CN114306273B - Multilayer hollow capsule and preparation method thereof - Google Patents
Multilayer hollow capsule and preparation method thereof Download PDFInfo
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- CN114306273B CN114306273B CN202210025652.5A CN202210025652A CN114306273B CN 114306273 B CN114306273 B CN 114306273B CN 202210025652 A CN202210025652 A CN 202210025652A CN 114306273 B CN114306273 B CN 114306273B
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- 239000002775 capsule Substances 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title abstract description 9
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 58
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 58
- 239000001341 hydroxy propyl starch Substances 0.000 claims abstract description 47
- 235000013828 hydroxypropyl starch Nutrition 0.000 claims abstract description 47
- 238000001035 drying Methods 0.000 claims description 47
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 45
- 235000019422 polyvinyl alcohol Nutrition 0.000 claims description 41
- 239000003292 glue Substances 0.000 claims description 40
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 38
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 38
- 239000000243 solution Substances 0.000 claims description 38
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 30
- 235000010418 carrageenan Nutrition 0.000 claims description 24
- 229920001525 carrageenan Polymers 0.000 claims description 24
- 238000007598 dipping method Methods 0.000 claims description 23
- 239000011259 mixed solution Substances 0.000 claims description 21
- 239000000679 carrageenan Substances 0.000 claims description 20
- 229940113118 carrageenan Drugs 0.000 claims description 20
- UHVMMEOXYDMDKI-JKYCWFKZSA-L zinc;1-(5-cyanopyridin-2-yl)-3-[(1s,2s)-2-(6-fluoro-2-hydroxy-3-propanoylphenyl)cyclopropyl]urea;diacetate Chemical compound [Zn+2].CC([O-])=O.CC([O-])=O.CCC(=O)C1=CC=C(F)C([C@H]2[C@H](C2)NC(=O)NC=2N=CC(=CC=2)C#N)=C1O UHVMMEOXYDMDKI-JKYCWFKZSA-L 0.000 claims description 20
- 235000011164 potassium chloride Nutrition 0.000 claims description 19
- 239000001103 potassium chloride Substances 0.000 claims description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 239000000377 silicon dioxide Substances 0.000 claims description 17
- 235000012239 silicon dioxide Nutrition 0.000 claims description 17
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 16
- CHHHXKFHOYLYRE-UHFFFAOYSA-M 2,4-Hexadienoic acid, potassium salt (1:1), (2E,4E)- Chemical compound [K+].CC=CC=CC([O-])=O CHHHXKFHOYLYRE-UHFFFAOYSA-M 0.000 claims description 15
- 235000015165 citric acid Nutrition 0.000 claims description 15
- 239000004302 potassium sorbate Substances 0.000 claims description 15
- 235000010241 potassium sorbate Nutrition 0.000 claims description 15
- 229940069338 potassium sorbate Drugs 0.000 claims description 15
- 229920002472 Starch Polymers 0.000 claims description 12
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 12
- 239000008107 starch Substances 0.000 claims description 12
- 235000019698 starch Nutrition 0.000 claims description 12
- BVKZGUZCCUSVTD-UHFFFAOYSA-M Bicarbonate Chemical compound OC([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-M 0.000 claims description 11
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 11
- 235000011187 glycerol Nutrition 0.000 claims description 10
- 239000011736 potassium bicarbonate Substances 0.000 claims description 10
- 235000015497 potassium bicarbonate Nutrition 0.000 claims description 10
- 229910000028 potassium bicarbonate Inorganic materials 0.000 claims description 10
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 claims description 10
- 229920001661 Chitosan Polymers 0.000 claims description 9
- 239000004373 Pullulan Substances 0.000 claims description 9
- 229920001218 Pullulan Polymers 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- 235000019423 pullulan Nutrition 0.000 claims description 9
- 229920001612 Hydroxyethyl starch Polymers 0.000 claims description 8
- 229940050526 hydroxyethylstarch Drugs 0.000 claims description 8
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 8
- 235000017550 sodium carbonate Nutrition 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 7
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 6
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 6
- 235000011181 potassium carbonates Nutrition 0.000 claims description 6
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 235000010413 sodium alginate Nutrition 0.000 claims description 5
- 239000000661 sodium alginate Substances 0.000 claims description 5
