A low-ester pectin microcapsule powder, capsule core material, capsule and its application

Abstract

The present invention provides a low-ester pectin microcapsule powder, a capsule core material, a capsule and their applications, belonging to the technical field of health foods. The present invention microencapsulates low-ester pectin by using an aqueous dispersion of polyacrylic acid resin and / or chitosan to obtain a low-ester pectin microcapsule powder. After entering the stomach, the low-ester pectin microcapsule powder can first disperse without agglomeration and then fully react with gastric acid to dissolve. The dissolved low-ester pectin then undergoes a bridging reaction with divalent cations precipitated from gastric acid to form a stable gel, enabling it to fully achieve the expected effects of increasing satiety and reducing postprandial blood glucose. The capsules of the present invention can improve blood glucose management and satiety in a convenient, controllable and effective manner, providing a convenient and effective auxiliary tool for people who need to manage blood glucose and body weight. Compared with traditional dietary interventions and drug treatments, the capsules of the present invention have the advantages of convenient administration, few side effects and stable effects.

Description

Technical Field

[0001] The present invention belongs to the technical field of health foods, and particularly relates to a low-ester pectin microcapsule powder, a capsule core material, a capsule and their applications. Background Art

[0002] Pectin is a natural polysaccharide with high cellulose and is widely present in fruits and vegetables. Research shows that pectin has good satiety and the effect of reducing postprandial blood glucose. This is mainly because pectin absorbs water and swells in the stomach to form a gel-like substance, which can prolong satiety and slow down the gastric emptying rate, thereby reducing the rapid rise of postprandial blood glucose. In addition, pectin is beneficial to reducing cholesterol and improving intestinal health. At the same time, it is found that divalent cation metal salts react with low-ester pectin under the action of gastric acid to form a more stable gel through a bridging reaction, so as to better control the retention time of food in the stomach, prolong satiety, and reduce the rapid rise of postprandial blood glucose (see

Cao L, LuW, MataA, Nishinari K, FangY. Egg-box model-based gelation of alginate and pectin: A review. Carbohydr Polym. 2020 Aug 15;242:116389. doi:10.1016 / j.carbpol.2020.116389. Epub 2020 May 14. PMID:32564839.

Celus, M., Kyomugasho, C., Salvia-Trujillo, L., Audenhove, J.V., Loey, A.M.V., Grauwet, T., et al. (2018). Interactions between citrus pectin and Zn2+ or Ca2+ and associated in vitro Zn2+ bioaccessibility as affected by degree of methylesterification and blockiness. Food Hydrocolloids, 79, 319-330.

[0003] The object of the present invention is to provide a low-ester pectin microcapsule powder, a capsule core material, a capsule and their applications. The present invention ensures the bridging reaction effect between low-ester pectin and divalent cations, so that the expected effects of increasing satiety and reducing postprandial blood glucose are fully achieved.

[0004] The present invention provides a low-ester pectin microcapsule powder, and the raw materials for preparation include a core material and a wall material; the core material includes low-ester pectin; the wall material includes an aqueous dispersion of polyacrylic resin and / or chitosan; the particle size of the low-ester pectin microcapsule powder is 150 - 300 μm.

[0005] The present invention also provides a preparation method of the low-ester pectin microcapsule powder described in the above solution, including the following steps:

[0006] Mix low-ester pectin and water to obtain a mucilage;

[0007] Mix the mucilage and the wall material to obtain a low-ester pectin microcapsule liquid;

[0008] Dry and sieve the low-ester pectin microcapsule liquid to obtain a low-ester pectin microcapsule powder.

[0009] The present invention also provides a capsule core material, including a low-ester pectin microcapsule powder and a divalent cation metal salt; the mass ratio of the low-ester pectin microcapsule powder to the divalent cation metal salt is (15 - 30):(0.4 - 1.8);

[0010] The low-ester pectin microcapsule powder includes the low-ester pectin microcapsule powder described in claim 1 or the low-ester pectin microcapsule powder prepared by the preparation method described in claim 2.

[0011] Preferably, the divalent cation metal salt includes one or more of calcium salts, magnesium salts and divalent iron salts.

[0012] Preferably, the capsule core material does not contain a disintegrant.

[0013] The present invention also provides a capsule, including a capsule shell and the capsule core material described in the above solution.

[0014] Preferably, the capsule shell includes a hypromellose capsule shell.

[0015] Preferably, the capsule shell contains a disintegrant.

[0016] Preferably, the capsule shell includes the following components in mass percentage: 13 - 25% hypromellose, 0.1 - 0.6% gelling agent, 0.01 - 0.3% plasticizer, 0.02 - 0.04% coagulant aid, 0.01 - 0.3% disintegrant and the balance of water.

[0017] The present invention also provides an application of the low-ester pectin microcapsule powder described in the above solution, or the low-ester pectin microcapsule powder prepared by the preparation method described above, or the capsule core material or the capsule in the preparation of a product for reducing postprandial blood glucose and / or increasing satiety.

