CN113116853A - Antibacterial and anti-pollution medicine capsule shell and preparation method thereof - Google Patents

Antibacterial and anti-pollution medicine capsule shell and preparation method thereof Download PDF

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CN113116853A
CN113116853A CN202110412658.3A CN202110412658A CN113116853A CN 113116853 A CN113116853 A CN 113116853A CN 202110412658 A CN202110412658 A CN 202110412658A CN 113116853 A CN113116853 A CN 113116853A
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capsule shell
antibacterial
solution
sodium alginate
stirring
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王光丰
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00Medicinal preparations characterised by special physical form
    • A61K9/48Preparations in capsules, e.g. of gelatin, of chocolate
    • A61K9/4816Wall or shell material
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61JCONTAINERS SPECIALLY ADAPTED FOR MEDICAL OR PHARMACEUTICAL PURPOSES; DEVICES OR METHODS SPECIALLY ADAPTED FOR BRINGING PHARMACEUTICAL PRODUCTS INTO PARTICULAR PHYSICAL OR ADMINISTERING FORMS; DEVICES FOR ADMINISTERING FOOD OR MEDICINES ORALLY; BABY COMFORTERS; DEVICES FOR RECEIVING SPITTLE
    • A61J3/00Devices or methods specially adapted for bringing pharmaceutical products into particular physical or administering forms
    • A61J3/07Devices or methods specially adapted for bringing pharmaceutical products into particular physical or administering forms into the form of capsules or similar small containers for oral use
    • A61J3/071Devices or methods specially adapted for bringing pharmaceutical products into particular physical or administering forms into the form of capsules or similar small containers for oral use into the form of telescopically engaged two-piece capsules
    • A61J3/077Manufacturing capsule shells
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K47/00Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/02Inorganic compounds
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K47/00Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/30Macromolecular organic or inorganic compounds, e.g. inorganic polyphosphates
    • A61K47/36Polysaccharides; Derivatives thereof, e.g. gums, starch, alginate, dextrin, hyaluronic acid, chitosan, inulin, agar or pectin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K47/00Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/30Macromolecular organic or inorganic compounds, e.g. inorganic polyphosphates
    • A61K47/36Polysaccharides; Derivatives thereof, e.g. gums, starch, alginate, dextrin, hyaluronic acid, chitosan, inulin, agar or pectin
    • A61K47/40Cyclodextrins; Derivatives thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00Medicinal preparations characterised by special physical form
    • A61K9/48Preparations in capsules, e.g. of gelatin, of chocolate
    • A61K9/4816Wall or shell material
    • A61K9/4825Proteins, e.g. gelatin

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  • Health & Medical Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Pharmacology & Pharmacy (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
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  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
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  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

The invention discloses an antibacterial and anti-pollution medicine capsule shell and a preparation method thereof, and relates to the technical field of new materials. The invention adopts an inner-outer double-layer structure to prepare a capsule shell for containing plant ash; when the outer layer of the capsule shell is prepared, calcium alginate oxide and beta-cyclodextrin are mixed to serve as a self-made cross-linking agent, gelatin and silver-loaded calcium alginate are cross-linked to prepare the calcium alginate composite membrane, so that the hardness of the capsule shell is increased, the capsule shell is not easy to move, and the heat resistance is good; the inner layer structure of the capsule shell is a calcium alginate composite protein aerogel structure, protein is added into the solution before the calcium alginate gel is dried and frozen, heating denaturation treatment is carried out, and freeze drying is carried out to prepare aerogel, so that the storage time of plant ash is prolonged. The antibacterial and anti-pollution medicine capsule shell prepared by the invention is convenient for the plant ash to be used as medicine while being antibacterial and anti-pollution.

Description

Antibacterial and anti-pollution medicine capsule shell and preparation method thereof
Technical Field
The invention relates to the field of new materials, in particular to an antibacterial and anti-pollution drug capsule shell and a preparation method thereof.