- 229940005550 sodium alginate Drugs 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 4
- 239000011734 sodium Substances 0.000 claims description 4
- 229910052708 sodium Inorganic materials 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 239000012528 membrane Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 3
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 3
- 239000004925 Acrylic resin Substances 0.000 claims description 2
- 229920000178 Acrylic resin Polymers 0.000 claims description 2
- 238000000465 moulding Methods 0.000 claims description 2
- 239000001254 oxidized starch Substances 0.000 claims description 2
- 235000013808 oxidized starch Nutrition 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 7
- 230000002349 favourable effect Effects 0.000 abstract description 3
- 239000000853 adhesive Substances 0.000 abstract 1
- 230000001070 adhesive effect Effects 0.000 abstract 1
- 239000007787 solid Substances 0.000 description 14
- 230000000694 effects Effects 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 7
- 238000010008 shearing Methods 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 230000001276 controlling effect Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000001879 gelation Methods 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 239000005543 nano-size silicon particle Substances 0.000 description 2
- 229920002689 polyvinyl acetate Polymers 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 description 1
- NKWPZUCBCARRDP-UHFFFAOYSA-L calcium bicarbonate Chemical compound [Ca+2].OC([O-])=O.OC([O-])=O NKWPZUCBCARRDP-UHFFFAOYSA-L 0.000 description 1
- 229910000020 calcium bicarbonate Inorganic materials 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 125000005587 carbonate group Chemical group 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000003349 gelling agent Substances 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- -1 hydroxypropyl methyl Chemical group 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 229910001414 potassium ion Inorganic materials 0.000 description 1
- 239000003755 preservative agent Substances 0.000 description 1
- 230000002335 preservative effect Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W90/00—Enabling technologies or technologies with a potential or indirect contribution to greenhouse gas [GHG] emissions mitigation
- Y02W90/10—Bio-packaging, e.g. packing containers made from renewable resources or bio-plastics
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- Medicinal Preparation (AREA)
Abstract
The application provides a multilayer hollow capsule and a preparation method thereof, and belongs to the technical field of capsule preparations. The polyvinyl alcohol hydroxypropyl starch adhesive comprises a polyvinyl alcohol layer and a hydroxypropyl starch layer, wherein a connecting layer is arranged between the polyvinyl alcohol layer and the hydroxypropyl starch layer, the polyvinyl alcohol layer is an inner layer, and the hydroxypropyl starch layer is an outer layer, or the polyvinyl alcohol layer is an outer layer and the hydroxypropyl starch layer is an inner layer. The hollow capsule inlayer of multilayer of this application is inseparabler with outer being connected, and the toughness and the intensity of capsule are bigger, and the friability index also has big improvement, and simultaneously, multilayer structure still is favorable to reducing the raw materials cost of capsule.
Description
Technical Field
The application relates to a multilayer hollow capsule and a preparation method thereof, belonging to the technical field of capsule preparations.
Background
The preparation process of the hollow capsule comprises the steps of sol, glue dipping, drying, demoulding, shearing, glue sleeving and the like, and at present, the production and manufacturing processes of the hollow capsule are all one-time glue dipping-drying-forming processes, so that the operation is simple, but the one-time glue dipping forming has many defects, such as high raw material cost in the production process; two or more main raw materials (such as starch and cellulose) cannot be uniformly mixed; the single property is shown, the double-layer effect cannot be exerted at the same time, and the synergistic effect cannot be realized; and the starch capsule always has the problem that the friability index is not qualified. The prior art method utilizes various starch raw materials for trial production, and is difficult to obtain ideal starch capsules. Therefore, how to improve the friability of the starch empty capsules is a key technical problem to be solved.