[0018] The present invention provides a low-ester pectin microcapsule powder, the core material includes low-ester pectin, and the wall material includes an aqueous dispersion of polyacrylic resin and / or chitosan; the particle size of the low-ester pectin microcapsule powder is 150-300 μm. In the present invention, the aqueous dispersion of polyacrylic resin and / or chitosan can remain stable in a neutral environment and can be dissolved in the stomach. The present invention uses the aqueous dispersion of polyacrylic resin and / or chitosan to microencapsulate low-ester pectin to obtain low-ester pectin microcapsule powder. After entering the stomach, the low-ester pectin microcapsule powder can first disperse without agglomeration and then fully react with gastric acid to dissolve. The dissolved low-ester pectin then undergoes a bridging reaction with divalent cations precipitated from gastric acid to form a stable gel, so as to fully achieve the expected effects of increasing satiety and reducing postprandial blood glucose. Brief Description of the Drawings

[0019] In order to more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the following will briefly introduce the drawings required to be used in the embodiments. Obviously, the drawings in the following description are only some embodiments of the present invention. For those of ordinary skill in the art, other drawings can be obtained based on these drawings without creative efforts.

[0020] Figure 1 It is a line graph of the average value of blood glucose response within 120 minutes after a meal;

[0021] Figure 2 It is a comparison of the area under the curve of the average blood glucose increase 2 hours after a meal;

[0022] Figure 3 It is a line graph of the average value of the eating desire score 3.5 hours after a meal;

[0023] Figure 4 It is a line graph of the average value of the hunger score 3.5 hours after a meal;

[0024] Figure 5 It is a line graph of the average value of the satiety score 3.5 hours after a meal;

[0025] Figure 6 It is a line graph of the average value of the expected food intake score 3.5 hours after a meal;

[0026] Figure 7 It is a line graph of the average value of the fullness score 3.5 hours after a meal;

[0027] Figure 8 It is a line graph of the average value of the total appetite suppression score 3.5 hours after a meal;

[0028] Figure 9 It is the area under the curve graph of the total appetite suppression score at 3.5 h after a meal;

[0029] Figure 10 It is the dissolution result of Example 1 at 7 min;

[0030] Figure 11 It is the dissolution result of Comparative Example 1 at 7 min;

[0031] Figure 12 It is the dissolution result of Comparative Example 2 at 7 min;

[0032] Figure 13 It is the production process flow chart. Detailed implementation manners

[0033] The present invention provides a low-ester pectin microcapsule powder, and the raw materials for preparation include a core material and a wall material; the core material includes low-ester pectin; the wall material includes an aqueous dispersion of polyacrylic resin and / or chitosan; the particle size of the low-ester pectin microcapsule powder is 150 - 300 μm.

[0034] In the present invention, the degree of esterification of the low-ester pectin is preferably 20% - 50%, more preferably 30% - 40%.

[0035] In the present invention, the wall material is a wall material that dissolves in the stomach and is stable in a neutral environment.

[0036] In the present invention, the wall material is preferably an aqueous dispersion of polyacrylic resin, which is a stable and homogeneous liquid with water as the dispersion medium obtained by copolymerizing dimethylaminoethyl methacrylate and methacrylate through adding a dispersion aid and a physical dispersion process. In the present invention, the aqueous dispersion of polyacrylic resin is sourced from conventional commercial products. In the specific implementation process of the present invention, the aqueous dispersion of polyacrylic resin is purchased from Rohm Company in Germany, and the specification model is: Eudragit E30D.

[0037] In the present invention, the raw materials for preparing the low-ester pectin microcapsule powder preferably further include water.

[0038] In the present invention, when the wall material is an aqueous dispersion of polyacrylic resin, the mass ratio of the low-ester pectin to the aqueous dispersion of polyacrylic resin is (3 - 6):(1 - 3) or (20 - 40):(5 - 8), more preferably (3 - 6):2.

[0039] After the low-ester pectin is microencapsulated by coating with a gastric-soluble coating material (aqueous dispersion of polyacrylic resin and / or chitosan), it can be fully dispersed and dissolved in the stomach. At the same time, when the divalent cation metal salt encounters gastric acid, divalent cations are precipitated, and the dispersed and dissolved low-ester pectin reacts with the divalent cations to form a gel. The resulting gel system has a high degree of structural integrity and can provide a better sense of fullness after consumption.

[0040] The present invention also provides a method for preparing the low-ester pectin microcapsule powder described in the above solution, which includes the following steps: mixing low-ester pectin and water to obtain a gum slurry; mixing the gum slurry and a wall material to obtain a low-ester pectin microcapsule liquid; drying and sieving the low-ester pectin microcapsule liquid to obtain the low-ester pectin microcapsule powder.

[0041] The present invention first mixes low-ester pectin and water to obtain a gum slurry.

[0042] In the present invention, the water is preferably purified water; the temperature of the mixing is preferably 40-100°C; after the mixing, the present invention preferably further includes homogenizing the mixed material; the time of the homogenization is preferably 15-45 min; the equipment used for the homogenization is preferably a homogenizer.

[0043] After obtaining the gum slurry, the present invention mixes the gum slurry and a wall material to obtain a low-ester pectin microcapsule liquid.

[0044] In the present invention, mixing the gum slurry and a wall material preferably includes adding the gum slurry to the wall material; the mixing method is preferably stirring and mixing; the time of the stirring and mixing is preferably 20-50 min.

[0045] After obtaining the low-ester pectin microcapsule liquid, the present invention dries and sieves the low-ester pectin microcapsule liquid to obtain the low-ester pectin microcapsule powder.

