Hydroxypropyl starch-based composition as well as preparation method and application thereof

Abstract

The invention discloses a hydroxypropyl starch-based composition as well as a preparation method and application thereof. The composition prepared by the invention is prepared from hydroxypropyl starch, polyvinyl alcohol, glycerol, sorbitol, carrageenan, potassium acetate, hydroxypropyl methyl cellulose, dimeticone and water. The hollow hard capsule shell prepared from the composition has the advantages of smooth surface, good transparency, high molding rate, low friability, short disintegration time and high stability, and can provide important reference for replacing traditional gelatin capsules. The preparation method is simple, the cost is low, and the capsule is good in apparent character, good in formability, remarkable in effect in the aspects of friability resistance, rapid disintegration, stable storage and the like, and has huge application prospects in the aspects of medical preparations, food packaging materials, health care product packaging and the like.

Description

Technical Field

[0001] The present invention belongs to the technical field of pharmaceutical packaging materials, in particular to the field of pharmaceutical capsule packaging materials, and specifically relates to a hydroxypropyl starch-based composition, a preparation method and use thereof. More specifically, the present invention relates to a hydroxypropyl starch-based composition formula, a capsule product thereof, a preparation method thereof and its application in the packaging of medicines, foods, and health products. Background Art

[0002] Capsules are an important packaging for modern medicines and functional foods. With the continuous improvement of people's health awareness and cognitive level, the market demand for hollow capsules is getting higher and higher. At present, the main ingredient of most hollow capsules used in medicines and health foods is gelatin. The gelatin used in traditional 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 allergy, unstable quality, and cross-linking with drugs. Therefore, finding alternatives to animal gelatin capsules has been a hot topic in the capsule field in recent years.

[0004] Starch is one of the most abundant natural biopolymers, which is polymerized by glucose units and generally consists of amylose and amylopectin. In recent years, starch has attracted widespread attention in the field of capsules due to its low cost, wide source, good film-forming property, safety, non-toxicity and renewability. However, natural starch has disadvantages such as poor mechanical properties, easy regeneration and difficulty in dissolving, which leads to problems such as poor formability, high brittleness, difficulty in disintegration and poor storage stability of starch-based capsules. There is still a big gap compared with the quality of gelatin capsules, which greatly limits the large-scale production and application of starch-based capsules. Therefore, it is urgent to develop starch-based capsule products with excellent qualities such as anti-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, by improving the appearance, forming rate, friability, disintegration time, storage stability and other properties of starch-based capsules, thereby comprehensively improving the quality of starch-based capsules, so as to solve the problems of easy brittleness, difficult disintegration and poor stability of existing starch-based capsule products, and provide an important reference for replacing traditional gelatin capsules.

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

[0007] In response to the problems of traditional starch-based capsules such as high brittleness, difficulty in disintegration, and poor storage stability, the inventors first selected hydroxypropyl pea starch as the raw material, and used its high amylose content, low gelatinization temperature, and good anti-retrogradation properties to improve the capsule molding rate and anti-retrogradation performance; then, polyvinyl alcohol and hydroxypropyl methyl fiber with high hydrophilicity and high molecular weight polymer properties were used as excipients to improve the mechanical properties and water solubility of the capsules; finally, by adjusting the formula and optimizing the process, high-quality starch-based capsules with anti-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 has a mass ratio of hydroxypropyl starch: polyvinyl alcohol: glycerol: sorbitol: carrageenan: potassium acetate: hydroxypropyl methylcellulose: dimethicone of 1: (0.04-0.06): (0.03-0.05): (0.01-0.02): (0.007-0021): (0.007-0.021): (0.001-0.005): (0.007-0.014).

[0010] Furthermore, the mass ratio of hydroxypropyl starch: polyvinyl alcohol: glycerol: 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: glycerol: 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: glycerol: 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: glycerol: 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: glycerol: 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: 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).

[0016] Furthermore, the mass ratio of hydroxypropyl starch: polyvinyl alcohol: glycerol: 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 in that it also contains 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, and the preparation method thereof is as follows:

[0019] Mix hydroxypropyl starch and water evenly to obtain solution A, mix carrageenan and water evenly to obtain solution B, heat solutions A and B at 85-95° C. with stirring for 40-80 min, then mix the two, add polyvinyl alcohol, glycerol, sorbitol, potassium acetate, hydroxypropyl methylcellulose, and dimethicone, continue heating and stirring at 85-95° C. for 60-90 min, then balance at 75-85° C. for 0-15 min, dip a capsule mold in the glue, dry for 4-6 h, and demold to obtain a hollow hard capsule.