Disclosure of Invention
In view of this, the application provides a multilayer hollow capsule, not only has fine toughness and intensity, and the friability index can be improved by a wide margin, can reduce hollow capsule raw materials cost simultaneously.
Specifically, the application is realized through the following scheme:
a multi-layer hollow capsule comprises a polyvinyl alcohol layer and a hydroxypropyl starch layer, a connecting layer is arranged between the polyvinyl alcohol layer and the hydroxypropyl starch layer,
the polyvinyl alcohol layer is composed of the following components in parts by mass:
the hydroxypropyl starch layer is composed of the following components in parts by mass:
the connecting layer is a cavity structure layer formed by drying a mixed solution on the surface of a corresponding layer, wherein the mixed solution comprises 2-15 parts by mass of carrageenan and 75-98 parts by mass of carbonate and/or bicarbonate.
The hollow capsule of this application adopts two-layer three group's structures: hydroxypropyl starch layer and polyvinyl alcohol layer are core structure layer, and mixed solution can form the hole on the layer structure surface of processing earlier when drying, and when carrying out second floor structure man-hour this moment, this structure will be filled earlier in the hole, and this hole forms the articulamentum between the two, and the articulamentum of hole structure makes inside and outside two-layer combination more inseparable, plays the effect of tenon fourth of the twelve earthly branches, is favorable to the combination between hydroxypropyl starch layer and the polyvinyl alcohol layer. In the two hierarchical structures, carrageenan is used as a gelling agent, so that the glue solution can be coagulated and formed; potassium chloride promotes gelation; citric acid is used for regulating the pH value and promoting the decomposition of carbonate; potassium sorbate can be used as a source of potassium ions and also as a preservative.
Based on the differences in the core ingredients (polyvinyl alcohol, hydroxypropyl starch), silica and glycerol were added separately. The three functions of the silicon dioxide are that firstly, the silicon dioxide can assist to generate a porous structure on the surface of the polyvinyl alcohol layer, secondly, the nano silicon dioxide on the surface of the polyvinyl alcohol layer can also increase the specific surface area of the polyvinyl alcohol layer and can increase the contact area of an inner layer and an outer layer, the two characteristics are beneficial to the combination of the outer layer, thirdly, the nano silicon dioxide can form hydrogen bonds with the polyvinyl alcohol inside the film, and the toughness of the polyvinyl alcohol film is enhanced. The hydroxyl of glycerol can form hydrogen bond with starch hydroxyl, and reduce starch rigidity, and glycerol also has moisture keeping effect.
When the first layer is dried to the moisture content of 50-60%, the film is completely shaped but has no rigidity, at the moment, the mixed solution is attached to the surface of the first layer, carbonate and bicarbonate can permeate below the surface of the first layer, and the carbonate and the bicarbonate are decomposed to form bubbles during drying, so that irregular holes are formed on the surface of the previously-formed layer, and the holes are formed after the holes are dried, so that the holes are combined and filled when the material of the outer layer structure is covered, the combination fastness of the inner layer structure and the outer layer structure is enhanced, and the formed capsule has a double-layer structure, is higher in strength and is greatly improved in friability index.
Further, as preferable:
the polyvinyl alcohol is used as a cheap and easily-obtained film-forming material and applied to capsules, so that the strength of the capsules can be improved, the cost of the capsules can be reduced, and sodium alginate, acrylic resin, chitosan and the like can be used for replacing the polyvinyl alcohol in a multilayer structure.
The hydroxypropyl starch is the main material of the capsule, and oxidized starch, hydroxyethyl starch, sodium carboxymethyl starch, pullulan and the like can be used as substitutes.
The bicarbonate is one or a mixture of sodium bicarbonate and potassium bicarbonate. The carbonate is one or mixture of sodium carbonate and potassium carbonate, and the two layers play a role in producing cavities, and other carbonates or bicarbonates can be used for achieving the same effect, such as calcium carbonate and calcium bicarbonate. More preferably, the mixed solution contains bicarbonate and carbonate at a mass ratio of 1.