Background
At present, along with the development of traditional Chinese medicines, more and more traditional Chinese medicines are prepared into capsules, but because the water content of the traditional Chinese medicines is low, the water in the filled gelatin hollow capsules migrates into medicinal powder, the phenomena of easy friability and breakage of the capsules, column formation due to water loss of the medicinal powder, color change of the medicinal powder and the like occur, and although the plant capsules can meet the filling requirements of partial traditional Chinese medicines at present, the plant capsules are always limited to be used due to the characteristics of high price, difficulty in control of production and the like.
Aiming at plant ash in the traditional Chinese medicine, the traditional Chinese medicine is not only inconvenient to store in a humid environment and easy to influence the property of the medicine, but also influences the property of the traditional Chinese medicine by adding time when the traditional Chinese medicine is decocted. Therefore, the invention needs to research and develop a medicine capsule shell which can resist bacteria and pollution, prolong the storage time and adjust the adding time of plant ash.
Disclosure of Invention
The invention aims to provide an antibacterial and anti-pollution medicine capsule shell to solve the problems in the background technology.
In order to solve the above technical problem, a first aspect of the present invention provides the following technical solutions: an antibacterial and anti-pollution medicine capsule shell is characterized by comprising the following raw materials in parts by weight:
10-20 parts of capsule shell outer layer and 10-20 parts of capsule shell inner layer.
Preferably, the outer layer of the capsule shell is a calcium alginate composite membrane.
Preferably, the calcium alginate composite membrane is prepared by crosslinking gelatin and silver-loaded calcium alginate by using a self-made crosslinking agent.
Preferably, the self-made cross-linking agent is prepared by mixing calcium alginate oxide and beta-cyclodextrin.
Preferably, the inner layer of the capsule shell is aerogel prepared by sodium alginate composite protein.
The second aspect of the present invention provides: a preparation method of an antibacterial and anti-pollution medicine capsule shell is characterized by comprising the following steps:
the process flow is as follows:
preparing a self-made cross-linking agent, preparing an outer layer of a capsule shell, preparing an inner layer of the capsule shell and preparing the capsule shell.
Preferably, the method comprises the following specific steps:
(1) dispersing sodium alginate in an absolute ethyl alcohol solution, wherein the mass ratio of the sodium alginate to the absolute ethyl alcohol is 1: and 5, adding the mixture into an absolute ethanol solution in a volume ratio of 1: stirring 17g/mL potassium periodate aqueous solution of 1 for 4 hours in a dark place, adding 0.2-0.5 time of beta-cyclodextrin, stirring uniformly, adding ethylene glycol with the same molar quantity as the potassium periodate, and adding the reaction mixed solution into absolute ethyl alcohol with the volume 4 times that of the reaction mixed solution for suction filtration under the condition of vigorous stirring; dissolving the solid obtained by suction filtration with deionized water, adding 4 times of volume of absolute ethyl alcohol dissolved with the deionized water for suction filtration, and carrying out vacuum drying on the product obtained by suction filtration at 50-60 ℃ to prepare a self-made crosslinking agent;
(2) preparing 4% sodium alginate aqueous solution, and adding the mixture into the reactor according to the mass ratio of 1: 5, stirring uniformly, and standing for 24 hours to prepare a silver-loaded sodium alginate solution; mixing sodium alginate and gelatin in proportion, preparing 10% gelatin water solution, stirring at 45-55 ℃ until the gelatin water solution is completely dissolved, and mixing the 10% gelatin water solution and the silver-loaded sodium alginate solution according to the volume ratio of 1: 1, mixing, ultrasonically defoaming for 10 hours after uniformly stirring, adding a self-made crosslinking agent with the mass of 1/10 of gelatin into the mixture with the ultrasonic frequency of 30-60 kHz, stirring and reacting for 30-50 min, and adding the mixture with the gelatin aqueous solution in a volume ratio of 20: 1, stirring and reacting the 5% calcium oxide aqueous solution at 40-60 ℃ for 30-50 min to form a glue solution, immersing a stainless steel mold into the glue solution, then extracting the liquid surface, cooling and extruding the glue solution on the mold, and demolding and cutting after drying to obtain the outer layer of the capsule shell;
(3) dissolving sodium alginate in ultrapure water to prepare a 40% sodium alginate aqueous solution, stirring for 6-8 h by magnetic force, dropwise adding a 0.2mol/L calcium chloride solution which is 5 times of the volume of the sodium alginate aqueous solution, and after dropwise adding, adding the sodium alginate aqueous solution in a volume ratio of 10: 1, performing magnetic stirring on 70% protein aqueous solution, quickly heating to 80-100 ℃ after 1-2 h, preserving heat for 5-10 min to obtain calcium alginate composite protein hydrogel, transferring to a low-temperature refrigerator for pre-freezing at-80 ℃ for 4h, and quickly putting into a freeze dryer for vacuum drying to obtain a capsule shell inner layer;
(4) and (3) putting the inner layer of the capsule shell into the outer layer of the capsule shell, tightly adhering to the inner wall of the capsule shell, heating to 60-80 ℃, preserving heat for 2-4 min, and rapidly cooling to obtain a finished product.