[0046] Before the drying, the present invention preferably further includes filtering the low-ester pectin microcapsule liquid through a 40-mesh sieve to remove insoluble substances; the drying method is preferably spray drying; the inlet air temperature of the spray drying is preferably 170-180°C; the outlet air temperature of the spray drying is preferably 70-90°C; the water content of the dried low-ester pectin microcapsule powder is preferably ≤2%; the equipment used for the spray drying is preferably a spray dryer.

[0047] In the present invention, the sieving preferably includes: passing the dried material through a 50-mesh sieve, passing the sieved powder through a 100-mesh sieve, and retaining the powder that cannot pass through the 100-mesh sieve, thus obtaining the low-ester pectin microcapsule powder with a particle size of 150-300 μm.

[0048] The present invention also provides a capsule core material, which comprises low-ester pectin microcapsule powder and divalent cation metal salt; the mass ratio of the low-ester pectin microcapsule powder to the divalent cation metal salt is (15 - 30):(0.4 - 1.8); the low-ester pectin microcapsule powder comprises the low-ester pectin microcapsule powder described in the above solution or the low-ester pectin microcapsule powder prepared by the described preparation method.

[0049] In the present invention, the divalent cation metal salt preferably comprises one or more of calcium salt, magnesium salt and divalent iron salt.

[0050] In the present invention, the mass ratio of the low-ester pectin microcapsule powder to the divalent cation metal salt is preferably (15 - 30):1. In the embodiments of the present invention, the mass ratio of the low-ester pectin microcapsule powder to the divalent cation metal salt is 450:16, 482:18 or 516:32.

[0051] In the present invention, the capsule core material preferably does not contain a disintegrant. The capsule core material of the present invention does not add a disintegrant, which can avoid the gas being filled while the gel formed by the cross-linking reaction of low-ester pectin and divalent cations is diffused, thereby ensuring the stability of the gel colloid.

[0052] In the present invention, the preparation method of the capsule core material preferably comprises the following steps:

[0053] First mix a part of the low-ester pectin microcapsule powder and the divalent cation metal salt to obtain a premix; then second mix the premix and the remaining low-ester pectin microcapsule powder to obtain the capsule core material; the mass ratio of the part of the low-ester pectin microcapsule powder to the divalent cation metal salt is preferably 1:1.

[0054] In the present invention, the first mixing preferably comprises: shaking and mixing in a transparent bag, observing the dispersion of the divalent cation metal salt, gently kneading the agglomerated materials through the transparent bag, and performing premixing after complete dispersion; the transparent bag is preferably a PE bag; the premixing is preferably carried out by a mixer; the premixing time is preferably 5 - 30 min.

[0055] In the present invention, the second mixing preferably comprises: passing the premix and the remaining low-ester pectin microcapsule powder through a 20-mesh vibrating sieve and then performing total mixing; the total mixing is preferably carried out by a mixer; the total mixing time is preferably 20 - 60 min.

[0056] The present invention also provides a capsule, which comprises a capsule shell and the capsule core material described in the above solution.

[0057] The present invention has no special limitation on the ratio of the capsule shell to the capsule core material, and the capsule core material fills the capsule shell.

[0058] In the present invention, the capsule shell is a hollow capsule shell. In the present invention, the capsule shell preferably comprises a hypromellose capsule shell. In the present invention, the capsule shell preferably contains a disintegrant, and the function of adding the disintegrant is to promote the decomposition and dissolution of the capsule shell. In the present invention, the thickness of the shell wall fitting part of the capsule shell is preferably 50-80 μm, and the thickness of other parts of the shell body is preferably 80-120 μm. The reason for controlling this specification is that after the capsule shells are fitted together, the thickness of the fitting part is lower. In combination with the form of adding a disintegrant, the capsule can disintegrate and dissolve faster, and the capsule core material can be released more quickly and completely.

[0059] In the present invention, the capsule shell preferably comprises the following components in mass percentage: 13-25% hypromellose, 0.1-0.6% gelling agent, 0.01-0.3% plasticizer, 0.02-0.04% coagulant aid, 0.01-0.3% disintegrant and the balance water.

[0060] A disintegrant is added to the capsule shell wall material of the present invention, and it has a special structure (the shell wall fitting part of the capsule shell). It can completely disintegrate in the stomach quickly after being taken before a meal, quickly release pectin and calcium ions, ensuring the bridging reaction effect of low-ester pectin and divalent cations, and fully achieving the expected effects of increasing satiety and reducing postprandial blood glucose.

[0061] In the present invention, the disintegrant preferably comprises one or more of microcrystalline cellulose, sodium carboxymethyl starch, cross-linked sodium carboxymethyl cellulose and starch, and more preferably microcrystalline cellulose or a mixture of microcrystalline cellulose and sodium carboxymethyl starch.

[0062] In the present invention, the gelling agent preferably comprises one or more of carrageenan, gellan gum, xanthan gum, konjac gum, arabic gum, agar and guar gum, and more preferably xanthan gum.

[0063] In the present invention, the coagulant aid preferably comprises potassium citrate, potassium chloride or calcium chloride, and more preferably potassium chloride.

[0064] In the present invention, the plasticizer preferably comprises one or several of glycerol, sorbitol, polyethylene glycol, propylene glycol, mannitol and xylitol, and more preferably glycerol.

