Plant rubber composition and preparation method thereof

Abstract

The invention belongs to the technical field of soft capsule shells, and particularly relates to a plant capsule shell composition and a preparation method thereof. The potato starch is subjected to enzymolysis modification through beta-1, 3-glucanase and pectinesterase, the disadvantage that natural starch is too large in viscosity is overcome, the potato starch is compounded with the hydroxypropyl starch and the wheat starch, the starch viscosity is effectively reduced, meanwhile, the gelatinization characteristic is improved, and gel is rapidly formed; the fluidity of the glue solution meets the requirements of pelleting equipment, and the disintegration performance is stable; aspergillus niger saccharifying enzyme and beta-glucanase are used for carrying out enzymolysis modification on the plant powder, and then the plant powder is mixed with hydroxypropyl methyl cellulose, so that a tough gel network of the plant capsule is facilitated, the rubber binding rate is increased, the oil leakage problem of the plant capsule is reduced, and the integrity of the capsule is improved. Therefore, the technical scheme provided by the invention is simple and convenient to operate, and the obtained rubber is high in integrity and stable in disintegration performance.

Description

Technical Field

[0001] This invention belongs to the field of soft capsule coating technology, specifically relating to a plant-based coating composition and its preparation method. Background Technology

[0002] The outer shell of a soft capsule is a thin film that encapsulates the contents (oils, suspensions, etc.). Its main functions are to protect the contents, facilitate administration, and control release. Therefore, it needs to have good film-forming and sealing properties, be able to isolate air and moisture to prevent oxidation or deterioration of the contents, and gradually dissolve in water to allow the contents to be released and absorbed in the gastrointestinal tract.

[0003] There are currently many reports on plant-based gelatin. For example, in Chinese patent CN 110075081 A, a plant-based soft capsule and its preparation method and uses, the weight-average molecular weight of carrageenan is controlled at 1.2 × 10⁻⁶. 6 -2.0×10 6 It can be combined with starch, plasticizer and water to prepare high-performance plant soft capsules with low production cost, but the preparation process is relatively complex. For example, in Chinese patent CN 110507629 A, a method for preparing a resistant cellulin soft capsule shell is described, in which 72.2-80.2 parts of purified water, 20-25 parts of resistant cellulin, 0.8-1.2 parts of gelling agent, 0.05-0.15 parts of preservative, 0.05-0.15 parts of opacifier, and 0.05-0.15 parts of pigment are mixed to prepare the soft capsule shell. Although this method reduces the safety risks of animal products, the preparation method is cumbersome and the disintegration performance is unstable. Therefore, if a plant-based rubber composition that is easy to prepare, has high integrity, and stable disintegration properties can be provided, it will be beneficial to promote the rapid development of this field. Summary of the Invention

[0004] The purpose of this invention is to provide a plant-based rubber composition and its preparation method, which is not only simple to prepare but also has the advantages of high integrity and stable disintegration performance.

[0005] This invention provides a method for preparing a plant-based rubber composition, comprising the following steps: Potato starch, β-1,3-glucanase, pectin esterase and water were mixed for the first enzymatic hydrolysis to obtain the first hydrolysate; The first enzymatic hydrolysate was subjected to enzyme inactivation and first vacuum drying to obtain resistant potato starch; Hydroxypropyl starch, resistant potato starch, and wheat starch are mixed evenly to obtain a first mixture; After the plant powder was cooled by a program, it was mixed with Aspergillus niger saccharifying enzyme, β-glucanase and water for a second enzymatic hydrolysis to obtain a second enzymatic hydrolysate. The second enzymatic hydrolysate was subjected to enzyme inactivation and then vacuum drying to obtain resistant cellulose; Hydroxypropyl methylcellulose and resistant cellulose are mixed evenly to obtain a second mixture; The first mixture, pullulan, carrageenan, gellan gum, konjac flour, mannitol, sorbitol, the second mixture, and water are mixed evenly to obtain a plant rubber composition. The first mixture comprises: hydroxypropyl starch, resistant potato starch, and wheat starch; The second mixture comprises hydroxypropyl methylcellulose and resistant cellulose.

[0006] Preferably, the plant powder includes: chicory powder or barley leaf powder.