Preferably, in the step (2): the mass ratio of sodium alginate to gelatin is 1: 4.
preferably, in the step (3): the freeze drying is carried out for 8-10 h under the conditions of-50 ℃ and 10 Pa.
Preferably, in the step (4): the cooling rate was 20 ℃/min.
Compared with the prior art, the invention has the following beneficial effects:
the outer layer of the capsule shell is a calcium alginate composite membrane, calcium alginate oxide and beta-cyclodextrin are mixed to be used as a self-made cross-linking agent, gelatin and silver-loaded calcium alginate are cross-linked to prepare the calcium alginate composite membrane, amino and carboxyl in the gelatin and hydroxyl and carboxylate radical in the calcium alginate form chemical bonds and hydrogen bonds under the action of static electricity, when a stable cross-network film is formed under the action of a cross-linking agent, the network structure not only has stronger heat resistance, but also locks cone-shaped beta-cyclodextrin molecules in the cross-network, and because of the randomness of positions and directions, the surface of the shell becomes uneven, the strength of the shell of the capsule is enhanced, the water absorbed at the tip part can not be transferred to the inside due to the existence of the cavity and is remained on the surface of the capsule shell to achieve the effect of weight increment, so that the weight of the capsule containing plant ash is increased and is not easy to move; when the heat-resistant capsule shell is used for boiling traditional Chinese medicines, the plant ash can be slowly released along with water entering the capsule only by changing small fire into big fire.
The inner layer structure of the capsule shell is a calcium alginate composite protein aerogel structure, protein is added into the solution before the calcium alginate gel is dried and frozen, heating denaturation treatment is carried out, and then freeze drying is carried out to prepare aerogel; the protein is denatured after heating, the spherical molecular structure is converted into the fibrous molecular structure, the protein exists in the water component in the calcium alginate gel, after freeze drying, the water is sublimated, the fibrous structure of the protein is left in the pore channels of the aerogel, the pores are reduced, the water is prevented from entering, and the storage time of the plant ash is prolonged.
When the capsule shell combines with the inner shell, the heating of short time is carried out, make outside and inside calcium alginate melting, solidify at rapid cooling, make the inseparable bonding of inner and outer shell together, make when decocting the traditional chinese medicine because the dissolution of capsule shell, the swelling of calcium alginate, the pore grow behind the swelling of inner shell aerogel calcium alginate, make moisture melt needs the certain time with plant ash by getting into capsule inside to outside, and then the time that plant ash got into the traditional chinese medicine when decocting the traditional chinese medicine has been prolonged, make things convenient for plant ash to go into the medicine more.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The first aspect of the invention provides the following technical scheme: an antibacterial and anti-pollution medicine capsule shell is characterized by comprising the following raw materials in parts by weight:
10-20 parts of capsule shell outer layer and 10-20 parts of capsule shell inner layer.
Preferably, the outer layer of the capsule shell is a calcium alginate composite membrane.
Preferably, the calcium alginate composite membrane is prepared by crosslinking gelatin and silver-loaded calcium alginate by using a self-made crosslinking agent.
Preferably, the self-made cross-linking agent is prepared by mixing calcium alginate oxide and beta-cyclodextrin.
Preferably, the inner layer of the capsule shell is aerogel prepared by sodium alginate composite protein.