[0065] In the present invention, the preparation method of the capsule shell preferably comprises the following steps:

[0066] Mix hypromellose and the disintegrant, and disperse the mixed material in the first part of water to obtain solution 1;

[0067] Add the gelling agent to the second part of water to swell to obtain solution 2;

[0068] Mix the solution 1 and the solution 2 to obtain the solution 3;

[0069] Add the coagulant aid to the remaining water for dissolution, and mix the obtained solution with the solution 3 to obtain the solution 4;

[0070] Mix the plasticizer with the solution 4 to obtain the solution 5;

[0071] Dip the capsule mold into the solution 5 to form a mold, and dry it to obtain a dried capsule rod;

[0072] Demold, cut, polish the fitting part, and fit the capsule rod to obtain the capsule shell.

[0073] In the present invention, hydroxypropyl methylcellulose and a disintegrant are mixed, and the mixed material is added to the first part of water for dispersion to obtain the solution 1. In the present invention, the water is preferably purified water; the volume content of the first part of water in all the water is preferably 40% to 60%; the temperature of the first part of water is preferably 60 to 90 °C; after adding the mixed material to the first part of water for dispersion, the present invention preferably further includes heat preservation for 20 to 50 min; stirring is preferably carried out during the heat preservation process.

[0074] In the present invention, the gelling agent is added to the second part of water for swelling to obtain the solution 2. In the present invention, the temperature of the second part of water is preferably 20 to 30 °C, more preferably 25 °C; the volume content of the second part of water in all the water is preferably 40% to 60%; the swelling preferably includes stirring and swelling; after the swelling, the present invention preferably further includes heating the swollen material to 80 to 95 °C and keeping it warm and standing for 30 to 60 min.

[0075] After obtaining the solution 1 and the solution 2, in the present invention, the solution 1 and the solution 2 are mixed to obtain the solution 3. In the present invention, the mixing is preferably carried out in a mixing kettle; the mixing is preferably stirring mixing; the stirring mixing time is preferably 5 to 20 min; after the mixing, the present invention preferably further includes cooling the mixed material to 40 to 70 °C.

[0076] After obtaining the solution 3, in the present invention, the coagulant aid is added to the remaining water for dissolution, and the obtained solution is mixed with the solution 3 to obtain the solution 4. In the present invention, the volume content of the remaining water in all the water is preferably 1% to 5%; the temperature of the water is preferably 40 to 60 °C; the dissolution is preferably stirring dissolution; during the process of mixing the obtained solution with the solution 3, stirring and vacuum filtration for degassing are preferably further included; after the mixing, the present invention preferably further includes cooling the mixed material to 40 to 60 °C.

[0077] After obtaining Solution 4, the present invention mixes a plasticizer with Solution 4 to obtain Solution 5. During the mixing process, stirring and vacuum filtration degassing are preferably included in the present invention; after the mixing, the present invention preferably further includes allowing the mixed material to stand at a temperature of 50-55°C for 1-2 h.

[0078] After obtaining Solution 5, the present invention dips a capsule mold into Solution 5 to form a mold, and then dries it to obtain a dried capsule rod. In the present invention, the temperature for dipping and forming the mold is preferably 40-60°C; the relative humidity for dipping and forming the mold is preferably 45%-65%. In the present invention, the drying temperature is preferably 20-35°C; the relative humidity for drying is preferably 30%-45%; the drying time is preferably 2-3 h.

[0079] After obtaining the dried capsule rod, the present invention demolds, cuts, polishes the fitting part, and fits the capsule rod to obtain a capsule shell.

[0080] The capsules of the present invention can be paired with any food and taken before meals, which can reduce postprandial blood glucose, and the eating method is convenient and easy to implement. The capsules of the present invention can improve blood glucose management and satiety in a convenient, controllable and effective manner, providing a convenient and effective auxiliary tool for people who need to manage blood glucose and body weight. Compared with traditional dietary intervention and drug treatment, the capsules of the present invention have the advantages of convenient administration, few side effects, and stable effects.

[0081] In the present invention, the capsules are preferably prepared by the following method: filling the capsule core material into the capsule shell, fitting the capsule cap body, and polishing to obtain the capsules.

[0082] The present invention also provides the application of the low-ester pectin microcapsule powder described in the above solution, or the low-ester pectin microcapsule powder prepared by the preparation method described above, or the capsule core material, or the capsule in the preparation of products for reducing postprandial blood glucose and / or increasing satiety.

[0083] To further illustrate the present invention, the following describes in detail a low-ester pectin microcapsule powder, a capsule core material, a capsule and their applications provided by the present invention with reference to the accompanying drawings and embodiments, but they should not be construed as limiting the protection scope of the present invention.

[0084] Example 1

[0085] The flowchart is shown in Figure 13 。

[0086] Preparation of the filler: 5 kg of low-ester pectin was added to purified water at 60°C and homogenized using a homogenizer for 20 min to prepare a pectin paste.

[0087] Take 1.2 kg of polyacrylic resin aqueous dispersion, add the homogenized pectin mucilage to the polyacrylic resin aqueous dispersion, and stir for 30 min to obtain low-ester pectin microcapsule liquid.

[0088] Filter the insoluble substances from the low-ester pectin microcapsule liquid through a 40-mesh sieve, and spray-dry the low-ester pectin microcapsule liquid using a spray dryer to obtain low-ester pectin microcapsule powder.

