A hydroxypropyl starch-based composition, its method of preparation and use

Abstract

The application discloses a hydroxypropyl starch-based composition, a preparation method and application thereof. The application discloses a preparation method of the composition, which comprises hydroxypropyl starch, polyvinyl alcohol, glycerol, sorbitol, carrageenan, potassium acetate, hydroxypropyl methyl cellulose, dimethicone and water. The composition is used for preparing a hard gelatin capsule shell, and the hard gelatin capsule shell has the advantages of smooth surface, good transparency, high forming rate, low friability, short disintegration time and high stability, and can provide an important reference for replacing traditional gelatin capsules. The preparation method is simple, and the cost is low. The capsule has good apparent properties and forming properties, and has remarkable effects in resisting friability, fast disintegration, storage stability and the like, and has great application prospects in medical preparations, food packaging materials, health product packaging and the like.

Description

A hydroxypropyl starch-based composition, its preparation method and uses Technical Field

[0001] This invention belongs to the field of pharmaceutical packaging materials technology, particularly the field of pharmaceutical capsule packaging materials, and specifically relates to a hydroxypropyl starch-based composition, its preparation method, and its uses. More specifically, this invention relates to a hydroxypropyl starch-based composition formulation, its capsule products, its preparation method, and its applications in pharmaceutical, food, and health product packaging materials. Background Technology

[0002] Capsules are an important packaging material for modern medicine and functional foods. With the continuous improvement of people's health awareness and understanding, the market demand for empty capsules is increasing. Currently, the main component of most pharmaceutical and health food empty capsules is gelatin. Traditionally, the gelatin used in capsule preparation is mainly animal gelatin, which has the advantages of high viscosity and good film-forming properties.

[0003] Traditional gelatin capsules have problems such as high raw material prices, low safety of animal-derived ingredients, easy allergens, unstable quality, and cross-linking with drugs. Therefore, finding alternatives to animal gelatin capsules has become a hot topic in capsule research in recent years.

[0004] Starch is one of the most abundant natural biopolymers, polymerized from glucose units, and generally consists of amylose and amylopectin. In recent years, starch has attracted widespread attention in the capsule industry due to its low cost, wide availability, good film-forming properties, safety, non-toxicity, and renewability. However, natural starch has drawbacks such as poor mechanical properties, easy retrogradation, and poor solubility, leading to problems such as poor formability, high brittleness, difficulty in disintegration, and poor storage stability in starch-based capsules. Compared to gelatin capsules, its quality is significantly inferior, thus greatly limiting the large-scale production and application of starch-based capsules. Therefore, there is an urgent need to develop starch-based capsule products with superior qualities such as resistance to brittleness, easy disintegration, and storage stability. Summary of the Invention

[0005] In view of this, the present invention aims to provide a hydroxypropyl starch-based composition for capsules and a preparation method thereof, which improves the appearance, molding rate, friability, disintegration time, and storage stability of starch-based capsules, thereby comprehensively improving the quality of starch-based capsules and solving the problems of easy friability, difficult disintegration, and poor stability of existing starch-based capsule products, providing an important reference for replacing traditional gelatin capsules.

[0006] To achieve the above objectives, the present invention is implemented through the following technical solution:

[0007] To address the problems of high brittleness, poor disintegration, and poor storage stability of traditional starch-based capsules, the inventors first selected hydroxypropyl pea starch as the raw material, utilizing its high amylose content, low gelatinization temperature, and good resistance to retrogradation to improve the capsule's formation rate and anti-retrogradation performance. Then, polyvinyl alcohol and hydroxypropyl methylcellulose, with their high hydrophilicity and polymer properties, were used as excipients to enhance the capsule's mechanical properties and water solubility. Finally, by adjusting the formulation and optimizing the process, high-quality starch-based capsules with resistance to brittleness, easy disintegration, and storage stability were prepared.

[0008] Specifically, the present invention provides a hydroxypropyl starch-based composition comprising hydroxypropyl starch, polyvinyl alcohol, glycerin, sorbitol, carrageenan, potassium acetate, hydroxypropyl methylcellulose, and dimethicone.

[0009] The hydroxypropyl starch-based composition of the present invention comprises hydroxypropyl starch, polyvinyl alcohol, glycerin, sorbitol, carrageenan, potassium acetate, hydroxypropyl methylcellulose, and dimethicone in a mass ratio of 1:(0.04-0.06):(0.03-0.05):(0.01-0.02):(0.007-0.021):(0.007-0.021):(0.001-0.005):(0.007-0.014).

[0010] Furthermore, the mass ratio of hydroxypropyl starch: polyvinyl alcohol: glycerin: sorbitol: carrageenan: potassium acetate: hydroxypropyl methylcellulose: dimethicone is 1:0.05:(0.03-0.05):(0.01-0.02):(0.007-0.021):(0.007-0.021):(0.001-0.005):(0.007-0.014).

[0011] Furthermore, the mass ratio of hydroxypropyl starch: polyvinyl alcohol: glycerin: sorbitol: carrageenan: potassium acetate: hydroxypropyl methylcellulose: dimethicone is 1:0.05:0.04:(0.01-0.02):(0.007-0.021):(0.007-0.021):(0.001-0.005):(0.007-0.014).