The mixed solution also contains potassium chloride for promoting the gelation.
The hydroxypropyl starch layer is an outer layer, the polyvinyl alcohol layer is an inner layer, or the hydroxypropyl methyl starch layer is an inner layer, and the polyvinyl alcohol layer is an outer layer. When the inner layer is polyvinyl alcohol, the silicon dioxide can be used for manufacturing a structure with concave-convex surface, and the middle layer can be used for manufacturing a cavity and pore channel structure, so that the combination of the inner layer and the outer layer is facilitated.
When the hydroxypropyl starch layer is the inlayer, when the polyvinyl alcohol layer is outer, the cavity is made to the intermediate coat, but does not have silicon dioxide in the inlayer, the internal surface can not produce unevenness's surface, and dip in the glue again, silicon dioxide in the outer layer can not play the effect that increases area of contact, consequently, the inlayer is hydroxypropyl starch, the outer scheme that is polyvinyl alcohol, it is polyvinyl alcohol not to have the inlayer, the outer scheme that is hydroxypropyl starch is contact area between two-layer bigger, consequently two-layer combination can not be more firm than first scheme. Therefore, the best scheme is that polyvinyl alcohol is used as an inner layer and hydroxypropyl starch is used as an outer layer.
The thickness of the connecting layer is 3-20 μm.
Simultaneously, the application also provides a preparation method of the multilayer hollow capsule, which comprises the following steps:
(1) Preparing a hydroxypropyl starch glue solution: taking hydroxypropyl starch, carrageenan, potassium chloride, glycerol, citric acid and potassium sorbate according to a certain proportion, mixing with water, heating to 85-90 ℃ while stirring, and preserving heat for 1-3 hours to prepare hydroxypropyl starch glue solution;
(2) Preparing polyvinyl alcohol glue solution: taking polyvinyl alcohol, carrageenan, potassium chloride, silicon dioxide, citric acid and potassium sorbate according to a certain proportion, and dissolving in water to prepare polyvinyl alcohol glue solution;
(3) Preparing a mixed solution: taking carrageenin, carbonate and/or bicarbonate according to the proportion to obtain a mixed solution;
(4) Molding: dipping the hydroxypropyl starch glue solution obtained in the step (1), drying, attaching the mixed solution obtained in the step (3) to the surface of the formed membrane, drying, dipping the polyvinyl alcohol glue solution obtained in the step (2), and drying; or dipping the polyvinyl alcohol glue solution obtained in the step (2), drying, attaching the mixed solution obtained in the step (3) to the surface of the formed film, drying, dipping the hydroxypropyl starch glue solution obtained in the step (1), and drying.
Further, it is preferable that:
the drying temperature of the hydroxypropyl starch glue solution is 25-30 ℃, the drying temperature of the mixed solution is 55-85 ℃, and the drying temperature of the polyvinyl alcohol glue solution is 25-30 ℃.
The solid content of the hydroxypropyl starch glue solution is 20-30%, the solid content of the polyvinyl alcohol glue solution is 5-15%, and the content of the mixed solution is 2-10%.
The capsule has a two-layer structure, the glue is dipped twice, the mixed solution is added between the two layers, and the inner layer and the outer layer can be adjusted in an interchangeable way, and are respectively:
(1) The method comprises the following steps of dipping a polyvinyl alcohol (PVA) layer in glue for the first time, attaching a mixed solution of potassium bicarbonate, sodium carbonate, potassium carbonate and the like to the surface of the PVA layer after the PVA layer is dipped in the glue, enabling the surface of the PVA layer to be uniformly distributed, decomposing carbonate in the drying process, generating bubbles, enabling the surface to form cavities, forming cavities after the cavities are dried, facilitating the next layer of film substance to enter the cavities for combination, dipping a hydroxypropyl starch (HPS) layer, enabling the hydroxypropyl starch to enter the cavities formed on the surface of the PVA layer, and drying the mixture to form capsules.