[0089] Pass the low-ester pectin microcapsule powder through a 50-mesh sieve, and then pass the sieved powder through a 100-mesh sieve. Retain the powder that cannot pass through the 100-mesh sieve to obtain low-ester pectin microcapsule powder with a particle size of 150 - 300 μm.

[0090] Weigh 450 g of low-ester pectin microcapsule powder with a particle size of 150 - 300 μm and 16 g of magnesium oxide.

[0091] Weigh an equal amount of low-ester pectin microcapsule powder as that of magnesium oxide, put it into a PE bag together with magnesium oxide, shake and mix them, observe the dispersion of magnesium oxide, gently knead the agglomerated materials through the plastic bag, and after completely dispersing them, put them into a mixer for premixing for 10 min to obtain a premixed material.

[0092] Put the premixed material together with the remaining low-ester pectin microcapsule powder through a vibrating sieve (20 mesh) and then put it into a mixer for total mixing for 25 min to obtain a filler.

[0093] Capsule preparation: Mix 8 kg of hydroxypropyl methylcellulose and 0.9 kg of microcrystalline cellulose, add them to 27 kg of purified water at 80 °C for dispersion, and keep warm for 35 min under continuous stirring to obtain Solution 1.

[0094] Add 40 g of xanthan gum to 23 kg of purified water at room temperature, stir to swell it, then heat it to 85 °C and keep it warm and static for 30 min to obtain Solution 2.

[0095] Add Solution 2 to Solution 1, continuously stir for 15 min to mix evenly, and then cool it to 50 °C to obtain Solution 3.

[0096] Add 8 g of potassium chloride to 1.3 kg of purified water at 50 °C, stir to dissolve it, then add it to Solution 3, stir and perform vacuum filtration and degassing for 10 min, and cool the solution temperature to 45 °C to obtain Solution 4.

[0097] Add 30 g of glycerol to Solution 4, stir and perform vacuum filtration and degassing for 15 min, and let it stand at 55 °C for 80 min to obtain Solution 5.

[0098] Under the environment of a temperature of 40 °C and a relative humidity of 40%, dip the capsule mold into Solution 5 to form a mold, adjust the shell wall thickness to 100 μm, and then dry it for 2.5 h under the environment of a drying oven temperature of 20 °C and a relative humidity of 32% to obtain a dried capsule rod.

[0099] Finally, through demolding, cutting, and grinding the fitting part to 60 μm, fitting, a plant hollow capsule is made.

[0100] Fill the prepared hollow capsule with the mixed filler to obtain a capsule for reducing postprandial blood glucose and increasing satiety.

[0101] Example 2

[0102] Filler preparation: Add 6.2 kg of low-ester pectin to purified water at 70 °C and homogenize it using a homogenizer for 15 min to prepare a pectin mucilage.

[0103] Take 2.5 kg of polyacrylic resin aqueous dispersion, add the homogenized pectin mucilage to the polyacrylic resin aqueous dispersion, and stir for 30 min to obtain a low-ester pectin microcapsule liquid.

[0104] Filter the insoluble substances from the low-ester pectin microcapsule liquid using a 40-mesh sieve, and spray-dry the low-ester pectin microcapsule liquid using a spray dryer to obtain low-ester pectin microcapsule powder.

[0105] Pass the low-ester pectin microcapsule powder through a 50-mesh sieve, and then pass the sieved powder through a 100-mesh sieve. Retain the powder that cannot pass through the 100-mesh sieve to obtain low-ester pectin microcapsule powder with a particle size of 150 - 300 μm.

[0106] Weigh 482 g of low-ester pectin microcapsule powder with a particle size of 150 - 300 μm and 18 g of calcium oxide.

[0107] Weigh an equal amount of low-ester pectin microcapsule powder as calcium oxide, put it into a PE bag together with calcium oxide, shake and mix, observe the dispersion of calcium oxide, gently knead the agglomerated materials through the plastic bag to make them completely disperse, and then put them into a mixer for premixing for 16 min to obtain a premix.

[0108] Put the premix together with the remaining low-ester pectin microcapsule powder through a vibrating sieve (20 mesh) and then put it into a mixer for total mixing for 28 min to obtain a filler.

[0109] Capsule preparation: Mix 8 kg of hydroxypropyl methylcellulose, 0.5 kg of microcrystalline cellulose, and 0.4 kg of sodium carboxymethyl starch, add them to 27 kg of purified water at 80 °C for dispersion, and keep it warm for 35 min under continuous stirring to obtain Solution 1.

[0110] Add 40 g of xanthan gum to 23 kg of purified water at room temperature, stir to swell, then heat to 85 °C and keep warm and static for 30 min to obtain Solution 2.

[0111] Add Solution 2 to Solution 1, continuously stir for 15 min, mix evenly, and then cool to 50 °C to obtain Solution 3.

[0112] Add 8 g of potassium chloride to 1.3 kg of purified water at 50 °C, stir to dissolve, then add it to Solution 3, stir and perform vacuum filtration and degassing for 10 min, and cool the solution temperature to 45 °C to obtain Solution 4.

[0113] Add 30 g of glycerol to Solution 4, stir and perform vacuum filtration and degassing for 15 min, and let it stand at 55 °C for 80 min to obtain Solution 5.

[0114] In an environment with a temperature of 40 °C and a relative humidity of 40%, dip the capsule mold in Solution 5 to form a mold, adjust the shell wall thickness to 120 μm, and then dry it in an environment with a drying oven temperature of 20 °C and a relative humidity of 32% for 2.5 h to obtain a dried capsule rod.