[0007] Preferably, the plant-based rubber composition comprises the following raw materials by weight percentage: The first mixture consists of 12%-22% pullulan, 0.5%-1% carrageenan, 0.5%-1% gellan gum, 0.8%-1.2% konjac flour, 1%-1.5% mannitol, 5%-10% sorbitol, the second mixture consists of 6%-12% and the remainder is water.

[0008] Preferably, in the first mixture, the mass ratio of hydroxypropyl starch, resistant potato starch and wheat starch is 1-1.5:6-8:2-2.5.

[0009] Preferably, the mass ratio of hydroxypropyl methylcellulose to resistant cellulose in the second mixture is 1-1.5:1.

[0010] Preferably, during the first enzymatic hydrolysis, the mass ratio of potato starch, β-1,3-glucanase, pectin esterase, and water is 10:0.2-0.4:0.6-0.8:20-30; The first enzymatic hydrolysis is performed at a temperature of 70-80℃ for 6-8 hours.

[0011] Preferably, during the second enzymatic hydrolysis, the mass ratio of plant powder to Aspergillus niger saccharifying enzyme, β-glucanase and water is 10:3-6:1-3:50-60; The second enzymatic hydrolysis is performed at a temperature of 50-60℃ for 3-5 hours.

[0012] Preferably, the programmed cooling includes: a first cooling, a second reheating, and a third cooling; The first cooling temperature is -4℃ to 0℃, and the time is 30-60 minutes; The second rewarming temperature is 1°C to 4°C, and the time is 15-25 minutes; The third cooling temperature is -15℃ to -10℃, and the time is 1-2 hours.

[0013] Preferably, the temperature of the first vacuum drying is 65-70℃, and the vacuum degree is -0.06 to -0.08 MPa; The temperature of the second vacuum drying is 45-50℃, and the vacuum degree is -0.03 to -0.05MPa.

[0014] The present invention provides a plant rubber composition obtained by the preparation method described in the above technical solution.

[0015] Beneficial effects: This invention provides a method for preparing a plant-based rubber composition, comprising the following steps: mixing potato starch, β-1,3-glucanase, pectin esterase, and water for a first enzymatic hydrolysis to obtain a first hydrolysate; subjecting the first hydrolysate to enzyme inactivation and a first vacuum drying to obtain resistant potato starch; mixing hydroxypropyl starch, resistant potato starch, and wheat starch uniformly to obtain a first mixture; subjecting plant powder to programmed cooling, then mixing it with Aspergillus niger saccharifying enzyme, β-glucanase, and water for a second enzymatic hydrolysis to obtain a second hydrolysate; subjecting the second hydrolysate to enzyme inactivation and a second vacuum drying to obtain resistant cellulose; mixing hydroxypropyl methylcellulose and resistant cellulose uniformly to obtain a second mixture; and stirring the first mixture, pullulan, carrageenan, gellan gum, konjac flour, mannitol, sorbitol, the second mixture, and water uniformly to obtain the plant-based rubber composition.

[0016] Compared with the prior art, the present invention has the following advantages: 1) This invention uses β-1,3-glucanase and pectin esterase to enzymatically modify potato starch, overcoming the disadvantage of excessive viscosity of natural starch. In addition, by compounding it with hydroxypropyl starch and wheat starch, the viscosity of starch is effectively reduced, while also improving gelation properties, rapidly dissolving and forming a gel, so that the flowability of the gel meets the requirements of pelleting equipment and the disintegration performance is stable. 2) In this invention, plant powder is enzymatically modified by Aspergillus niger saccharifying enzyme and β-glucanase, and then mixed with hydroxypropyl methylcellulose. This process is beneficial for the formation of a strong gel network, which improves the binding rate of the capsule, reduces the problem of oil leakage in plant capsules, improves the integrity of the capsules, and enhances the resistance to deformation.

[0017] Therefore, the technical solution provided by the present invention has the advantages of simple operation, high integrity and stable disintegration performance. Detailed Implementation

[0018] Unless otherwise specified, the raw materials, equipment and methods used in this invention are all conventional choices.