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

[0021] In the above preparation method, after adding polyvinyl alcohol, glycerol, sorbitol, potassium acetate, hydroxypropyl methylcellulose and dimethicone, heating and stirring can be performed at 95° C. for 60 minutes; balancing can be performed at 80° C. for 5 minutes; and drying can be performed at 40° C. for 5 hours.

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

[0023] Mix hydroxypropyl starch and water evenly to obtain solution A, mix carrageenan and water evenly to obtain solution B, mix solutions A and B, heat and stir at 85-95° C. for 40-80 min, add polyvinyl alcohol, glycerol, sorbitol, potassium acetate, hydroxypropyl methylcellulose and dimethicone, continue heating and stirring at 85-95° C. for 60-90 min, then balance at 75-85° C. for 0-15 min, dip a capsule mold in the glue, dry for 4-6 h, and demold to obtain a hollow hard capsule.

[0024] The present invention also provides a hydroxypropyl starch-based composition, which can be used to prepare capsule materials, including for humans, animals, including pets.

[0025] The hydroxypropyl starch-based composition of the present invention can be used to prepare capsule materials, including but not limited to: pharmaceutical capsule materials, food capsule materials, health care capsule materials, etc., such as hollow hard capsules; and can be used for pharmaceutical packaging materials, health care product packaging materials, food packaging materials, etc.

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

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

[0028] The present invention utilizes the high amylose content, low gelatinization temperature and anti-retrogradation characteristics of hydroxypropyl pea starch, combined with the enhancement effect of polyvinyl alcohol and hydroxypropyl methylcellulose on the mechanical properties and water solubility of the starch matrix, to prepare a hydroxypropyl starch composition and capsule. The prepared hollow hard capsule has great improvements in friability, disintegration time, storage stability and other aspects.

[0029] The hollow hard capsule prepared by the composition prepared by the present invention has a smooth surface, good transparency, high forming rate (>95%), strong resistance to brittleness (zero brittleness), short disintegration time (<10mmin), and good stability (accelerated stability>90d), which meets the standards of hollow hard capsules in the "Chinese Pharmacopoeia" (2020 edition) and reaches the quality of commercial gelatin capsules. It can provide an important reference for replacing traditional gelatin capsules. The preparation method of the present invention is simple and low in cost. The capsule has good appearance and formability, and has significant effects in resisting brittleness, rapid disintegration, and storage stability. It has great application prospects in medical preparations, food packaging materials, and health care product packaging. BRIEF DESCRIPTION OF THE DRAWINGS

[0030] Figure 1 The figure is a flow chart of the preparation of hydroxypropyl starch-based hollow hard capsules in the present invention;

[0031] Figure 2 The figure is a flow chart of the accelerated stability test of hard capsules in the present invention. DETAILED DESCRIPTION

[0032] Unless otherwise defined, the technical terms used in the following examples have the same meanings as those generally understood by those skilled in the art to which the present invention belongs. The test reagents used in the following examples, unless otherwise specified, are all conventional biochemical reagents; the experimental methods, unless otherwise specified, are all conventional methods.

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

[0034] Commercial gelatin capsules: Commercially available No. 0 capsules, purchased from Zhejiang Enerkang Company.

[0035] Example 1 Prescription 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, carrageenan and water are mixed evenly to prepare solution B, solutions A and B are heated and stirred at 90°C for 40 minutes, then the two are mixed, polyvinyl alcohol, glycerol, sorbitol, potassium acetate, hydroxypropyl methylcellulose, and dimethicone are added, and heating and stirring at 90°C for 40 minutes are continued, and then balanced at 80°C for 5 minutes, and the capsule mold is dipped in glue, and dried at 40°C for 6 hours to prepare hard capsules.