[0012] Furthermore, the mass ratio of hydroxypropyl starch: polyvinyl alcohol: glycerin: sorbitol: carrageenan: potassium acetate: hydroxypropyl methylcellulose: dimethicone is 1:0.05:0.04:0.01:(0.007-0.021):(0.007-0.021):(0.001-0.005):(0.007-0.014).

[0013] Furthermore, the mass ratio of hydroxypropyl starch: polyvinyl alcohol: glycerin: sorbitol: carrageenan: potassium acetate: hydroxypropyl methylcellulose: dimethicone is 1:0.05:004:0.01:0.021:(0.007-0.021):(0.001-0.005):(0.007-0.014).

[0014] Furthermore, the mass ratio of hydroxypropyl starch: polyvinyl alcohol: glycerin: sorbitol: carrageenan: potassium acetate: hydroxypropyl methylcellulose: dimethicone is 1:0.05:0.04:0.01:0.021:0.021:(0.001-0.005):(0.007-0.014).

[0015] Furthermore, the mass ratio of hydroxypropyl starch: polyvinyl alcohol: glycerin: sorbitol: carrageenan: potassium acetate: hydroxypropyl methylcellulose: dimethicone is 1:0.05:0.04:0.01:0.021:0.021:0.003:(0.007-0.014).

[0016] Furthermore, the mass ratio of hydroxypropyl starch: polyvinyl alcohol: glycerin: sorbitol: carrageenan: potassium acetate: hydroxypropyl methylcellulose: dimethicone is 1:0.05:0.04:001:0.021:0.021:0003:0007.

[0017] The hydroxypropyl starch-based composition of the present invention is characterized by further comprising water, wherein the water accounts for 82.9%-84.2% of the total mass of the composition; preferably, the water accounts for 83.5% of the total mass of the composition.

[0018] The present invention also provides a hollow hard capsule prepared from a hydroxypropyl starch-based composition, the preparation method of which is as follows:

[0019] Hydroxypropyl starch is mixed with water to obtain solution A, and carrageenan is mixed with water to obtain solution B. Solutions A and B are heated and stirred at 85-95℃ for 40-80 minutes. Then, the two are mixed, and polyvinyl alcohol, glycerin, sorbitol, potassium acetate, hydroxypropyl methylcellulose, and dimethicone are added. The mixture is heated and stirred at 85-95℃ for 60-90 minutes, and then equilibrated at 75-85℃ for 0-15 minutes. The capsules are dipped into the gelatin using a capsule mold, dried for 4-6 hours, and then demolded to obtain hollow hard capsules.

[0020] In the above preparation method, solutions A and B are heated and stirred at 90°C for 60 min before mixing.

[0021] In the above preparation method, after adding polyvinyl alcohol, glycerol, sorbitol, potassium acetate, hydroxypropyl methylcellulose, and dimethicone, the mixture can be heated and stirred at 95°C for 60 min; equilibrated at 80°C for 5 min; and dried at 40°C for 5 h.

[0022] The hollow hard capsules prepared from the hydroxypropyl starch-based composition of the present invention can also be prepared by the following method:

[0023] Hydroxypropyl starch is mixed with water to obtain solution A, and carrageenan is mixed with water to obtain solution B. Solutions A and B are mixed and heated and stirred at 85-95℃ for 40-80 min. Polyvinyl alcohol, glycerin, sorbitol, potassium acetate, hydroxypropyl methylcellulose, and dimethicone are added. Heating and stirring are continued at 85-95℃ for 60-90 min, and then equilibrated at 75-85℃ for 0-15 min. The capsule is dipped into the glue using a capsule mold, dried for 4-6 h, and demolded to obtain hollow hard capsules.

[0024] The present invention also provides hydroxypropyl starch-based compositions that can be used to prepare capsule materials, including those for human, animal, and pet use.

[0025] The hydroxypropyl starch-based composition described in this invention can be used to prepare capsule materials. These capsule materials include, but are not limited to, pharmaceutical capsule materials, food capsule materials, and health product capsule materials, such as empty hard capsules; they can be used in pharmaceutical packaging materials, health product packaging materials, food packaging materials, etc.

[0026] The starch source of the hydroxypropyl starch described in this invention is pea starch.

[0027] Compared with the prior art, the present invention has the following advantages:

[0028] This invention utilizes the high amylose content, low gelatinization temperature, and anti-retrogradation properties of hydroxypropyl pea starch, combined with the enhancing effects of polyvinyl alcohol and hydroxypropyl methylcellulose on the mechanical properties and water solubility of the starch matrix, to prepare a hydroxypropyl starch composition and capsules. The prepared hollow hard capsules show significant improvements in many aspects, including friability, disintegration time, and storage stability.