[0019] To further illustrate the present invention, the solutions provided by the present invention will be described in detail below with reference to the embodiments, but they should not be construed as limiting the scope of protection of the present invention.

[0020] Example 1 A method for preparing a plant-based rubber composition, comprising the following steps: (1) Preparation of the first mixture Potato starch, β-1,3-glucanase, pectin esterase, and water were mixed evenly in a mass ratio of 10:0.4:0.6:30 and then enzymatically hydrolyzed at 75°C for 8 hours to obtain an enzymatic hydrolysate. The enzymatic hydrolysate was then heated at 85°C for 15 minutes to inactivate the enzyme, resulting in an enzyme-inactivated hydrolysate. The enzyme-inactivated hydrolysate was then vacuum-dried at 65°C and a vacuum degree of -0.08 MPa (until the mass no longer changed) to obtain resistant potato starch. Hydroxypropyl starch, resistant potato starch and wheat starch were mixed evenly in a mass ratio of 1:6:2.5 to obtain the first mixture. (2) Preparation of the second mixture Chicory ( Chicory intybus Clean, dry and crush to obtain chicory powder to be modified (the particle size of the chicory powder to be modified is ≤0.1cm). The chicory powder to be modified was cooled at -4℃ for 60 min, then kept at 1℃ for 15 min, and finally kept at -15℃ for 2 h to obtain the pretreated chicory powder. Pretreated chicory powder, Aspergillus niger saccharifying enzyme, β-glucanase, and water were mixed evenly in a mass ratio of 10:3:1:50 and enzymatically hydrolyzed at 50℃ for 3 hours to obtain an enzymatic hydrolysate. The enzymatic hydrolysate was then heated at 85℃ for 15 minutes to inactivate the enzyme, resulting in an enzyme-inactivated hydrolysate. The enzyme-inactivated hydrolysate was then vacuum-dried at 50℃ and a vacuum degree of -0.05MPa (until the mass no longer changed) to obtain resistant cellulose. Hydroxypropyl methylcellulose and resistant cellulose were mixed evenly at a mass ratio of 1.5:1 to obtain a second mixture. (3) Preparation of plant rubber composition The plant gelatin composition comprises, by weight percentage, the following raw materials: 22% of a first mixture, 0.5% pullulan, 0.5% carrageenan, 0.8% gellan gum, 1% konjac flour, 5% mannitol, 5% sorbitol, 12% of a second mixture, and the balance being water; The first mixture, pullulan, carrageenan, gellan gum, konjac flour, mannitol, sorbitol, the second mixture, and water are mixed evenly to obtain a plant rubber composition.

[0021] Example 2 The only difference from Example 1 is that barley leaf powder is used instead of chicory powder in Example 1 in Example 2; The method for pretreatment of barley leaf powder is as follows: young barley leaves ( Barley L. Clean, dry and crush the barley leaves to obtain barley leaf powder to be modified (the particle size of the barley leaf powder to be modified is ≤0.1cm).

[0022] Comparative Example 1 The only difference from Example 1 is that the process of step (1) in Comparative Example 1 is as follows: (1) Preparation of the first mixture Hydroxypropyl starch, potato starch and wheat starch were mixed evenly in a mass ratio of 1:6:2.5 to obtain the first mixture.

[0023] Comparative Example 2 The only difference from Example 1 is that the process of step (1) in Comparative Example 2 is as follows: (1) Preparation of the first mixture Potato starch, β-1,3-glucanase, pectin esterase, and water were mixed evenly in a mass ratio of 10:0.4:0.6:30 and then enzymatically hydrolyzed at 75°C for 8 hours to obtain an enzymatic hydrolysate. The enzymatic hydrolysate was then heated at 85°C for 15 minutes to inactivate the enzyme, resulting in an enzyme-inactivated hydrolysate. The enzyme-inactivated hydrolysate was then vacuum-dried at 65°C and a vacuum degree of -0.08 MPa (until the mass no longer changed) to obtain resistant potato starch. Hydroxypropyl starch, resistant potato starch and wheat starch were mixed evenly in a mass ratio of 1:1:1 to obtain the first mixture.