[0115] Finally, through demolding, cutting, and polishing the fitting part to 80 μm, fitting, plant hollow capsules are made.

[0116] Fill the prepared hollow capsules with the mixed filler to obtain capsules that can reduce postprandial blood glucose and increase satiety.

[0117] Example 3

[0118] Filler preparation: Add 4.7 kg of low-ester pectin to purified water at 65 °C and homogenize it using a homogenizer for 25 min to prepare pectin mucilage.

[0119] Take 1.5 kg of polyacrylic resin aqueous dispersion, add the homogenized pectin mucilage to the polyacrylic resin aqueous dispersion, and stir for 35 min to obtain low-ester pectin microcapsule liquid.

[0120] Filter the insoluble substances in the low-ester pectin microcapsule liquid with a 40-mesh sieve, and spray-dry the low-ester pectin microcapsule liquid using a spray dryer to obtain low-ester pectin microcapsule powder.

[0121] Pass the low-ester pectin microcapsule powder through a 50-mesh sieve, and then pass the sieved powder through a 100-mesh sieve, and retain the powder that cannot pass through the 100-mesh sieve to obtain low-ester pectin microcapsule powder with a particle size of 150 - 300 μm.

[0122] Weigh 516 g of low-ester pectin microcapsule powder with a particle size of 150 - 300 μm and 32 g of anhydrous calcium hydrogen phosphate.

[0123] Weigh an equal amount of low-ester pectin microcapsule powder as that of calcium hydrogen phosphate, put it into a PE bag together with calcium hydrogen phosphate, and shake and mix them. Observe the dispersion of calcium hydrogen phosphate. Knead the agglomerated materials slightly through the plastic bag to make them disperse completely, and then put them into a mixer for premixing for 18 minutes to obtain a premixed material.

[0124] Put the premixed material together with the remaining low-ester pectin microcapsule powder through a vibrating sieve (20 mesh), and then put it into a mixer for total mixing for 30 minutes to obtain a filler.

[0125] Capsule preparation: Mix 8 kg of hydroxypropyl methylcellulose and 0.8 kg of sodium carboxymethylcellulose, add them to 27 kg of purified water at 80 °C for dispersion, and keep warm for 35 minutes under continuous stirring to obtain Solution 1.

[0126] Add 40 g of xanthan gum to 23 kg of purified water at room temperature and stir to swell it, then heat it to 85 °C and keep it warm and static for 30 minutes to obtain Solution 2.

[0127] Add Solution 2 to Solution 1, continuously stir for 15 minutes to mix evenly, and then cool it to 50 °C to obtain Solution 3.

[0128] Add 8 g of potassium chloride to 1.3 kg of purified water at 50 °C and stir to dissolve it, then add it to Solution 3, stir and carry out vacuum filtration and degassing for 10 minutes, and cool the solution temperature to 45 °C to obtain Solution 4.

[0129] Add 30 g of glycerol to Solution 4, stir and carry out vacuum filtration and degassing for 15 minutes, and let it stand at 55 °C for 80 minutes to obtain Solution 5.

[0130] Under the environment of a temperature of 40 °C and a relative humidity of 40%, dip the capsule mold in the cellulose gum solution to form a mold, adjust the shell wall thickness to 90 μm, and then dry it in an environment of a baking room temperature of 20 °C and a relative humidity of 32% for 2.5 hours to obtain a dried capsule rod.

[0131] Finally, through demolding, cutting, grinding the fitting part to 50 μm, and fitting, a plant hollow capsule is made.

[0132] Fill the mixed filler into the made hollow capsule to obtain a capsule for reducing postprandial blood glucose and increasing satiety.

[0133] Comparative Example 1

[0134] On the basis of Example 3, change the low-ester pectin microcapsule powder to ordinary low-ester pectin with an equal pectin content, and keep other parameters unchanged.

[0135] Comparative Example 2

[0136] On the basis of Example 3, the improved hollow capsule shell was changed to a common commercially available hypromellose hollow capsule shell purchased from Jiangsu Chenxing Pharmaceutical Co., Ltd., with the specification: transparent size 0 hypromellose hollow capsule, and other parameters remained unchanged.

[0137] Test Example 1

[0138] Experimental protocol

[0139] Select 10 healthy subjects without blood glucose abnormalities and chronic diseases with a BMI (kg / m 2 ) between 18 and 24 and under 40 years old (as shown in Table 1 below). Conduct 6 tests on 6 experimental days respectively. Specifically: These 10 healthy subjects ate the same kind of meal on each experimental day, namely the standard meal and 5 experimental meals. The subjects had regular work and rest and normal diet in the first three days. They started fasting 12 hours before the test, and only drank 50 - 100 ml of plain water during the fasting period. The fixed unified time on the experimental day was used as the start time for eating, and there was a 2-day interval between each experimental day as the washout period; after the meal, simple daily activities could be carried out, but strenuous exercise was not allowed, and the mood should be kept stable. Do not eat anything and do not drink water or beverages within 3.5 hours; do not drink alcohol the night before the test; do not do strenuous exercise on the morning of the test day; start eating on time and finish the corresponding meal and 250 ml of water on the same day within 5 - 10 minutes.