[0029] The hollow hard capsules prepared by the composition of this invention have a smooth surface, good transparency, and high molding rate (>95%). They possess advantages such as strong resistance to brittleness (zero brittleness), short disintegration time (<10 min), and good stability (accelerated stability >90 days), meeting the standards for hollow hard capsules in the Chinese Pharmacopoeia (2020 edition) and reaching the quality of commercial gelatin capsules. This invention can provide an important reference for replacing traditional gelatin capsules. The preparation method of this invention is simple and low-cost, and the capsules have excellent appearance and molding properties. They are highly effective in resisting brittleness, rapid disintegration, and storage stability, and have great application prospects in medical preparations, food packaging materials, and health product packaging. Attached Figure Description

[0030] Figure 1 is a flowchart of the preparation process of hydroxypropyl starch-based hollow hard capsules in this invention;

[0031] Figure 2 is a flowchart of the accelerated stability test of hard capsules in this invention. Detailed Implementation

[0032] Unless otherwise defined, the technical terms used in the following embodiments have the same meanings as commonly understood by those skilled in the art. Unless otherwise specified, the experimental reagents used in the following embodiments are conventional biochemical reagents; and the experimental methods described are conventional methods.

[0033] The present invention will be described in detail below with reference to the embodiments.

[0034] Product: Gelatin capsules: Commercially available No. 0 capsules, purchased from Zhejiang Enercon Company.

[0035] Example 1: A formulation and preparation of a hard capsule

[0036] In the hydroxypropyl starch composition, the mass ratio of hydroxypropyl pea starch: polyvinyl alcohol: glycerol: sorbitol: carrageenan: potassium acetate: hydroxypropyl methylcellulose: dimethicone is 1:0.05:0.04:0.01:0.021:0.021:0.005:0.014. Water accounts for 83.5% of the total mass of the composition. Hydroxypropyl starch and water are mixed evenly to prepare solution A, and carrageenan and water are mixed evenly to prepare solution B. Solutions A and B are heated and stirred at 90°C for 40 min. Then, they are mixed, and polyvinyl alcohol, glycerol, sorbitol, potassium acetate, hydroxypropyl methylcellulose, and dimethicone are added. Heating and stirring are continued at 90°C for 40 min, followed by equilibration at 80°C for 5 min. The mixture is then dipped into a capsule mold and dried at 40°C for 6 h to prepare hard capsules.

[0037] Example 2: A formulation and preparation of a hard capsule

[0038] In the hydroxypropyl starch composition, the mass ratio of hydroxypropyl pea starch: polyvinyl alcohol: glycerol: sorbitol: carrageenan: potassium acetate: hydroxypropyl methylcellulose: dimethicone is 1:0.05:0.04:0.01:0.021:0.021:0.003:0.007. Water accounts for 83.5% of the total mass of the composition. Hydroxypropyl starch and water are mixed evenly to prepare solution A, and carrageenan and water are mixed evenly to prepare solution B. Solutions A and B are heated and stirred at 90°C for 40 min. Then, they are mixed, and polyvinyl alcohol, glycerol, sorbitol, potassium acetate, hydroxypropyl methylcellulose, and dimethicone are added. The mixture is heated and stirred at 95°C for 50 min, then equilibrated at 80°C for 5 min. The mixture is then dipped into a capsule mold and dried at 40°C for 6 h to prepare hard capsules.

[0039] Example 3: A formulation and preparation of a hard capsule

[0040] In the hydroxypropyl starch composition, the mass ratio of hydroxypropyl pea starch: polyvinyl alcohol: glycerol: sorbitol: carrageenan: potassium acetate: hydroxypropyl methylcellulose: dimethicone is 1:0.05:0.04:0.01:0.021:0.021:0.003:0.0007. Water accounts for 83.5% of the total mass of the composition. Hydroxypropyl starch and water are mixed evenly to prepare solution A, and carrageenan and water are mixed evenly to prepare solution B. Solutions A and B are heated and stirred at 90°C for 50 min, then mixed together. Polyvinyl alcohol, glycerol, sorbitol, potassium acetate, hydroxypropyl methylcellulose, and dimethicone are added, and the mixture is heated and stirred at 95°C for 60 min. Then, it is equilibrated at 80°C for 5 min. The mixture is then dipped into a capsule mold and dried at 40°C for 6 h to prepare hard capsules.

[0041] Example 4: A formulation and preparation of a hard capsule

[0042] In the hydroxypropyl starch composition, the mass ratio of hydroxypropyl pea starch: polyvinyl alcohol: glycerol: sorbitol: carrageenan: potassium acetate: hydroxypropyl methylcellulose: dimethicone is 1:0.05:0.05:0.01:0.021:0.021:0.003:0.0014. Water accounts for 83.5% of the total mass of the composition. Hydroxypropyl starch and water are mixed evenly to prepare solution A, and carrageenan and water are mixed evenly to prepare solution B. Solutions A and B are heated and stirred at 95°C for 50 min. Then, they are mixed, and polyvinyl alcohol, glycerol, sorbitol, potassium acetate, hydroxypropyl methylcellulose, and dimethicone are added. Heating and stirring are continued at 95°C for 50 min, and then equilibrated at 80°C for 5 min. The mixture is then dipped into a capsule mold and dried at 40°C for 6 h to prepare hard capsules.