[0024] Comparative Example 3 The only difference from Example 1 is that the process of step (2) in Comparative Example 3 is as follows: (2) Preparation of the second mixture Hydroxypropyl methylcellulose and carboxymethyl cellulose were mixed evenly at a mass ratio of 1.5:1 to obtain a second mixture.

[0025] Comparative Example 4 The only difference from Example 1 is that the process of step (2) in Comparative Example 4 is as follows: (2) Preparation of the second mixture Chicory ( Chicory intybus Clean, dry and crush to obtain chicory powder to be modified (the particle size of the chicory powder to be modified is ≤0.1cm). Chicory powder to be modified, Aspergillus niger saccharifying enzyme, and water were mixed evenly at a mass ratio of 10:3:50 and enzymatically hydrolyzed at 50℃ for 3 hours to obtain an enzymatic hydrolysate. The enzymatic hydrolysate was then heated at 85℃ for 15 minutes to inactivate the enzyme, resulting in an enzyme-inactivated hydrolysate. The enzyme-inactivated hydrolysate was then vacuum dried at 50℃ and a vacuum degree of -0.05MPa (until the mass no longer changed) to obtain resistant cellulose. Hydroxypropyl methylcellulose and resistant cellulose were mixed evenly at a mass ratio of 1.5:1 to obtain a second mixture.

[0026] Comparative Example 5 The only difference from Example 1 is that the process of step (3) in Comparative Example 5 is as follows: (3) Preparation of plant rubber composition The plant gelatin composition comprises, by weight percentage, the following raw materials: 32% of a first mixture, 0.5% pullulan, 0.5% carrageenan, 0.8% gellan gum, 1% konjac flour, 5% mannitol, 5% sorbitol, 5% of a second mixture, and the balance being water; The first mixture, pullulan, carrageenan, gellan gum, konjac flour, mannitol, sorbitol, the second mixture, and water are mixed evenly to obtain a plant rubber composition.

[0027] The plant rubber compositions prepared in Examples 1-2 and Comparative Examples 1-5 were used as test objects. Each test object was made into a rubber sheet (thickness of 0.7 mm) by a rubber wheel, and then prepared into soft capsules.

[0028] The rubber sheets in each treatment were placed in an environment of 23℃ and 50% relative humidity for 5 hours to equilibrate. Then, the tensile strength and elongation at break of each sample were measured. The results are shown in Table 1.

[0029] Table 1. Tensile strength and elongation at break of rubber sheets under different treatments

[0030] As can be seen from the data in Table 1, the prepared rubber sheets, whether in the examples or comparative examples, all have good mechanical properties.

[0031] The disintegration time of each soft capsule was tested according to the method in the appendix of the Chinese Pharmacopoeia. The initial disintegration time of each soft capsule was tested in an artificial gastric fluid environment. Then, the soft capsules were placed in an intelligent disintegration instrument and aged at a temperature of 40°C and a relative humidity of 75%. Samples (10 soft capsules each time) were taken out at 30d, 60d, 90d and 120d for disintegration time testing. The specific results are shown in Table 2.

[0032] Table 2. Average disintegration time of soft capsules under different treatments

[0033] As shown in Table 2, compared with the comparative example, the soft capsules prepared in Example 1 or Example 2 had a disintegration time of 10.8 min at 120 days. This indicates that the technical solution of the present invention is beneficial for extending the storage period and has relatively stable disintegration performance.

[0034] Thirty soft capsules each from Examples 1-2, Comparative Example 2, and Comparative Example 5 were prepared and placed in an intelligent disintegration apparatus. The soft capsules were aged at a temperature of 40°C and a relative humidity of 75%. The capsule integrity was tested at 60d, 90d, and 120d. The results are shown in Table 3.

[0035] Table 3. Capsule integrity under different treatments

[0036] As shown in Table 3, compared with the comparative example, the soft capsules prepared in Example 1 or Example 2 exhibited high capsule integrity at 120 days, with only one capsule shell being incomplete or leaking oil; while the capsules prepared in the comparative example showed low integrity. This indicates that the technical solution of the present invention is beneficial for improving the stability of the capsule shell.