The second aspect of the present invention provides: a preparation method of an antibacterial and anti-pollution medicine capsule shell is characterized by comprising the following steps:
the process flow is as follows:
preparing a self-made cross-linking agent, preparing an outer layer of a capsule shell, preparing an inner layer of the capsule shell and preparing the capsule shell.
Preferably, the method comprises the following specific steps:
(1) dispersing sodium alginate in an absolute ethyl alcohol solution, wherein the mass ratio of the sodium alginate to the absolute ethyl alcohol is 1: and 5, adding the mixture into an absolute ethanol solution in a volume ratio of 1: 1, stirring and reacting 17g/mL potassium periodate aqueous solution for 4 hours in a dark place, adding beta-cyclodextrin with the mass of 0.2-0.5 time that of sodium alginate, stirring uniformly, adding ethylene glycol with the same molar quantity as that of potassium periodate, and adding the reaction mixed solution into absolute ethyl alcohol with the volume of 4 times that of the reaction mixed solution for suction filtration under the condition of vigorous stirring; dissolving the solid obtained by suction filtration with deionized water, adding 4 times of volume of absolute ethyl alcohol dissolved with the deionized water for suction filtration, and carrying out vacuum drying on the product obtained by suction filtration at 50-60 ℃ to prepare a self-made crosslinking agent;
(2) preparing 4% sodium alginate aqueous solution, and adding the mixture into the reactor according to the mass ratio of 1: 5, stirring uniformly, and standing for 24 hours to prepare a silver-loaded sodium alginate solution; mixing sodium alginate and gelatin in proportion, preparing 10% gelatin water solution, stirring at 45-55 ℃ until the gelatin water solution is completely dissolved, and mixing the 10% gelatin water solution and the silver-loaded sodium alginate solution according to the volume ratio of 1: 1, mixing, ultrasonically defoaming for 10 hours after uniformly stirring, adding a self-made crosslinking agent with the mass of 1/10 of gelatin into the mixture with the ultrasonic frequency of 30-60 kHz, stirring and reacting for 30-50 min, and adding the mixture with the gelatin aqueous solution in a volume ratio of 20: 1, stirring and reacting the 5% calcium oxide aqueous solution at 40-60 ℃ for 30-50 min to form a glue solution, immersing a stainless steel mold into the glue solution, then extracting the liquid surface, cooling and extruding the glue solution on the mold, and demolding and cutting after drying to obtain the outer layer of the capsule shell;
(3) dissolving sodium alginate in ultrapure water to prepare a 40% sodium alginate aqueous solution, stirring for 6-8 h by magnetic force, dropwise adding a 0.2mol/L calcium chloride solution which is 5 times of the volume of the sodium alginate aqueous solution, and after dropwise adding, adding the sodium alginate aqueous solution in a volume ratio of 10: 1, performing magnetic stirring on 70% protein aqueous solution, quickly heating to 80-100 ℃ after 1-2 h, preserving heat for 5-10 min to obtain calcium alginate composite protein hydrogel, transferring to a low-temperature refrigerator for pre-freezing at-80 ℃ for 4h, and quickly putting into a freeze dryer for vacuum drying to obtain a capsule shell inner layer;
(4) and (3) putting the inner layer of the capsule shell into the outer layer of the capsule shell, tightly adhering to the inner wall of the capsule shell, heating to 60-80 ℃, preserving heat for 2-4 min, and rapidly cooling to obtain a finished product.
Preferably, in the step (2): the mass ratio of sodium alginate to gelatin is 1: 4.
preferably, in the step (3): the freeze drying is carried out for 8-10 h under the conditions of-50 ℃ and 10 Pa.
Preferably, in the step (4): the cooling rate was 20 ℃/min.
Example 1: the first antibacterial and anti-pollution medicine capsule shell:
an antibacterial and anti-pollution medicine capsule shell mainly comprises the following components in parts by weight:
10 parts of capsule shell outer layer and 10 parts of capsule shell inner layer.