[0043] Example 5: A formulation and preparation of a hard capsule

[0044] In the hydroxypropyl starch composition, the mass ratio of hydroxypropyl pea starch: polyvinyl alcohol: glycerol: sorbitol: carrageenan: potassium acetate: hydroxypropyl methylcellulose: dimethicone is 1:0.05:0.05:0.01:0.021:0.021:0.003:0.0014. Water accounts for 83.5% of the total mass of the composition. Hydroxypropyl starch and water are mixed evenly to prepare solution A, and carrageenan and water are mixed evenly to prepare solution B. Solutions A and B are heated and stirred at 95°C for 60 min, then mixed together. Polyvinyl alcohol, glycerol, sorbitol, potassium acetate, hydroxypropyl methylcellulose, and dimethicone are added, and the mixture is heated and stirred at 95°C for another 60 min. The mixture is then equilibrated at 80°C for 5 min, dipped into a capsule mold, and dried at 40°C for 6 h to prepare hard capsules.

[0045] Example 6: A formulation and preparation of a hard capsule

[0046] In the hydroxypropyl starch composition, the mass ratio of hydroxypropyl pea starch: polyvinyl alcohol: glycerol: sorbitol: carrageenan: potassium acetate: hydroxypropyl methylcellulose: dimethicone is 1:0.04:0.05:0.01:0.021:0.021:0.003:0.0014. Water accounts for 83.5% of the total mass of the composition. Hydroxypropyl starch and water are mixed evenly to prepare solution A, and carrageenan and water are mixed evenly to prepare solution B. Solutions A and B are heated and stirred at 95°C for 50 min, then mixed together. Polyvinyl alcohol, glycerol, sorbitol, potassium acetate, hydroxypropyl methylcellulose, and dimethicone are added, and the mixture is heated and stirred at 95°C for another 60 min. The mixture is then equilibrated at 80°C for 5 min. The capsules are dipped into the gel using a capsule mold and dried at 40°C for 6 h to prepare hard capsules.

[0047] Example 7: A formulation and preparation of a hard capsule

[0048] In the hydroxypropyl starch composition, the mass ratio of hydroxypropyl pea starch: polyvinyl alcohol: glycerol: sorbitol: carrageenan: potassium acetate: hydroxypropyl methylcellulose: dimethicone is 1:0.06:0.05:0.01:0.021:0.021:0.003:0.0014. Water accounts for 83.5% of the total mass of the composition. Hydroxypropyl starch and water are mixed evenly to prepare solution A, and carrageenan and water are mixed evenly to prepare solution B. Solutions A and B are heated and stirred at 95°C for 50 min, then mixed together. Polyvinyl alcohol, glycerol, sorbitol, potassium acetate, hydroxypropyl methylcellulose, and dimethicone are added, and the mixture is heated and stirred at 95°C for 60 min. Then, it is equilibrated at 80°C for 5 min. The mixture is then dipped into a capsule mold and dried at 40°C for 6 h to prepare hard capsules.

[0049] Example 8: A formulation and preparation of a hard capsule

[0050] In the hydroxypropyl starch composition, the mass ratio of hydroxypropyl pea starch: polyvinyl alcohol: glycerol: sorbitol: carrageenan: potassium acetate: hydroxypropyl methylcellulose: dimethicone is 1:0.05:0.04:0.01:0.021:0.021:0.003:0.014. Water accounts for 83.5% of the total mass of the composition. Hydroxypropyl starch and water are mixed evenly to prepare solution A, and carrageenan and water are mixed evenly to prepare solution B. Solutions A and B are heated and stirred at 95°C for 60 min. Then, they are mixed, and polyvinyl alcohol, glycerol, sorbitol, potassium acetate, hydroxypropyl methylcellulose, and dimethicone are added. Heating and stirring are continued at 95°C for 60 min, followed by equilibration at 80°C for 5 min. The mixture is then dipped into a capsule mold and dried at 40°C for 6 h to prepare hard capsules.

[0051] Example 9: A formulation and preparation of a hard capsule

[0052] In the hydroxypropyl starch composition, the mass ratio of hydroxypropyl pea starch: polyvinyl alcohol: glycerol: sorbitol: carrageenan: potassium acetate: hydroxypropyl methylcellulose: dimethicone is 1:0.05:0.04:0.01:0.021:0.021:0.003:0.014. Water accounts for 82.9% of the total mass of the composition. Hydroxypropyl starch and water are mixed evenly to prepare solution A, and carrageenan and water are mixed evenly to prepare solution B. Solutions A and B are heated and stirred at 95°C for 60 min. Then, they are mixed, and polyvinyl alcohol, glycerol, sorbitol, potassium acetate, hydroxypropyl methylcellulose, and dimethicone are added. Heating and stirring are continued at 95°C for 60 min, followed by equilibration at 80°C for 10 min. The mixture is then dipped into a capsule mold and dried at 40°C for 6 h to prepare hard capsules.