[0140] The subjects were given a standard meal consisting of 3 commercially available red bean buns (35 g each) plus 250 mL of warm water. On the basis of the standard meal, for the experimental meal, capsules with a total content of 5 g were taken 5 minutes before the meal. There were a total of 5 experimental meals, namely the standard meal plus the capsule of Example 1, the standard meal plus the capsule of Example 2, the standard meal plus the capsule of Example 3, the standard meal plus the capsule of Comparative Example 1, and the standard meal plus the capsule of Comparative Example 2. Blood glucose tests were carried out (blood glucose conditions at 5 minutes before the meal, 15 minutes, 30 minutes, 45 minutes, 60 minutes, 90 minutes, and 120 minutes after the meal), and appetite scores were evaluated (using the Visual Analog Scale questionnaire (VAS) to evaluate the subjective appetite and satiety of the subjects, etc. The specific indicators included satiety, hunger, fullness, and expected food intake. Each indicator was evaluated from 0 to 100 points, representing two extremes. For example, for the evaluation of hunger, 0 points indicated not hungry at all, and 100 points indicated extremely hungry. The first questionnaire was filled out by the subjects within 5 minutes before starting to eat (t0), and then once every 15 minutes for the next 1 hour, and once every 30 minutes after 1 hour, lasting for a total of 3.5 hours. That is, the questionnaire filling time points were: t0, t15, t30, t45, t60, t90, t120, t150, t180, t210. The Overall Appetite Suppression Score (OASS) = [satiety score + fullness score + (100 - hunger score) + (100 - expected food intake score)] / 4).

[0141] The broken line of the average blood glucose within 120 minutes after the meal is as follows Figure 1 shown: The average blood glucose at each time point in the experimental meal group was lower than that in the corresponding time point of only consuming the standard meal. Among them, the differences were significant especially at 15 minutes, 30 minutes, and 90 minutes after the meal.

[0142] And the comparison of the area under the curve of the blood glucose increase within 120 minutes after the meal is as Figure 2 shown: The area under the curve of the blood glucose increase within 120 minutes after the meal in the experimental meal group was significantly lower than that in the standard meal group, indicating that the postprandial blood glucose in the experimental meal group was more stable and the blood glucose fluctuation was smaller.

[0143] The eating desire at 210 minutes after the meal is as Figure 3 shown: In the experimental meal group within 210 minutes, the average eating desire was continuously lower than that in the standard meal group. It can be seen that taking the capsules of the present invention can continuously and effectively reduce the eating desire.

[0144] The hunger at 210 minutes after the meal is as Figure 4As shown: In the first 90 minutes, the average hunger level of the experimental meal group was significantly lower than that of the standard meal group. After 90 minutes, the average hunger levels of both groups were similar, but the situation where the experimental meal group had the same or similar hunger levels occurred approximately 30 minutes later than in the standard meal group, indicating that taking the capsules of the present invention can effectively delay the onset of hunger.

[0145] The satiety graph at 210 minutes after a meal is shown in Figure 5: At the 30th minute after eating, the satiety was the strongest. At the 45th minute and the 60th minute, the satiety of the experimental meal group was similar to that of the standard meal. However, starting from the 90th minute, the downward trend of the satiety score in the experimental meal group was significantly slower than that in the standard meal group.

[0146] The expected food intake at 210 minutes after a meal is as Figure 6 shown: The expected food intake of the experimental meal group was lower than that of the standard meal group at each time point after the meal, indicating that taking the capsules of the present invention with meals can reduce the food intake of the next meal.

[0147] The satiety at 210 minutes after a meal Figure 7 is shown: The satiety of the experimental meal group remained higher than that of the standard meal group at 210 minutes after the meal.

[0148] According to the average value of the total appetite suppression score at 3.5 hours after a meal ( Figure 8 shown) and the area under the curve of the total appetite suppression score at 3.5 hours after a meal ( Figure 9 shown), it can be seen that taking the capsules of the present invention with meals can effectively suppress appetite, reduce the desire to eat, and thus achieve the purpose of weight loss.

[0149] Table 1 Subject Information

[0150]

[0151]

[0152] Test Example 2

[0153] Capsule shell disintegration speed test: According to the regulations on the disintegration time limit of "hydroxypropyl methylcellulose hollow capsules" in the fourth part of the Chinese Pharmacopoeia 2020 edition: Take 6 commercially available ordinary hydroxypropyl methylcellulose capsules (specification: transparent size 0 hydroxypropyl methylcellulose hollow capsules) purchased from Jiangsu Chenxing Pharmaceutical Co., Ltd., 6 commercially available ordinary gelatin capsules (specification: transparent size 0 gelatin hollow capsules) purchased from Anhui Huangshan Capsule Co., Ltd., the capsules prepared in Example 1, the capsules prepared in Example 2, and the capsules prepared in Example 3, each filled with talc powder. When the water temperature in the disintegration apparatus rises to 37 °C, place the capsules in the glass tubes of the hanging basket respectively, and check according to the method for checking the disintegration time limit (General Rule 0921 of the fourth part of the Chinese Pharmacopoeia 2020 edition) for capsules, that is: record the disintegration time (min) of each commercially available capsule or example capsule.

[0154] The test results are shown in Table 2. It can be seen that the capsules prepared in Examples 1 to 3 all started to break and disintegrate within 3 minutes and were completely disintegrated within 8 minutes, which were all shorter than those of common commercially available capsules.