The preparation method of the medicine capsule shell comprises the following steps:
(1) dispersing sodium alginate in an absolute ethyl alcohol solution, wherein the mass ratio of the sodium alginate to the absolute ethyl alcohol is 1: and 5, adding the mixture into an absolute ethanol solution in a volume ratio of 1: 1, stirring and reacting 17g/mL potassium periodate aqueous solution for 4 hours in a dark place, adding beta-cyclodextrin with the mass of 0.2 time that of sodium alginate, stirring uniformly, adding ethylene glycol with the same molar quantity as potassium periodate, and adding the reaction mixed solution into absolute ethyl alcohol with the volume of 4 times that of the reaction mixed solution for suction filtration under the condition of vigorous stirring; dissolving the solid obtained by suction filtration with deionized water, adding 4 times of anhydrous ethanol dissolved with the deionized water for suction filtration, and vacuum drying the product obtained by suction filtration at 50 ℃ to obtain a self-made crosslinking agent;
(2) preparing 4% sodium alginate aqueous solution, and adding the mixture into the reactor according to the mass ratio of 1: 5, stirring uniformly, and standing for 24 hours to prepare a silver-loaded sodium alginate solution; mixing sodium alginate and gelatin in proportion, preparing 10% gelatin water solution, stirring at 45 deg.C until completely dissolving, mixing 10% gelatin water solution and silver-loaded sodium alginate solution at volume ratio of 1: 1, mixing, ultrasonically defoaming for 10 hours after uniformly stirring, adding a self-made crosslinking agent with the mass of 1/10 of gelatin into the mixture with the ultrasonic frequency of 30kHz, stirring and reacting for 30min, and adding the mixture into a gelatin aqueous solution in a volume ratio of 20: 1, stirring and reacting at 40 ℃ for 30min to form a glue solution, immersing a stainless steel mold into the glue solution, then extracting the liquid surface, cooling and extruding the glue solution on the mold, and demolding and cutting after drying to obtain an outer layer of a capsule shell;
(3) dissolving sodium alginate in ultrapure water to prepare a 40% sodium alginate aqueous solution, stirring for 6 hours by magnetic force, dropwise adding a 0.2mol/L calcium chloride solution which is 5 times of the volume of the sodium alginate aqueous solution, and after dropwise adding, adding the sodium alginate aqueous solution in a volume ratio of 10: 1, rapidly heating to 80 ℃ after 1 hour, preserving heat for 5min to obtain calcium alginate composite protein hydrogel, transferring to a low-temperature refrigerator for pre-freezing at-80 ℃ for 4 hours, rapidly putting into a freeze dryer for vacuum drying, and performing vacuum drying at-50 ℃ and 10Pa for 8 hours to obtain an inner layer of a capsule shell;
(4) putting the inner layer of the capsule shell into the outer layer of the capsule shell, tightly adhering to the inner wall of the capsule shell, heating to 60 ℃, preserving heat for 2min, and rapidly cooling at a cooling rate of 20 ℃/min to obtain a finished product.
Example 2: and (2) antibacterial and anti-pollution medicine capsule shell II:
an antibacterial and anti-pollution medicine capsule shell mainly comprises the following components in parts by weight:
20 parts of capsule shell outer layer and 20 parts of capsule shell inner layer.