[0053] Example 10: A formulation and preparation of a hard capsule

[0054] In the hydroxypropyl starch composition, the mass ratio of hydroxypropyl pea starch: polyvinyl alcohol: glycerol: sorbitol: carrageenan: potassium acetate: hydroxypropyl methylcellulose: dimethicone is 1:0.05:0.04:0.01:0.021:0.021:0.003:0.014. Water accounts for 84.2% of the total mass of the composition. Hydroxypropyl starch and water are mixed evenly to prepare solution A, and carrageenan and water are mixed evenly to prepare solution B. Solutions A and B are heated and stirred at 95°C for 60 min. Then, they are mixed, and polyvinyl alcohol, glycerol, sorbitol, potassium acetate, hydroxypropyl methylcellulose, and dimethicone are added. Heating and stirring are continued at 95°C for 60 min, followed by equilibration at 80°C for 15 min. The mixture is then dipped into a capsule mold and dried at 40°C for 6 h to prepare hard capsules.

[0055] Example 11: A formulation and preparation of a hard capsule

[0056] In the hydroxypropyl starch composition, the mass ratio of hydroxypropyl pea starch: polyvinyl alcohol: glycerol: sorbitol: carrageenan: potassium acetate: hydroxypropyl methylcellulose: dimethicone is 1:0.05:0.04:0.01:0.021:0.021:0.003:0.014. Water accounts for 83.5% of the total mass of the composition. Hydroxypropyl starch and water are mixed evenly to prepare solution A, and carrageenan and water are mixed evenly to prepare solution B. Solutions A and B are heated and stirred at 95°C for 60 min. Then, they are mixed, and polyvinyl alcohol, glycerol, sorbitol, potassium acetate, hydroxypropyl methylcellulose, and dimethicone are added. Heating and stirring are continued at 95°C for another 60 min. The mixture is then dipped into a capsule mold and dried at 40°C for 6 h to prepare hard capsules.

[0057] Example 12: A formulation and preparation of a hard capsule

[0058] In the hydroxypropyl starch composition, the mass ratio of hydroxypropyl pea starch: polyvinyl alcohol: glycerol: sorbitol: carrageenan: potassium acetate: hydroxypropyl methylcellulose: dimethicone is 1:0.05:0.04:0.01:0.021:0.021:0.001:0.007. Water accounts for 83.5% of the total mass of the composition. Hydroxypropyl starch and water are mixed evenly to prepare solution A, and carrageenan and water are mixed evenly to prepare solution B. Solutions A and B are heated and stirred at 95°C for 60 min. Then, they are mixed, and polyvinyl alcohol, glycerol, sorbitol, potassium acetate, hydroxypropyl methylcellulose, and dimethicone are added. Heating and stirring are continued at 95°C for 60 min, followed by equilibration at 80°C for 5 min. The mixture is then dipped into a capsule mold and dried at 40°C for 6 h to prepare hard capsules.

[0059] Example 13: A formulation and preparation of a hard capsule

[0060] In the hydroxypropyl starch composition, the mass ratio of hydroxypropyl pea starch: polyvinyl alcohol: glycerol: sorbitol: carrageenan: potassium acetate: hydroxypropyl methylcellulose: dimethicone is 1:0.05:0.04:0.01:0.007:0.021:0.001:0.014. Water accounts for 83.5% of the total mass of the composition. Hydroxypropyl starch and water are mixed evenly to prepare solution A, and carrageenan and water are mixed evenly to prepare solution B. Solutions A and B are heated and stirred at 95°C for 60 min. Then, they are mixed, and polyvinyl alcohol, glycerol, sorbitol, potassium acetate, hydroxypropyl methylcellulose, and dimethicone are added. Heating and stirring are continued at 95°C for 60 min, followed by equilibration at 80°C for 5 min. The mixture is then dipped into a capsule mold and dried at 40°C for 6 h to prepare hard capsules.

[0061] Example 14: A formulation and preparation of a hard capsule

[0062] In the hydroxypropyl starch composition, the mass ratio of hydroxypropyl pea starch: polyvinyl alcohol: glycerol: sorbitol: carrageenan: potassium acetate: hydroxypropyl methylcellulose: dimethicone is 1:0.06:0.05:0.02:0.021:0.021:0.005:0.014. Water accounts for 82.9% of the total mass of the composition. Hydroxypropyl starch and water are mixed evenly to prepare solution A, and carrageenan and water are mixed evenly to prepare solution B. Solutions A and B are heated and stirred at 95°C for 60 min. Then, they are mixed, and polyvinyl alcohol, glycerol, sorbitol, potassium acetate, hydroxypropyl methylcellulose, and dimethicone are added. Heating and stirring are continued at 95°C for 60 min, followed by equilibration at 80°C for 5 min. The mixture is then dipped into a capsule mold and dried at 40°C for 6 h to prepare hard capsules.

[0063] Example 15: A formulation and preparation of a hard capsule

[0064] In the hydroxypropyl starch composition, the mass ratio of hydroxypropyl pea starch: polyvinyl alcohol: glycerol: sorbitol: carrageenan: potassium acetate: hydroxypropyl methylcellulose: dimethicone is 1:0.04:0.03:0.01:0.007:0.007:0.001:0.007. Water accounts for 84.2% of the total mass of the composition. Hydroxypropyl starch and water are mixed evenly to prepare solution A, and carrageenan and water are mixed evenly to prepare solution B. Solutions A and B are heated and stirred at 95°C for 60 min, then mixed together. Polyvinyl alcohol, glycerol, sorbitol, potassium acetate, hydroxypropyl methylcellulose, and dimethicone are added, and the mixture is heated and stirred at 95°C for another 60 min. The mixture is then equilibrated at 80°C for 5 min, dipped into a capsule mold, and dried at 40°C for 6 h to prepare hard capsules.