[0037] In summary, this invention utilizes β-1,3-glucanase and pectin esterase to enzymatically modify potato starch, overcoming the disadvantage of excessive viscosity in natural starch. Furthermore, by combining it with hydroxypropyl starch and wheat starch, the viscosity is effectively reduced while also improving gelation properties, enabling rapid gelation and ensuring the fluidity of the gel meets the requirements of granulation equipment, while maintaining stable disintegration performance. Enzymatic modification of plant powder using Aspergillus niger saccharifying enzyme and β-glucanase, followed by mixing with hydroxypropyl methylcellulose, promotes a strong gel network, increases the binding rate of the capsule shell, reduces oil leakage from plant capsules, improves capsule integrity, and enhances resistance to deformation.

[0038] Although the above embodiments have provided a detailed description of the present invention, they are only some embodiments of the present invention, and not all embodiments. People can obtain other embodiments based on these embodiments without creative effort, and these embodiments all fall within the protection scope of the present invention.

Claims

1. A method for preparing a plant-based rubber composition, characterized in that, Includes the following steps: Potato starch, β-1,3-glucanase, pectin esterase and water were mixed for the first enzymatic hydrolysis to obtain the first hydrolysate; The first enzymatic hydrolysate was subjected to enzyme inactivation and first vacuum drying to obtain resistant potato starch; Hydroxypropyl starch, resistant potato starch, and wheat starch are mixed evenly to obtain a first mixture; After the plant powder was cooled by a program, it was mixed with Aspergillus niger saccharifying enzyme, β-glucanase and water for a second enzymatic hydrolysis to obtain a second enzymatic hydrolysate. The second enzymatic hydrolysate was subjected to enzyme inactivation and then vacuum drying to obtain resistant cellulose; Hydroxypropyl methylcellulose and resistant cellulose are mixed evenly to obtain a second mixture; The first mixture, pullulan, carrageenan, gellan gum, konjac flour, mannitol, sorbitol, the second mixture, and water are mixed evenly to obtain a plant rubber composition.

2. The preparation method according to claim 1, characterized in that, The plant powder includes: chicory powder or barley leaf powder.

3. The preparation method according to claim 1, characterized in that, The plant-based rubber composition comprises the following raw materials by weight percentage: The first mixture consists of 12%-22% pullulan, 0.5%-1% carrageenan, 0.5%-1% gellan gum, 0.8%-1.2% konjac flour, 1%-1.5% mannitol, 5%-10% sorbitol, the second mixture consists of 6%-12% and the remainder is water.

4. The preparation method according to claim 1 or 3, characterized in that, In the first mixture, the mass ratio of hydroxypropyl starch, resistant potato starch and wheat starch is 1-1.5:6-8:2-2.

5.

5. The preparation method according to claim 1 or 3, characterized in that, The mass ratio of hydroxypropyl methylcellulose to resistant cellulose in the second mixture is 1-1.5:

1.

6. The preparation method according to claim 1, characterized in that, During the first enzymatic hydrolysis, the mass ratio of potato starch, β-1,3-glucanase, pectin esterase, and water was 10:0.2-0.4:0.6-0.8:20-30. The first enzymatic hydrolysis is performed at a temperature of 70-80℃ for 6-8 hours.

7. The preparation method according to claim 1, characterized in that, During the second enzymatic hydrolysis, the mass ratio of plant powder to Aspergillus niger saccharifying enzyme, β-glucanase and water is 10:3-6:1-3:50-60; The second enzymatic hydrolysis is performed at a temperature of 50-60℃ for 3-5 hours.

8. The preparation method according to claim 1, characterized in that, The cooling process includes: a first cooling, a second reheating, and a third cooling. The first cooling temperature is -4℃ to 0℃, and the time is 30-60 minutes; The second rewarming temperature is 1°C to 4°C, and the time is 15-25 minutes; The third cooling temperature is -15℃ to -10℃, and the time is 1-2 hours.

9. The preparation method according to claim 1, characterized in that, The temperature of the first vacuum drying is 65-70℃, and the vacuum degree is -0.06 to -0.08 MPa; The temperature of the second vacuum drying is 45-50℃, and the vacuum degree is -0.03 to -0.05MPa.

10. The plant rubber composition obtained by the preparation method according to any one of claims 1-9.

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