The preparation method of the medicine capsule shell comprises the following steps:
(1) dispersing sodium alginate in an absolute ethyl alcohol solution, wherein the mass ratio of the sodium alginate to the absolute ethyl alcohol is 1: and 5, adding the mixture into an absolute ethanol solution in a volume ratio of 1: 1, stirring and reacting 17g/mL potassium periodate aqueous solution for 4 hours in a dark place, adding beta-cyclodextrin with the mass of 0.4 time that of sodium alginate, stirring uniformly, adding ethylene glycol with the same molar quantity as potassium periodate, and adding the reaction mixed solution into absolute ethyl alcohol with the volume of 4 times that of the reaction mixed solution for suction filtration under the condition of vigorous stirring; dissolving the solid obtained by suction filtration with deionized water, adding 4 times of anhydrous ethanol dissolved with the deionized water for suction filtration, and vacuum drying the product obtained by suction filtration at 60 ℃ to obtain a self-made crosslinking agent;
(2) preparing 4% sodium alginate aqueous solution, and adding the mixture into the reactor according to the mass ratio of 1: 5, stirring uniformly, and standing for 24 hours to prepare a silver-loaded sodium alginate solution; mixing sodium alginate and gelatin in proportion, preparing 10% gelatin water solution, stirring at 55 deg.C until completely dissolving, mixing 10% gelatin water solution and silver-loaded sodium alginate solution at volume ratio of 1: 1, mixing, ultrasonically defoaming for 10 hours after uniformly stirring, adding a self-made crosslinking agent with the mass of 1/10 gelatin, stirring and reacting for 50min, and adding a crosslinking agent which is 20: 1, stirring and reacting at 60 ℃ for 50min to form a glue solution, immersing a stainless steel mold into the glue solution, then extracting the liquid surface, cooling and extruding the glue solution on the mold, and demolding and cutting after drying to obtain an outer layer of a capsule shell;
(3) dissolving sodium alginate in ultrapure water to prepare a 40% sodium alginate aqueous solution, stirring for 6 hours by magnetic force, dropwise adding a 0.2mol/L calcium chloride solution which is 5 times of the volume of the sodium alginate aqueous solution, and after dropwise adding, adding the sodium alginate aqueous solution in a volume ratio of 10: 1, performing magnetic stirring on 70% protein aqueous solution, quickly heating to 100 ℃ after 2 hours, preserving heat for 10 minutes to obtain calcium alginate composite protein hydrogel, transferring the calcium alginate composite protein hydrogel to a low-temperature refrigerator for pre-freezing at-80 ℃ for 4 hours, quickly putting the calcium alginate composite protein hydrogel into a freeze dryer for vacuum drying, wherein the freeze drying condition is vacuum drying at-50 ℃ and 10Pa for 8 hours to prepare a capsule shell inner layer;
(4) putting the inner layer of the capsule shell into the outer layer of the capsule shell, tightly adhering to the inner wall of the capsule shell, heating to 80 ℃, keeping the temperature for 4min, and rapidly cooling at a cooling rate of 20 ℃/min to obtain a finished product.
Comparative example 1
The formulation of comparative example 1 was the same as example 1. The preparation method of the antibacterial and anti-pollution medicine capsule shell is different from the preparation method of the example 1 only in the difference of the step (1), and the step (4) is modified as follows: dispersing sodium alginate in an absolute ethyl alcohol solution, wherein the mass ratio of the sodium alginate to the absolute ethyl alcohol is 1: and 5, adding the mixture into an absolute ethanol solution in a volume ratio of 1: 1, stirring and reacting the potassium periodate aqueous solution of 17g/mL in a dark place for 4 hours, adding ethylene glycol with the same molar weight as the potassium periodate, and adding the reaction mixed solution into absolute ethyl alcohol with the volume 4 times that of the reaction mixed solution for suction filtration under the condition of vigorous stirring; dissolving the solid obtained by suction filtration with deionized water, adding 4 times of anhydrous ethanol dissolved with the deionized water for suction filtration, and vacuum drying the product obtained by suction filtration at 60 ℃ to obtain a self-made crosslinking agent; the rest of the preparation steps are the same as example 1.
Comparative example 2
Comparative example 2 was formulated as in example 1. The preparation method of the antibacterial and anti-pollution medicine capsule shell is different from the example 1 only in the difference of the step (3), and the step (3) is modified as follows: dissolving sodium alginate in ultrapure water to prepare a 40% sodium alginate aqueous solution, magnetically stirring for 6 hours, and then dropwise adding a sodium alginate aqueous solution in a volume ratio of 1: 5, magnetically stirring the solution for 2 hours, quickly heating the solution to 100 ℃, preserving the temperature for 10 minutes to obtain calcium alginate composite protein hydrogel, transferring the calcium alginate composite protein hydrogel to a low-temperature refrigerator for prefreezing the hydrogel for 4 hours at-80 ℃, quickly putting the hydrogel into a freeze dryer for vacuum drying, and preparing the inner layer of the capsule shell by vacuum drying for 8 hours at-50 ℃ and 10 Pa; the rest of the preparation steps are the same as example 1.