[0065] Comparative Example 1: Natural Pea Starch Hard Capsules

[0066] The mass ratio of natural pea starch: glycerol: sorbitol: carrageenan: potassium acetate: dimethicone is 1:0.04:0.01:0.021:0.021:0.007. Water accounts for 84.3% of the total mass of the composition. Solution A is prepared by uniformly mixing natural pea starch with water, and solution B is prepared by uniformly mixing carrageenan with water. Solutions A and B are heated and stirred at 90°C for 30 min, then combined. Glycerol, potassium acetate, and dimethicone are added, and the mixture is heated and stirred at 90°C for 60 min. The mixture is then equilibrated at 80°C for 5 min. The capsules are then dipped into the gelatin using a capsule mold and dried at 40°C for 6 h to prepare hard capsules.

[0067] Comparative Example 2: Hydroxypropyl Pea Starch Hard Capsules with Different Compositions

[0068] The mass ratio of hydroxypropyl pea starch: glycerol: carrageenan: potassium acetate: dimethicone is 1:0.04:0.021:0.021:0007. Water accounts for 84.4% of the total mass of the composition. Hydroxypropyl starch and water are mixed evenly to prepare solution A, and carrageenan and water are mixed evenly to prepare solution B. Solutions A and B are heated and stirred at 90°C for 30 min. Then, they are mixed, and glycerol, potassium acetate, and dimethicone are added. The mixture is heated and stirred at 90°C for another 60 min, then equilibrated at 80°C for 5 min. The capsules are then dipped into the gelatin using a capsule mold and dried at 40°C for 6 h to prepare hard capsules.

[0069] Comparative Example 3: Hydroxypropyl Pea Starch Hard Capsules with Different Compositions

[0070] The mass ratio of hydroxypropyl pea starch:sorbitol:carrageenan:potassium acetate:dimethyl silicone oil is 1:0.04:0.021:0.021:0.007. Water accounts for 84.4% of the total mass of the composition. Hydroxypropyl starch is mixed with water evenly to prepare solution A, and carrageenan is mixed with water evenly to prepare solution B. Solution A and B are heated and stirred at 90 °C for 30 min, then the two are mixed, and sorbitol, potassium acetate, and dimethyl silicone oil are added, and heating and stirring are continued at 90 °C for 60 min, then balanced at 80 °C for 5 min, and a capsule mold is used to dip the glue, and dried at 40 °C for 6 h to prepare hard capsules.

[0071] Comparative Example 4 Hydroxypropyl Pea Starch Hard Capsules with Different Compositions

[0072] The mass ratio of hydroxypropyl pea starch:glycerol:sorbitol:carrageenan:potassium acetate:dimethyl silicone oil is 1:0.04:0.01:0.021:0.021:0.007. Water accounts for 84.3% of the total mass of the composition. Hydroxypropyl starch is mixed with water evenly to prepare solution A, and carrageenan is mixed with water evenly to prepare solution B. Solution A and B are heated and stirred at 90 °C for 30 mmin, then the two are mixed, and glycerol, potassium acetate, and dimethyl silicone oil are added, and heating and stirring are continued at 90 °C for 60 min, then balanced at 80 °C for 5 min, and a capsule mold is used to dip the glue, and dried at 40 °C for 6 h to prepare hard capsules.

[0073] Comparative Example 5 Hydroxypropyl Pea Starch Hard Capsules with Different Compositions

[0074] The mass ratio of hydroxypropyl pea starch:glycerol:konjac gum:potassium acetate:dimethyl silicone oil is 1:0.04:0.021:0.021:0.007. Water accounts for 84.4% of the total mass of the composition. Hydroxypropyl starch is mixed with water evenly to prepare solution A, and konjac gum is mixed with water evenly to prepare solution B. Solution A and B are heated and stirred at 90 °C for 30 min, then the two are mixed, and glycerol, potassium acetate, and dimethyl silicone oil are added, and heating and stirring are continued at 90 °C for 60 min, then balanced at 80 °C for 5 mmin, and a capsule mold is used to dip the glue, and dried at 40 °C for 6 h to prepare hard capsules.

[0075] Example 16 Apparent Properties and Molding Rate

[0076] Observation of apparent properties and calculation of molding rate: The finished capsules are cylindrical, and the capsule body should be smooth, uniform in color, and without deformation. Meeting the above requirements is qualified.

[0077] The capsule molding rate = the number of capsules with qualified apparent properties (pieces) / the total number of capsules (pieces) × 100%.

[0078] The results are shown in Figure 1 and Table 1. The results show that the hydroxypropyl starch-based capsules prepared in Examples 1-8 have smooth surfaces, uniform color, and no deformation. Compared with Comparative Examples 1-5, the capsule formation rate in Examples 1-8 is higher (>95%), indicating that the prepared capsules are easy to form and have good appearance.

[0079] Table 1 Performance of Hydroxypropyl Starch-Based Capsules

[0080]

[0081]

[0082] Example 17 Thickness

[0083] The single wall thickness of the capsule was determined using a thickness gauge with an accuracy of 0.001 mm. The results are shown in Table 1.