[0037] Example 2 Prescription 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, carrageenan and water are mixed evenly to prepare solution B, solutions A and B are heated and stirred at 90°C for 40 minutes, then the two are mixed, polyvinyl alcohol, glycerol, sorbitol, potassium acetate, hydroxypropyl methylcellulose, and dimethicone are added, and heating and stirring at 95°C are continued for 50 minutes, and then balanced at 80°C for 5 minutes, and the capsule mold is dipped in glue, and dried at 40°C for 6 hours to prepare hard capsules.

[0039] Example 3 Prescription 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, carrageenan and water are mixed evenly to prepare solution B, solutions A and B are heated and stirred at 90°C for 50 minutes, then the two are mixed, polyvinyl alcohol, glycerol, sorbitol, potassium acetate, hydroxypropyl methylcellulose, and dimethicone are added, and heating and stirring at 95°C for 60 minutes, and then balanced at 80°C for 5 minutes, and the capsule mold is dipped in glue, and dried at 40°C for 6 hours to prepare hard capsules.

[0041] Example 4 Prescription 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, carrageenan and water are mixed evenly to prepare solution B, solutions A and B are heated and stirred at 95°C for 50min, then the two are mixed, polyvinyl alcohol, glycerol, sorbitol, potassium acetate, hydroxypropyl methylcellulose, and dimethicone are added, and heating and stirring at 95°C for 50min are continued, and then balanced at 80°C for 5min, a capsule mold is dipped in glue, and dried at 40°C for 6h to prepare a hard capsule.

[0043] Example 5 Prescription 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, carrageenan and water are mixed evenly to prepare solution B, solutions A and B are heated and stirred at 95°C for 60min, then the two are mixed, polyvinyl alcohol, glycerol, sorbitol, potassium acetate, hydroxypropyl methylcellulose, and dimethicone are added, and heating and stirring at 95°C for 60min are continued, and then balanced at 80°C for 5min, a capsule mold is dipped in glue, and dried at 40°C for 6h to prepare a hard capsule.

[0045] Example 6 Prescription 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, carrageenan and water are mixed evenly to prepare solution B, solutions A and B are heated and stirred at 95°C for 50min, then the two are mixed, polyvinyl alcohol, glycerol, sorbitol, potassium acetate, hydroxypropyl methylcellulose, dimethicone are added, heating and stirring at 95°C for 60min, and then balanced at 80°C for 5min, a capsule mold is dipped in glue, and dried at 40°C for 6h to prepare a hard capsule.

[0047] Example 7 Prescription 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, carrageenan and water are mixed evenly to prepare solution B, solutions A and B are heated and stirred at 95°C for 50min, then the two are mixed, polyvinyl alcohol, glycerol, sorbitol, potassium acetate, hydroxypropyl methylcellulose, and dimethicone are added, and heating and stirring at 95°C for 60min are continued, and then balanced at 80°C for 5min, a capsule mold is dipped in glue, and dried at 40°C for 6h to prepare a hard capsule.

[0049] Example 8 Prescription 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, carrageenan and water are mixed evenly to prepare solution B, solutions A and B are heated and stirred at 95°C for 60 minutes, then the two are mixed, polyvinyl alcohol, glycerol, sorbitol, potassium acetate, hydroxypropyl methylcellulose, and dimethicone are added, and heating and stirring at 95°C for 60 minutes are continued, and then balanced at 80°C for 5 minutes, and the capsule mold is dipped in glue, and dried at 40°C for 6 hours to prepare hard capsules.

[0051] Example 9 Prescription 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, carrageenan and water are mixed evenly to prepare solution B, solutions A and B are heated and stirred at 95°C for 60 minutes, then the two are mixed, polyvinyl alcohol, glycerol, sorbitol, potassium acetate, hydroxypropyl methylcellulose, and dimethicone are added, and heating and stirring at 95°C for 60 minutes are continued, and then balanced at 80°C for 10 minutes, and the capsule mold is dipped in glue, and dried at 40°C for 6 hours to prepare hard capsules.

[0053] Example 10 Prescription 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, carrageenan and water are mixed evenly to prepare solution B, solutions A and B are heated and stirred at 95°C for 60 minutes, then the two are mixed, polyvinyl alcohol, glycerol, sorbitol, potassium acetate, hydroxypropyl methylcellulose, and dimethicone are added, and heating and stirring at 95°C for 60 minutes are continued, and then balanced at 80°C for 15 minutes, and the capsule mold is dipped in glue, and dried at 40°C for 6 hours to prepare hard capsules.