Test example 1
1. Test method
Example 1 and comparative examples 1 and 2 are control tests, and 2g of plant ash is respectively put into the capsule shells prepared in example 1 and comparative examples 1 and 2, placed in the same humid environment, weighed before and after 7d, and compared.
2. Test results
Example 1 compares the plant ash retention capacity with comparative examples 1 and 2.
TABLE 1 weight (g)
Weight before 7d After 7d weight
Example 1 3.1 3.5
Comparative example 1 3.0 4.1
Comparative example 2 3.0 3.9
By comparing the weighing before and after 7d of the example 1 and the comparative examples 1 and 2, the result shows that the mass change of the medicine capsule shell 7d prepared in the example 1 is small, the capsule prepared in the example 1 absorbs less moisture, and the beta-cyclodextrin and the protein used in the preparation can prolong the storage time of the plant ash in the capsule to different degrees, which indicates that the antibacterial and anti-pollution medicine capsule shell prepared in the invention has the function of prolonging the storage time of the plant ash in a humid condition.
Test example 2
1. Test method
Example 1 and comparative example 1 are comparative tests, in which 2g of plant ash was placed in the capsule shells prepared in example 1 and comparative example 1, respectively, and heated in a transparent pot with water at 800W for 10min and then at 2100W for 10min, and the time of color change in the pot was recorded and compared.
2. Test results
Comparison of the release time of the plant ash controlled in example 1 and comparative example 2
TABLE 2 canister color change time (min)
Time to color change in 800W canister Time to color change in 2100W canister
Example 1 Color is not changed 2.6
Comparative example 2 3.4 -
By comparing the color change time of the medicine cans in the example 1 and the comparative example 1, it can be obviously found that the medicine capsule shell prepared in the example 1 has no color change at 800W, while the comparative example 1 has color change, which indicates that the plant ash in the medicine capsule shell prepared in the example 1 is not released, and indicates that the antibacterial and anti-pollution medicine capsule shell prepared in the invention can prolong the storage time of the plant ash under a humid condition and control the release of the plant ash.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (10)

1. An antibacterial and anti-pollution medicine capsule shell is characterized by comprising the following raw materials in parts by weight: 10-20 parts of capsule shell outer layer and 10-20 parts of capsule shell inner layer.
2. An antibacterial and antipollution pharmaceutical capsule shell according to claim 1, wherein: the outer layer of the capsule shell is a calcium alginate composite membrane.
3. An antibacterial and antipollution pharmaceutical capsule shell according to claim 2, characterized in that: the calcium alginate composite membrane is prepared by crosslinking gelatin and silver-loaded calcium alginate by using a self-made crosslinking agent.
4. An antibacterial and antipollution pharmaceutical capsule shell according to claim 3, characterized in that: the self-made cross-linking agent is prepared by mixing calcium alginate oxide and beta-cyclodextrin.
5. An antibacterial and antipollution pharmaceutical capsule shell according to claim 4, wherein: the inner layer of the capsule shell is aerogel prepared by sodium alginate composite protein.
6. The preparation method of the antibacterial and anti-pollution medicine capsule shell is characterized in that the process flow for preparing the antibacterial and anti-pollution medicine capsule shell is as follows: preparing a self-made cross-linking agent, preparing an outer layer of a capsule shell, preparing an inner layer of the capsule shell and preparing the capsule shell.