(2) Dipping a glue hydroxypropyl starch layer for the first time, then attaching a mixed solution of potassium bicarbonate, sodium carbonate, potassium carbonate and the like on the surface of a hydroxypropyl starch film to ensure that the surface is uniformly distributed, forming cavities on the surface in the drying process, dipping polyvinyl alcohol after drying, and drying to form capsules.
The existence of the cavity and the pore canal ensures that the two layers are combined more tightly, is similar to a mortise and tenon structure and is beneficial to the combination between the hydroxypropyl starch and the polyvinyl alcohol layer.
Detailed Description
Example 1
96.3 parts of hydroxypropyl starch, 1.2 parts of carrageenan, 1.2 parts of potassium chloride, 1.2 parts of glycerol, 0.05 part of citric acid and 0.05 part of potassium sorbate are mixed with water according to the weight ratio, the solid content is 25 percent, the mixture is heated to 90 ℃ while stirring, and the temperature is kept for 2 hours.
82.7 parts of polyvinyl alcohol, 15 parts of carrageenan, 1.5 parts of potassium chloride, 0.5 part of silicon dioxide, 0.05 part of citric acid and 0.05 part of potassium sorbate are taken and dissolved in water to prepare a solution with the solid content of 8.0%.
55 parts of sodium bicarbonate, 34 parts of sodium carbonate, 10 parts of carrageenan and 1 part of potassium chloride are taken according to the weight proportion to prepare an aqueous solution with the solid content of 5 percent.
Controlling the temperature of polyvinyl alcohol glue solution to be 55 ℃, the room temperature to be 25 ℃, dipping a layer of PVA glue solution, drying for 0.5 hour at the temperature of 30 ℃ until the water content is 50 percent, attaching a layer of sodium carbonate/sodium bicarbonate with the attaching thickness of 10 microns on the surface of a polyvinyl alcohol film, heating to 60 ℃, drying for 0.5 hour, dipping a layer of hydroxypropyl starch glue solution after drying, shearing and coating glue, wherein the drying temperature is 30 ℃, and the drying time is 2 hours.
Example 2
96.3 parts of sodium carboxymethyl starch, 1.2 parts of carrageenan, 1.2 parts of potassium chloride, 1.2 parts of glycerol, 0.05 part of citric acid and 0.05 part of potassium sorbate are mixed with water according to the weight ratio, the solid content is 25 percent, the mixture is heated to 90 ℃ while being stirred, and the temperature is kept for 2 hours.
82.7 parts of sodium alginate, 15 parts of carrageenan, 1.5 parts of potassium chloride, 0.5 part of silicon dioxide, 0.05 part of citric acid and 0.05 part of potassium sorbate are taken and dissolved in water to prepare a solution with the solid content of 8.0%.
Taking 60 parts of potassium bicarbonate, 33 parts of potassium carbonate and 2 parts of carrageenan according to the weight ratio to prepare an aqueous solution with the solid content of 5%.
Controlling the temperature of sodium alginate glue solution to be 55 ℃, the room temperature to be 25 ℃, dipping a layer of PVA glue solution, drying for 0.5 hour at 30 ℃, drying until the water content is 55%, attaching a layer of potassium carbonate/potassium bicarbonate with the attaching thickness of 10 microns on the surface of a sodium alginate membrane, heating to 80 ℃, drying for 0.5 hour, dipping a layer of sodium carboxymethyl starch glue solution after drying, shearing and coating glue, wherein the drying temperature is 30 ℃, and the drying time is 2 hours.
Example 3
96.3 parts of hydroxyethyl starch, 1.2 parts of carrageenan, 1.2 parts of potassium chloride, 1.2 parts of glycerol, 0.05 part of citric acid and 0.05 part of potassium sorbate are mixed with water according to the weight ratio, the solid content is 25 percent, the mixture is heated to 90 ℃ while being stirred, and the temperature is kept for 2 hours.