[0155] Table 2 Dissolution time of capsules in each example

[0156] Item Initial disintegration time / min Complete disintegration time / min Commercially available ordinary hypromellose capsules 6′35″ 15′21″ Commercially available ordinary gelatin capsules 3′28″ 8′45″ Example 1 2′24″ 7′26″ Example 2 1′41″ 7′43″ Example 3 1′27″ 6′52″

[0157] Comparison of the dissolution of the capsule contents by the capsule shell: The capsule prepared in Example 3 was used as the experimental sample, and the capsule prepared in Comparative Example 2 was used as the comparative sample. 50 mL of hydrochloric acid solution (9-1000) was prepared in advance and kept at a constant temperature of 37 °C. Start timing when the capsule is placed in this hydrochloric acid solution, stir gently, observe the dissolution of the capsule contents and record the corresponding dissolution time. At 7 minutes, the dissolution result of Example 1 was as Figure 10 shown, and the contents were completely dissolved to form a gel. The dissolution result of Comparative Example 1 was as Figure 11 shown. Similarly, at 7 minutes, the capsule shell was completely dissolved, but the contents agglomerated and failed to form a gel. The dissolution result of Comparative Example 2 was as Figure 12 shown. Similarly, at 7 minutes, there were transparent gel-like lumps around the capsule, and the powder in the central part was hydrated and undissolved, with high hardness.

[0158] It can be seen that in the application of the present invention, if ordinary pectin powder is used, the pectin powder is prone to agglomerate after the capsule disintegrates, does not form a stable gel, affects the cross-linking reaction between pectin and divalent cation metal salts, and cannot achieve the ideal effects of increasing satiety and reducing postprandial blood glucose. At the same time, the faster the capsule disintegration time, the more rapidly the low-ester pectin microcapsule powder can be dispersed in the gastric juice, avoiding the situation that due to the slow disintegration of the capsule shell, the low-ester pectin microcapsule powder cannot be dispersed after partial breakage and reacts with the gastric juice at the breakage to cause hydration, resulting in the incomplete reaction of the filler in the capsule to form a gel, affecting the effects of the product in increasing satiety and reducing postprandial blood glucose.

[0159] The experimental protocol was the same as the blood glucose detection and appetite scoring protocol in the examples.

[0160] Comparative Example 3

[0161] The instant low-ester pectin powder was used to replace the low-ester pectin microcapsule powder, and the rest was the same as in Example 3.

[0162] Using the instant low-ester pectin powder to replace the low-ester pectin microcapsule powder can also make the pectin disperse in the stomach without agglomeration after the capsule dissolves, achieving the purpose of increasing satiety and reducing postprandial blood glucose. However, the instant pectin powder has a loose texture and a small bulk density, making the filling quality of the capsule smaller. When consuming an equal effective dose, more capsules need to be taken, greatly increasing the difficulty of taking and making it difficult for people to execute for a long time.

[0163] Comparative Example 4

[0164] Using ordinary pectin + divalent cation metal salt, carrying a disintegrant and / or an effervescent agent

[0165] It can prevent pectin from undergoing a hydration reaction. A large number of bubbles will be generated when the disintegrant and / or effervescent agent undergoes a bridging reaction with pectin and divalent cations, which may affect the viscosity of the generated gel, and its effect needs to be further verified.

[0166] Although the above embodiments have described the present invention in detail, they are only a part of the embodiments of the present invention, rather than all embodiments. People can also obtain other embodiments based on these embodiments without creative efforts, and these embodiments all fall within the protection scope of the present invention.

Claims

1. A capsule core material, characterized in that, It includes low-ester pectin microcapsule powder and divalent cation metal salts; the mass ratio of the low-ester pectin microcapsule powder to the divalent cation metal salts is (15 - 30):(0.4 - 1.8); The raw materials for preparing the low-ester pectin microcapsule powder consist of a core material and a wall material; the core material is low-ester pectin; the wall material is an aqueous dispersion of polyacrylic resin; the particle size of the low-ester pectin microcapsule powder is 150 - 300 μm; The divalent cation metal salts include one or more of calcium salts, magnesium salts, and divalent iron salts; The capsule core material does not contain a disintegrant.

2. The capsule core material according to claim 1, wherein The method for preparing the low-ester pectin microcapsule powder includes the following steps: Mix low-ester pectin and water to obtain a mucilage; Mix the mucilage with the wall material to obtain a low-ester pectin microcapsule liquid; Dry and sieve the low-ester pectin microcapsule liquid to obtain low-ester pectin microcapsule powder.

3. A capsule, characterized in that, It includes a capsule shell and the capsule core material as claimed in claim 1 or 2.

4. The capsule according to claim 3, characterized in that, The capsule shell includes a hypromellose capsule shell.

5. The capsule according to claim 3 or 4, characterized in that, The capsule shell contains a disintegrant.

6. The capsule according to claim 5, characterized in that, The capsule shell includes the following components in mass percentage: 13 - 25% hypromellose, 0.1 - 0.6% gelling agent, 0.01 - 0.3% plasticizer, 0.02 - 0.04% coagulant aid, 0.01 - 0.3% disintegrant, and the balance water.

7. Use of the capsule core material as claimed in claim 1 or 2 or the capsule as claimed in any one of claims 3 - 6 in the preparation of a product for reducing postprandial blood glucose and / or increasing satiety.

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