[0084] The results showed that the hydroxypropyl starch-based capsules prepared in Examples 1-8 had thinner walls compared to Comparative Examples 1-5.

[0085] The hydroxypropyl starch-based capsules prepared in Examples 3 and 8 have a wall thickness similar to that of commercial gelatin capsules.

[0086] Example 18 Tightness

[0087] The tightness of the prepared capsules was determined using the testing methods in the 2020 edition of the Chinese Pharmacopoeia. The results are shown in Table 1.

[0088] The results showed that, compared with Comparative Examples 1-5, the hydroxypropyl starch-based empty capsules prepared in Examples 1-8 did not exhibit powder leakage, meeting the requirements of the Chinese Pharmacopoeia (2020), indicating that they possessed good elasticity.

[0089] Example 19 Friability

[0090] The friability of the prepared capsules was determined using the detection methods in the 2020 edition of the Chinese Pharmacopoeia. The results are shown in Table 1.

[0091] The results showed that, compared with Comparative Examples 1-5, the hydroxypropyl starch-based empty capsules prepared in Examples 1-8 did not exhibit brittleness and met the requirements of the Chinese Pharmacopoeia (2020), indicating that they possess excellent anti-brittleness ability.

[0092] Example 20 Disintegration Time Limit

[0093] The disintegration time of the prepared capsules was determined using the detection methods in the 2020 edition of the Chinese Pharmacopoeia. The results are shown in Table 1.

[0094] The results showed that, compared with Comparative Examples 1-5, the hydroxypropyl starch-based empty capsules prepared in Examples 1-8 had a disintegration time of <20 min, which meets the requirements of the Chinese Pharmacopoeia (2020). The disintegration time of the empty hard capsules prepared in Example 8 was similar to that of commercial gelatin capsules (<10 min), indicating that it has rapid disintegration capability.

[0095] Example 21 Loss on drying

[0096] The loss on drying of the prepared capsules was determined using the detection methods in the 2020 edition of the Chinese Pharmacopoeia. The results are shown in Table 1.

[0097] The results showed that the drying loss of the hydroxypropyl starch-based empty capsules prepared in Examples 1-8 was less than 15%, which met the requirements of the Chinese Pharmacopoeia (2020).

[0098] Example 22 Accelerated Stability Test

[0099] Referring to the testing method in the 2020 edition of the Chinese Pharmacopoeia, as shown in Figure 2, the capsules were placed in 8-micron polyethylene packaging bags and sealed using a sealing machine. The samples were then placed in corrugated cardboard boxes and sealed with tape. Finally, they were placed in a temperature and humidity test chamber (purchased from Shanghai Yiheng Instrument Co., Ltd.) with pre-set conditions of 30℃ and 65% RH. The accelerated testing period was 90 days, with the capsule fragility and disintegration time measured every 30 days, for a total of 4 measurements.

[0100] The results showed that during the test period (90 days), the brittleness and disintegration time of the hydroxypropyl starch-based hollow capsules prepared in Examples 7 and 8 did not change significantly, indicating that the hydroxypropyl starch-based hollow capsules were stable under accelerated storage conditions and had good storage stability.

[0101]

[0102] In summary, we utilized the high amylose content, low gelatinization temperature, and resistance to retrogradation of hydroxypropyl pea starch, combined with the enhancing effects of polyvinyl alcohol and hydroxypropyl methylcellulose on the mechanical properties and water solubility of the starch matrix, to prepare a hydroxypropyl starch composition, which was then used to prepare starch-based hard capsules. The prepared hollow hard capsules showed significant improvements in friability, disintegration time, and storage stability. The hollow hard capsules prepared using the composition of this invention have a smooth surface, good transparency, and high molding rate (>95%). They possess advantages such as strong resistance to friability (no friability), short disintegration time (<10 min), and good storage stability (≥90 days under accelerated conditions), meeting the standards for hollow hard capsules in the Chinese Pharmacopoeia (2020 edition) and reaching the quality of commercial gelatin capsules. This provides an important reference for replacing traditional gelatin capsules. The preparation method of this invention is simple and low in cost. The prepared hydroxypropyl starch-based hollow hard capsules have good appearance and formability, and are highly effective in resisting brittleness, rapid disintegration, and stable storage. Therefore, they have great application prospects in medical preparations, food packaging materials, and health product packaging.

[0103] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A hydroxypropyl starch-based composition comprising: hydroxypropyl starch, polyvinyl alcohol, glycerin, sorbitol, carrageenan, potassium acetate, hydroxypropyl methylcellulose, and dimethicone, characterized in that: The mass ratio of hydroxypropyl starch:polyvinyl alcohol:glycerol:sorbitol:carrageenan:potassium acetate:hydroxypropyl methylcellulose:dimethicone is 1:(0.04-0.06):(0.03-0.05):(0.01-0.02):(0.007-0.021):(0.007-0.021):(0.001-0.005):(0.007-0.014); wherein, the hydroxypropyl starch is derived from hydroxypropyl pea starch.