82.7 parts of polyvinyl alcohol, 15 parts of carrageenan, 1.5 parts of potassium chloride, 0.5 part of silicon dioxide, 0.05 part of citric acid and 0.05 part of potassium sorbate are taken and dissolved in water to prepare a solution with the solid content of 8.0%.
Taking 60 parts of potassium bicarbonate, 33 parts of sodium carbonate and 3 parts of carrageenan by weight ratio to prepare an aqueous solution with the solid content of 5%.
Controlling the temperature of hydroxyethyl starch glue solution to be 55 ℃, keeping the room temperature at 25 ℃, dipping a layer of hydroxyethyl starch glue solution, drying for 1 hour at 25 ℃ until the water content is 60%, then attaching a layer of sodium carbonate/potassium bicarbonate with the attachment thickness of 10 microns on the surface of a hydroxyethyl starch film, heating to 60 ℃, drying for 0.5 hour, dipping a layer of polyvinyl alcohol glue solution after drying, shearing and coating glue, wherein the drying temperature is 30 ℃, and the drying time is 2 hours.
Example 4
Mixing 96.3 parts of pullulan polysaccharide, 1.2 parts of carrageenan, 1.2 parts of potassium chloride, 1.2 parts of glycerol, 0.05 part of citric acid and 0.05 part of potassium sorbate with water according to the weight ratio, stirring and heating to 90 ℃, and keeping the temperature for 2 hours, wherein the solid content is 25%.
82.7 parts of chitosan, 15 parts of carrageenan, 1.5 parts of potassium chloride, 0.5 part of silicon dioxide, 0.05 part of citric acid and 0.05 part of potassium sorbate are taken and dissolved in water to prepare a solution with the solid content of 8.0%.
Preparing an aqueous solution with the solid content of 5 percent by taking 98 parts of potassium bicarbonate and 2 parts of carrageenan according to the weight proportion.
Controlling the temperature of pullulan gum solution to be 55 ℃, the room temperature to be 25 ℃, dipping a layer of pullulan gum solution, drying for 0.5 hour at the temperature of 30 ℃ until the water content is 55 percent, then attaching a layer of potassium bicarbonate on the surface of the pullulan film, wherein the attaching thickness is 10 microns, heating to 60 ℃, drying for 0.2 hour, dipping a layer of chitosan gum solution after drying, shearing and coating, wherein the drying temperature is 30 ℃, and the drying time is 2 hours.
The performance tests were performed on the empty capsules of the different embodiments described above, and the results are summarized as follows:
table 1: capsule performance parameter comparison table under different preparation methods
The formulation of the comparative hydroxypropyl starch capsules was: 97 parts of hydroxypropyl starch, 2 parts of carrageenan and 1 part of potassium chloride, preparing a suspension with the content of 20%, dissolving in sol at 90 ℃, dipping in the sol at 40 ℃, and drying for 3 hours at 25-30 ℃.
As can be seen from the above table, the friability index of the comparative hydroxypropyl starch capsule does not meet the pharmacopeia requirements, while the embodiment has an effect of enhancing toughness through the multilayer structure in the capsule manufacturing process, and the friability index meets the requirements of the chinese pharmacopeia. Therefore, the invention has good application effect on improving the friability index of the capsule.
Compared with the other 3 examples, the 2-piece product in example 3 has the friability meeting the pharmacopoeia requirements, but is broken because the inner layer is hydroxyethyl starch, and silicon dioxide is not added into the hydroxyethyl starch, so that the specific surface area is small, the combined surface of the inner layer and the outer layer is reduced, and the friability index is not favorable.
