-4) had a higher hardness and a lower friability. Comparative Example 2 used only glycerol, with insufficient plasticizing effect, the lowest hardness, and a higher friability. The synergistic effect between the adsorbent and the plasticizer is the key to improving the odor removal rate and mechanical properties. High air volume and mixed solvents can significantly shorten the drying time, but the influence of solvent selection on the quality of the gelatin film needs to be balanced. The results of the comparative examples verified the necessity of the adsorption, plasticization, and drying steps in the process of this solution.

[0085] For the capsule preparation method for removing the odor of the gelatin capsule shell in this solution, the calcium phosphate compound effectively captures odor molecules such as residual sulfides and amines in the gelatin through physical adsorption and chemical bonding, combined with the process design of high-efficiency solvent evaporation, air volume, rotation speed, etc. in rotary drying, realizing low-cost and high-efficiency removal of the odor of the gelatin capsule from both the material itself and the solvent removal operation.

[0086] It should be noted that the present invention is not limited to the above embodiments. The above embodiments are only examples, and embodiments having the same composition and the same effect as the technical idea within the technical scope of the present invention are all included in the technical scope of the present invention. In addition, within the scope not departing from the gist of the present invention, various modifications that can be conceived by those skilled in the art to the embodiments, and other ways constructed by combining some constituent elements of the embodiments are also included in the scope of the present invention.

Claims

1. A method for preparing capsules for removing the odor of gelatin capsule shells, characterized in that, The preparation method comprises the following steps: Mix gelatin particles with purified water by heating, add calcium phosphate compound, and filter to obtain a first glue solution; Add a plasticizer to the first glue solution, stir, control the viscosity and degas to obtain a second glue solution; Adopt the rotary die pressing method to press the glue into two half membranes, fill with drugs, seal by hot pressing, and then dry and sterilize the product to obtain a gelatin capsule without peculiar smell.

2. The method for preparing a capsule for removing the odor of the gelatin capsule shell according to claim 1, characterized in that, The mass ratio of the gelatin particles to the purified water is (60-80):(70-100).

3. The method for preparing a capsule for removing the odor of the gelatin capsule shell according to claim 1, characterized in that, The calcium phosphate compound comprises at least one of hydroxyapatite, dicalcium phosphate, and amorphous calcium phosphate.

4. The method for preparing a capsule for removing the odor of the gelatin capsule shell according to claim 1, wherein, The added mass of the plasticizer is 30wt%-70wt% of the dry weight of the gelatin particles.

5. The method for preparing a capsule for removing the odor of the gelatin capsule shell according to claim 4, characterized in that, The plasticizer is a plasticizer mixed with glycerol, sorbitol, and polyethylene glycol in a mass ratio of 7:3:(0.1-0.5).

6. The method for preparing capsules for removing the odor of gelatin capsule shells according to claim 1, characterized in that, The viscosity is 3000mPa·s-5000mPa·s.

7. The method for preparing a capsule for removing the odor of the gelatin capsule shell according to claim 1, wherein The drying includes air-drying the semi-finished capsules in a rotating cage, and the rotating cage includes an oil-absorbing cloth wetted with a solvent.

8. The method for preparing a capsule for removing the odor of the gelatin capsule shell according to claim 7, wherein The solvent is a mixed solvent of isopropyl alcohol and ethanol with a volume ratio of (3-5):

2.

9. The method for preparing a capsule for removing the odor of the gelatin capsule shell according to claim 7, wherein The air volume in the rotating cage is 2000 3 / h to 3500 m 3 / h.

10. The method for preparing a capsule for removing the odor of the gelatin capsule shell according to claim 9, characterized in that, The rotation speed of the rotating cage is 15rpm-20rpm.