2. The hydroxypropyl starch-based composition according to claim 1, characterized in that... The mass ratio of hydroxypropyl starch:polyvinyl alcohol:glycerin:sorbitol:carrageenan:potassium acetate:hydroxypropyl methylcellulose:dimethicone is 1:0.05:(0.03-0.05):(0.01-0.02):(0.007-0.021):(0.007-0.021):(0.001-0.005):(0.007-0.014).

3. The hydroxypropyl starch-based composition according to claim 2, characterized in that... The mass ratio of hydroxypropyl starch:polyvinyl alcohol:glycerin:sorbitol:carrageenan:potassium acetate:hydroxypropyl methylcellulose:dimethicone is 1:0.05:0.04:(0.01-0.02):(0.007-0.021):(0.007-0.021):(0.001-0.005):(0.007-0.014).

4. The hydroxypropyl starch-based composition according to claim 3, characterized in that... The mass ratio of hydroxypropyl starch:polyvinyl alcohol:glycerin:sorbitol:carrageenan:potassium acetate:hydroxypropyl methylcellulose:dimethicone is 1:0.05:0.04:0.01:(0.007-0.021):(0.007-0.021):(0.001-0.005):(0.007-0.014).

5. The hydroxypropyl starch-based composition according to claim 4, characterized in that... The mass ratio of hydroxypropyl starch:polyvinyl alcohol:glycerin:sorbitol:carrageenan:potassium acetate:hydroxypropyl methylcellulose:dimethicone is 1:0.05:0.04:0.01:0.021:(0.007-0.021):(0.001-0.005):(0.007-0.014).

6. The hydroxypropyl starch-based composition according to claim 5, characterized in that... The mass ratio of hydroxypropyl starch:polyvinyl alcohol:glycerin:sorbitol:carrageenan:potassium acetate:hydroxypropyl methylcellulose:dimethicone is 1:0.05:0.04:0.01:0.021:0.021:(0.001-0.005):(0.007-0.014).

7. The hydroxypropyl starch-based composition according to claim 6, characterized in that... The mass ratio of hydroxypropyl starch: polyvinyl alcohol: glycerol: sorbitol: carrageenan: potassium acetate: hydroxypropyl methylcellulose: dimethicone is 1:0.05:0.04:0.01:0.021:0.021:0.003:(0.007-0.014).

8. The hydroxypropyl starch-based composition according to claim 7, characterized in that... The mass ratio of hydroxypropyl starch: polyvinyl alcohol: glycerol: sorbitol: carrageenan: potassium acetate: hydroxypropyl methylcellulose: dimethicone is 1:0.05:0.04:0.01:0.021:0.021:0.003:0.

007.

9. The hydroxypropyl starch-based composition according to claim 1, characterized in that... It also contains water, which accounts for 82.9% to 84.2% of the total mass of the composition.

10. The hydroxypropyl starch-based composition of claim 9, characterized in that... Water constitutes 83.5% of the total mass of the composition.

11. A hollow hard capsule prepared from the hydroxypropyl starch-based composition of claim 1.

12. A method for preparing the capsule of claim 11: hydroxypropyl starch is mixed with water to obtain solution A, and carrageenan is mixed with water to obtain solution B. Solutions A and B are heated and stirred at 85-95 °C for 40-80 min. Then, the two are mixed, and polyvinyl alcohol, glycerin, sorbitol, potassium acetate, hydroxypropyl methylcellulose, and dimethicone are added. The mixture is heated and stirred at 85-95 °C for 60-90 min, and then equilibrated at 75-85 °C for 0-15 min. The capsule is dipped in the gelatin using a capsule mold, dried for 4-6 h, and then demolded to obtain a hollow hard capsule.

13. The method for preparing the capsule according to claim 12, characterized in that, Before mixing solutions A and B, heat and stir at 90 °C for 60 min.

14. The method for preparing the capsule according to claim 12, characterized in that, After adding polyvinyl alcohol, glycerin, sorbitol, potassium acetate, hydroxypropyl methylcellulose, and dimethicone, heat and stir at 95 °C for 60 min.

15. The method for preparing the capsule according to claim 12, characterized in that, Equilibrate at 80 ℃ for 5 min.

16. The method for preparing the capsule according to claim 12, characterized in that, Dry at 40℃ for 5 hours.

17. A method for preparing the capsule of claim 11: Hydroxypropyl starch is mixed with water to obtain solution A, carrageenan is mixed with water to obtain solution B, solutions A and B are mixed, heated and stirred at 85-95 °C for 40-80 min, polyvinyl alcohol, glycerin, sorbitol, potassium acetate, hydroxypropyl methylcellulose, and dimethicone are added, and the mixture is heated and stirred at 85-95 °C for 60-90 min. Then, the mixture is equilibrated at 75-85 °C for 0-15 min, dipped in the gelatin using a capsule mold, dried for 4-6 h, and demolded to obtain hollow hard capsules.

18. The use of the hydroxypropyl starch-based composition of claim 1 in the preparation of hollow hard capsules.

19. The application of claim 18, wherein the hard capsule material is suitable for human use.

20. The application of claim 18, wherein the hard capsule material is used in animals.

21. The application of claim 20, wherein the hard capsule material can be used for pets.

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