In example 4, the inner layer is pullulan and the outer layer is chitosan, although no silica is added to the inner layer, the friability index is still good, mainly due to the generation of a cavity structure, so that the inner layer and the outer layer are tightly combined, and the pullulan and the chitosan have excellent performance. As is well known, the chitosan capsule has good film forming property and very high price of water-soluble chitosan, so the raw material cost of the chitosan capsule is very high, the pullulan is added into the inner layer of the capsule, the raw material cost of the capsule can be effectively reduced, and the cost can be reduced by 20 percent.
Claims (6)
1. A multilayer hollow capsule is characterized by comprising a polyvinyl alcohol layer and a hydroxypropyl starch layer, wherein a connecting layer is arranged between the polyvinyl alcohol layer and the hydroxypropyl starch layer, the hydroxypropyl starch layer is an outer layer, the polyvinyl alcohol layer is an inner layer, or the hydroxypropyl starch layer is an inner layer, the polyvinyl alcohol layer is an outer layer,
the polyvinyl alcohol layer is composed of the following components in parts by mass:
polyvinyl alcohol: 80-90,
carrageenin: 10-20,
potassium chloride: 1-5,
silicon dioxide: 0.1-1,
and (3) citric acid: 0.01-0.1,
potassium sorbate: 0.01-0.1;
the hydroxypropyl starch layer is composed of the following components in parts by mass:
hydroxypropyl starch: 75-96,
carrageenin: 1-5,
potassium chloride: 1-3,
glycerol: 1-3,
citric acid: 0.01-0.1,
potassium sorbate: 0.01-0.1;
the connecting layer is a cavity structure layer formed by drying a mixed solution on the surface of a corresponding layer, the mixed solution comprises 2-15 parts by mass of carrageenan, 75-98 parts by mass of carbonate and bicarbonate, the mass ratio of the carbonate to the bicarbonate is 1-2,
the forming process of each layer is as follows:
(1) Preparing a hydroxypropyl starch glue solution: taking hydroxypropyl starch, carrageenan, potassium chloride, glycerol, citric acid and potassium sorbate according to a certain proportion, mixing with water, heating to 85-90 ℃ while stirring, and preserving heat for 1-3 hours to prepare hydroxypropyl starch glue solution;
(2) Preparing polyvinyl alcohol glue solution: taking polyvinyl alcohol, carrageenan, potassium chloride, silicon dioxide, citric acid and potassium sorbate according to a certain proportion, and dissolving in water to prepare polyvinyl alcohol glue solution;
(3) Preparing a mixed solution: taking carrageenin, carbonate and bicarbonate according to a proportion to obtain a mixed aqueous solution;
(4) Molding: dipping the hydroxypropyl starch glue solution in the step (1), drying at 25-30 ℃ until the water content is 50-60%, attaching the mixed solution in the step (3) on the surface of the formed membrane, drying at 55-85 ℃, dipping the polyvinyl alcohol glue solution in the step (2), and drying at 25-30 ℃; or dipping the polyvinyl alcohol glue solution in the step (2), drying at 25-30 ℃ until the water content is 50-60%, attaching the mixed solution in the step (3), drying at 55-85 ℃, dipping the hydroxypropyl starch glue solution in the step (1), and drying at 25-30 ℃.
2. A multilayer empty capsule according to claim 1, wherein: the particle size of the silicon dioxide is 10-40nm, and the silicon dioxide is uniformly dispersed in a polyvinyl alcohol solution.
3. A multilayer empty capsule according to claim 1, wherein: the polyvinyl alcohol is replaced by any one of sodium alginate, acrylic resin and chitosan.
4. A multi-layered hollow capsule according to claim 1, wherein: the hydroxypropyl starch is replaced by any one of oxidized starch, hydroxyethyl starch, sodium carboxymethyl starch and pullulan.
5. A multi-layered hollow capsule according to claim 1, wherein: the bicarbonate is one or a mixture of sodium bicarbonate and potassium bicarbonate, and the carbonate is one or a mixture of sodium carbonate and potassium carbonate.
6. A multi-layered hollow capsule according to claim 1, wherein: the mixed solution also contains potassium chloride.
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