7. The method for preparing antibacterial and antipollution medicine capsule shells according to claim 6, characterized by comprising the following specific steps:
(1) dispersing sodium alginate in an absolute ethyl alcohol solution, wherein the mass ratio of the sodium alginate to the absolute ethyl alcohol is 1: and 5, adding the mixture into an absolute ethanol solution in a volume ratio of 1: stirring 17g/mL potassium periodate aqueous solution of 1 for 4 hours in a dark place, adding 0.2-0.5 time of beta-cyclodextrin, stirring uniformly, adding ethylene glycol with the same molar quantity as the potassium periodate, and adding the reaction mixed solution into absolute ethyl alcohol with the volume 4 times that of the reaction mixed solution for suction filtration under the condition of vigorous stirring; dissolving the solid obtained by suction filtration with deionized water, adding 4 times of volume of absolute ethyl alcohol dissolved with the deionized water for suction filtration, and carrying out vacuum drying on the product obtained by suction filtration at 50-60 ℃ to prepare a self-made crosslinking agent;
(2) preparing 4% sodium alginate aqueous solution, and adding the mixture into the reactor according to the mass ratio of 1: 5, stirring uniformly, and standing for 24 hours to prepare a silver-loaded sodium alginate solution; mixing sodium alginate and gelatin in proportion, preparing 10% gelatin water solution, stirring at 45-55 ℃ until the gelatin water solution is completely dissolved, and mixing the 10% gelatin water solution and the silver-loaded sodium alginate solution according to the volume ratio of 1: 1, mixing, ultrasonically defoaming for 10 hours after uniformly stirring, adding a self-made crosslinking agent with the mass of 1/10 of gelatin into the mixture with the ultrasonic frequency of 30-60 kHz, stirring and reacting for 30-50 min, and adding the mixture with the gelatin aqueous solution in a volume ratio of 20: 1, stirring and reacting the 5% calcium oxide aqueous solution at 40-60 ℃ for 30-50 min to form a glue solution, immersing a stainless steel mold into the glue solution, then extracting the liquid surface, cooling and extruding the glue solution on the mold, and demolding and cutting after drying to obtain the outer layer of the capsule shell;
(3) dissolving sodium alginate in ultrapure water to prepare a 40% sodium alginate aqueous solution, stirring for 6-8 h by magnetic force, dropwise adding a 0.2mol/L calcium chloride solution which is 5 times of the volume of the sodium alginate aqueous solution, and after dropwise adding, adding the sodium alginate aqueous solution in a volume ratio of 10: 1, performing magnetic stirring on 70% protein aqueous solution, quickly heating to 80-100 ℃ after 1-2 h, preserving heat for 5-10 min to obtain calcium alginate composite protein hydrogel, transferring to a low-temperature refrigerator for pre-freezing at-80 ℃ for 4h, and quickly putting into a freeze dryer for vacuum drying to obtain a capsule shell inner layer;
(4) and (3) putting the inner layer of the capsule shell into the outer layer of the capsule shell, tightly adhering to the inner wall of the capsule shell, heating to 60-80 ℃, preserving heat for 2-4 min, and rapidly cooling to obtain a finished product.
8. The process for preparing an antibacterial and antipollution pharmaceutical capsule shell according to claim 7, wherein: in the step (2): the mass ratio of sodium alginate to gelatin is 1: 4.
9. the process for preparing antibacterial and antipollution pharmaceutical capsule shells according to claim 7, wherein in the step (3): the freeze drying is carried out for 8-10 h under the conditions of-50 ℃ and 10 Pa.
10. The process for preparing antibacterial and antipollution pharmaceutical capsule shells according to claim 7, wherein in the step (4): the cooling rate was 20 ℃/min.
CN202110412658.3A 2021-04-16 2021-04-16 Antibacterial and anti-pollution medicine capsule shell and preparation method thereof Pending CN113116853A (en)

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CN104548187A (en) * 2014-12-24 2015-04-29 青岛明月生物医用材料有限公司 Modified alginic acid and gelatin blended sponge as well as preparing method and application thereof
CN105533610A (en) * 2015-12-18 2016-05-04 湖南尔康制药股份有限公司 Spice capsule
CN108816161A (en) * 2018-06-11 2018-11-16 佛山皖阳生物科技有限公司 A kind of preparation method being retained anti-oxidant starch base capsule

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CN104548187A (en) * 2014-12-24 2015-04-29 青岛明月生物医用材料有限公司 Modified alginic acid and gelatin blended sponge as well as preparing method and application thereof
CN105533610A (en) * 2015-12-18 2016-05-04 湖南尔康制药股份有限公司 Spice capsule
CN108816161A (en) * 2018-06-11 2018-11-16 佛山皖阳生物科技有限公司 A kind of preparation method being retained anti-oxidant starch base capsule

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