[0055] Example 11 Prescription 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, carrageenan and water are mixed evenly to prepare solution B, solutions A and B are heated and stirred at 95°C for 60 minutes, then the two are mixed, polyvinyl alcohol, glycerol, sorbitol, potassium acetate, hydroxypropyl methylcellulose, and dimethicone are added, and heating and stirring at 95°C for 60 minutes are continued. The capsule mold is dipped in glue and dried at 40°C for 6 hours to prepare hard capsules.

[0057] Example 12 Prescription 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, carrageenan and water are mixed evenly to prepare solution B, solutions A and B are heated and stirred at 95°C for 60 minutes, then the two are mixed, polyvinyl alcohol, glycerol, sorbitol, potassium acetate, hydroxypropyl methylcellulose, and dimethicone are added, and heating and stirring at 95°C for 60 minutes are continued, and then balanced at 80°C for 5 minutes, and the capsule mold is dipped in glue, and dried at 40°C for 6 hours to prepare hard capsules.

[0059] Example 13 Prescription 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, carrageenan and water are mixed evenly to prepare solution B, solutions A and B are heated and stirred at 95°C for 60 minutes, then the two are mixed, polyvinyl alcohol, glycerol, sorbitol, potassium acetate, hydroxypropyl methylcellulose, and dimethicone are added, and heating and stirring at 95°C for 60 minutes are continued, and then balanced at 80°C for 5 minutes, and the capsule mold is dipped in glue, and dried at 40°C for 6 hours to prepare hard capsules.

[0061] Example 14 Prescription 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, carrageenan and water are mixed evenly to prepare solution B, solutions A and B are heated and stirred at 95°C for 60min, then the two are mixed, polyvinyl alcohol, glycerol, sorbitol, potassium acetate, hydroxypropyl methylcellulose, and dimethicone are added, and heating and stirring at 95°C for 60min are continued, and then balanced at 80°C for 5min, a capsule mold is dipped in glue, and dried at 40°C for 6h to prepare a hard capsule.

[0063] Example 15 Prescription 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 minutes, then the two are mixed, polyvinyl alcohol, glycerol, sorbitol, potassium acetate, hydroxypropyl methylcellulose and dimethicone are added, and heating and stirring at 95°C for 60 minutes are continued, and then balanced at 80°C for 5 minutes, and the capsule mold is dipped in glue, and dried at 40°C for 6 hours to prepare hard capsules.

[0065] Comparative Example 1 Natural pea starch hard capsule

[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. The natural pea starch and water are mixed evenly to prepare solution A, and the carrageenan and water are mixed evenly to prepare solution B. Solutions A and B are heated and stirred at 90°C for 30min, and then the two are mixed, glycerol, potassium acetate, and dimethicone are added, and heating and stirring at 90°C are continued for 60min, and then balanced at 80°C for 5min, and the capsule mold is dipped in glue, and dried at 40°C for 6h 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, carrageenan and water are mixed evenly to prepare solution B, solutions A and B are heated and stirred at 90°C for 30 minutes, then the two are mixed, glycerol, potassium acetate, and dimethicone are added, and heating and stirring at 90°C are continued for 60 minutes, and then balanced at 80°C for 5 minutes, and the capsule mold is dipped in glue, and dried at 40°C for 6 hours 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: dimethicone is 1: 0.04: 0.021: 0.021: 0.007. 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 minutes, then the two are mixed, sorbitol, potassium acetate, and dimethicone are added, and heating and stirring at 90°C are continued for 60 minutes, and then balanced at 80°C for 5 minutes, and the capsule mold is dipped in glue, and dried at 40°C for 6 hours 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: 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. 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 30min, then the two are mixed, glycerol, potassium acetate and dimethicone are added, and heating and stirring at 90°C are continued for 60min, and then balanced at 80°C for 5min, and a capsule mold is dipped in the glue, and dried at 40°C for 6h to prepare a hard capsule.

[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: dimethicone is 1: 0.04: 0.021: 0.021: 0.007. Water accounts for 84.4% of the total mass of the composition. Hydroxypropyl starch and water are mixed evenly to prepare solution A, and konjac gum and water are mixed evenly to prepare solution B. Solutions A and B are heated and stirred at 90°C for 30 minutes, then the two are mixed, glycerol, potassium acetate, and dimethicone are added, and heating and stirring at 90°C are continued for 60 minutes, and then balanced at 80°C for 5 minutes, and a capsule mold is used to dip the glue, and it is dried at 40°C for 6 hours to prepare a hard capsule.

[0075] Example 16 Appearance and Forming Rate

[0076] Observation of appearance and calculation of forming rate: The finished capsule is cylindrical, with smooth body, uniform color and no deformation. It is qualified if it meets the above requirements.

[0077] Capsule forming rate = number of capsules with qualified appearance properties (pieces) / total number of capsules (pieces) × 100%.

[0078] The results are as follows Figure 1 As shown in Table 1. The results show that the hydroxypropyl starch-based capsules prepared in Examples 1-8 are smooth, uniform in color, and free of deformation, and compared with Comparative Examples 1-5, the capsule forming rate in Examples 1-8 is higher (>95%), indicating that the prepared capsules are easy to form and have good appearance properties.

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

[0080]

[0081]

[0082] Example 17 Thickness

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

[0084] The results show that the hydroxypropyl starch-based capsule walls prepared in Examples 1-8 are thinner than those in Comparative Examples 1-5.

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

[0086] Example 18 tightness

[0087] The tightness of the prepared capsules was measured using the test method in the 2020 edition of the Chinese Pharmacopoeia. The results are shown in Table 1.

[0088] The results show that compared with Comparative Examples 1-5, the hydroxypropyl starch-based hollow capsules prepared in Examples 1-8 have no powder leakage phenomenon, which meets the requirements of the "Chinese Pharmacopoeia" (2020), indicating that they have good tightness.

[0089] Example 19 Friability

[0090] The friability of the prepared capsules was measured using the test method in the 2020 edition of the Chinese Pharmacopoeia. The results are shown in Table 1.

[0091] The results show that compared with Comparative Examples 1-5, the hydroxypropyl starch-based hollow capsules prepared in Examples 1-8 have no brittleness phenomenon, which meets the requirements of the "Chinese Pharmacopoeia" (2020), indicating that they have excellent anti-brittleness ability.

[0092] Example 20 Disintegration Time

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

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

[0095] Example 21 Loss on Drying

[0096] The drying loss of the prepared capsules was measured using the test method in the 2020 edition of the Chinese Pharmacopoeia. The results are shown in Table 1.

[0097] The results show that the drying weight loss rates of the hydroxypropyl starch-based empty capsules prepared in Examples 1-8 are all less than 15%, which meets the requirements of the Chinese Pharmacopoeia (2020).

[0098] Example 22 Accelerated stability test

[0099] Refer to the test method in the 2020 edition of the Chinese Pharmacopoeia, such as Figure 2 As shown, the capsules were placed in 8-filament polyethylene packaging bags and sealed with a sealing machine, and then the samples were placed in corrugated paper boxes and sealed with tape, and finally placed in a constant temperature and humidity test box (purchased from Shanghai Yiheng Instrument Co., Ltd.) with set conditions, set at 30°C and 65%RH. The accelerated test time was 90 days in total, and the brittleness rate and disintegration time of the capsules were measured every 30 days, for a total of 4 times.

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

[0101]

[0102] In summary, we utilize the high amylose content, low gelatinization temperature and anti-retrogradation characteristics of hydroxypropyl pea starch, combined with the enhancement of the mechanical properties and water solubility of polyvinyl alcohol and hydroxypropyl methylcellulose on the starch matrix, to prepare a hydroxypropyl starch composition, and further prepare starch-based hard capsules. The prepared hollow hard capsules have great improvements in friability, disintegration time, storage stability and many other aspects. The hollow hard capsules prepared by the composition prepared by the present invention have a smooth surface, good transparency, and a high molding rate (>95%). It has the advantages of strong resistance to brittleness (no brittleness), short disintegration time (<10 min), and good storage stability (≥90 days under accelerated conditions). It meets the standards for hollow hard capsules in the "Chinese Pharmacopoeia" (2020 edition), reaches the quality of commercial gelatin capsules, and can provide an important reference for replacing traditional gelatin capsules. The preparation method of the invention is simple and low in cost. The prepared hydroxypropyl starch-based hollow hard capsules have good appearance and formability, and are remarkable in terms of resistance to brittleness, rapid disintegration, stable storage, etc. Therefore, the capsules have great application prospects in medical preparations, food packaging materials, health care product packaging, etc.

[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 in the protection scope of the present invention.

Claims

1. A hydroxypropyl starch-based composition comprising: hydroxypropyl starch, polyvinyl alcohol, glycerol, sorbitol, carrageenan, potassium acetate, hydroxypropyl methylcellulose, and dimethicone.

2. The hydroxypropyl starch-based composition of claim 1, 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)。 3. The hydroxypropyl starch-based composition of claim 2, characterized in that Hydroxypropyl starch: The mass ratio of polyvinyl alcohol: glycerol: 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)。 4. The hydroxypropyl starch-based composition of claim 3, characterized in that Hydroxypropyl starch: The mass ratio of polyvinyl alcohol: glycoside oil: sorbitol: carrageenan: potassium acetate: hydroxypropyl methylcellulose: dimethicone is 1: 0.05: 0.04: (0.01-0.02): (0007-0.021): (0007-0.021): (0.001-0.005): (0007-0.014).

5. The hydroxypropyl starch-based composition of claim 4, characterized in that Hydroxypropyl starch: The mass ratio of polyvinyl alcohol: glycerol: 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).

6. The hydroxypropyl starch-based composition of claim 5, characterized in that Hydroxypropyl starch: The mass ratio of polyvinyl alcohol: glycerol: 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).

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

8. The hydroxypropyl starch-based composition of claim 7, characterized in that Hydroxypropyl starch: The mass ratio of 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).

9. The hydroxypropyl starch-based composition of claim 8, characterized in that Hydroxypropyl starch: The mass ratio of 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.

10. The hydroxypropyl starch-based composition of claim 1, characterized in that: The starch source is pea starch.

11. The hydroxypropyl starch-based composition of claim 1, characterized in that It also contains water, wherein the water accounts for 82.9% to 84.2% of the total weight of the composition.

12. The hydroxypropyl starch-based composition of claim 11, characterized in that Water accounts for 83.5% of the total mass of the composition.

13. A hollow hard capsule prepared from the hydroxypropyl starch-based composition according to claim 1.

14. A method for preparing the capsule according to claim 13: Mix hydroxypropyl starch and water evenly to obtain solution A, mix carrageenan and water evenly to obtain solution B, heat and stir solutions A and B at 85-95° C. for 40-80 min, then mix the two, add polyvinyl alcohol, glycerol, sorbitol, potassium acetate, hydroxypropyl methylcellulose, and dimethicone, continue heating and stirring at 85-95° C. for 60-90 min, then balance at 75-85° C. for 0-15 min, dip a capsule mold in the glue, dry for 4-6 h, and demold to obtain a hollow hard capsule.

15. The method for preparing the capsule according to claim 14, characterized in that: Before mixing solutions A and B, they were heated and stirred at 90°C for 60 min.

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

17. The method for preparing the capsule according to claim 14, characterized in that: Equilibrate at 80°C for 5 min.

18. The method for preparing the capsule according to claim 14, characterized in that: Dry at 40℃ for 5h.

19. A method for preparing the capsule according to claim 13: Mix hydroxypropyl starch and water evenly to obtain solution A, mix carrageenan and water evenly to obtain solution B, mix solutions A and B, heat and stir at 85-95° C. for 40-80 min, add polyvinyl alcohol, glycerol, sorbitol, potassium acetate, hydroxypropyl methylcellulose and dimethicone, continue heating and stirring at 85-95° C. for 60-90 min, then balance at 75-85° C. for 0-15 min, dip a capsule mold in the glue, dry for 4-6 h, and demold to obtain a hollow hard capsule.

20. Use of the hydroxypropyl starch-based composition according to claim 1 in the preparation of hollow hard capsules.

21. The use according to claim 20, wherein the hard capsule material can be used for humans and animals.

22. The use according to claim 21, wherein the hard capsule material can be used for pets.

23. The use of claim 20, wherein the hard capsule material comprises: Pharmaceutical packaging materials, health care product packaging materials, food packaging materials.

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