WO2003094893A1 - Process for preparing an injection type solid chitosan powder - Google Patents

Process for preparing an injection type solid chitosan powder Download PDF

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Publication number
WO2003094893A1
WO2003094893A1 PCT/KR2003/000911 KR0300911W WO03094893A1 WO 2003094893 A1 WO2003094893 A1 WO 2003094893A1 KR 0300911 W KR0300911 W KR 0300911W WO 03094893 A1 WO03094893 A1 WO 03094893A1
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Prior art keywords
chitosan
powder
chitosan powder
solid
solution
Prior art date
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PCT/KR2003/000911
Other languages
French (fr)
Inventor
Hee-Young Lee
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Hee-Young Lee
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Publication of WO2003094893A1 publication Critical patent/WO2003094893A1/en

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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/14—Macromolecular materials
    • A61L27/20—Polysaccharides
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
    • A61L27/56—Porous materials, e.g. foams or sponges
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61M—DEVICES FOR INTRODUCING MEDIA INTO, OR ONTO, THE BODY; DEVICES FOR TRANSDUCING BODY MEDIA OR FOR TAKING MEDIA FROM THE BODY; DEVICES FOR PRODUCING OR ENDING SLEEP OR STUPOR
    • A61M5/00—Devices for bringing media into the body in a subcutaneous, intra-vascular or intramuscular way; Accessories therefor, e.g. filling or cleaning devices, arm-rests
    • A61M5/178—Syringes
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L5/00—Compositions of polysaccharides or of their derivatives not provided for in groups C08L1/00 or C08L3/00
    • C08L5/08—Chitin; Chondroitin sulfate; Hyaluronic acid; Derivatives thereof
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61M—DEVICES FOR INTRODUCING MEDIA INTO, OR ONTO, THE BODY; DEVICES FOR TRANSDUCING BODY MEDIA OR FOR TAKING MEDIA FROM THE BODY; DEVICES FOR PRODUCING OR ENDING SLEEP OR STUPOR
    • A61M5/00—Devices for bringing media into the body in a subcutaneous, intra-vascular or intramuscular way; Accessories therefor, e.g. filling or cleaning devices, arm-rests
    • A61M5/178—Syringes
    • A61M5/31—Details
    • A61M2005/3123—Details having air entrapping or venting means, e.g. purging channels in pistons
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00—Applications
    • C08L2203/02—Applications for biomedical use

Definitions

  • the present invention relates to a process for producing an injectable solid chitosan powder which can substitute human soft tissues.
  • Korean Patent Laid-Open No. 10-2002-0012004 discloses a solid chitosan capable of being used as an injection for replacing the human soft tissues and a process for producing the solid chitosan.
  • the solid chitosan can be used as an injectable material for filling the volume of soft tissues, like a bag used in augmentation mammoplasty.
  • the solid chitosan has a sponge structure.
  • the process for producing the solid chitosan is carried out by any one of the following processes ⁇ a vacuum expansion process including heating a chitosan powder to form a high-pressure state, and depressurizing for a short time to form fine air bubbles inside the chitosan particles!
  • a spray scatter-lyophilization process including mixing chitosan particles and distilled water, rapidly cooling while spraying the mixture using a sprayer, and freeze-drying the cooled mixture; and an ultrasonic scatter-lyophilization process including mixing chitosan particles and distilled water, rapidly cooling while ultrasonically vibrating to scatter the tnixture, and freeze-drying the cooled mixture.
  • the solid chitosan has a particle size of 50 ⁇ 250 ⁇ m sufficient to pass through a syringe needle. However, the size of the solid chitosan is too large to be ingested by macrophages. In addition, the solid chitosan having this size range can form fine air bubbles inside the chitosan particles. The fine air bubbles provide spaces for cell growth within the chitosan particles, thereby substituting human soft tissues.
  • the solid chitosan can be produced by the vacuum expansion process, the spray scatter-lyophilization process and the ultrasonic scatter- lyophilization process as discussed above.
  • the above processes are characterized by including vacuum expanding a chitosan powder or spraying a solution of the chitosan powder in distilled water.
  • the chitosan powder is obtained by grinding a lump of chitosan to a particle size of 25-41 ⁇ m.
  • the lyophilization step is carried out to form fine air bubbles inside the chitosan particles.
  • the present invention has been made in view of the above problems of the conventional processes for producing a chitosan powder, and it is an object of the present invention to provide a process for producing an injectable solid chitosan powder in which the screening of chitosan particles is possible, the quality of the solid chitosan powder is uniform, unnecessary steps are eliminated and mass -production of the chitosan powder is possible.
  • a process for producing an injectable solid chitosan powder which comprises the steps of freezing an aqueous chitosan solution, lyophilizing and screening, the solid chitosan powder having a particle size of 250 ⁇ m or smaller and having fine air bubbles formed inside the chitosan particles.
  • the solid chitosan powder can be used as an injectable material for filling the volume of soft tissues, such as injection, cell culture and bags for breast augmentation.
  • the solid chitosan powder is produced by purifying and neutralizing an aqueous chitosan solution and powdering the aqueous chitosan solution to form air bubbles inside the chitosan particles and screening the chitosan particles having a particle size of 250 ⁇ m or less.
  • aqueous chitosan solution is obtained in accordance with a known process.
  • the aqueous chitosan solution is obtained by dissolving a lump of chitosan in acetic acid, adding caustic soda to the chitosan solution, and purifying and completely neutralizing the mixture.
  • any one of the following processes is used: a process including freezing an aqueous chitosan solution, grinding the frozen chitosan solution, and lyophilizing the grinded chitosan solution; a process including freezing an aqueous chitosan solution, lyophilizing the chitosan solution to form a lump of chitosan with a sponge structure, and grinding the lump of chitosan into fine particles; a process including scattering an aqueous chitosan solution to make a mist form using an ultrasonic vibrator, cooling the chitosan mist to obtain ice powder of chitosan, and lyophilizing the ice powder of chitosan; and a process including scattering an aqueous chitosan solution using an ultrasonic vibrator or a sprayer, dipping the scattered chitosan in isopropyl
  • the screening of the chitosan powder is carried out to obtain chitosan powder having a particle size of 20-250 ⁇ m with fine air bubbles formed therein.
  • the chitosan powder is passed through a dual filter.
  • the dual filter consists of a pair of a large filter and a small filter spaced each other.
  • the chitosan powder having a particle size exceeding 250 ⁇ m cannot pass through the large filter, and the chitosan powder having a particle size exceeding 20 ⁇ m cannot pass through the small filter.
  • the chitosan powder is shot toward the large filter and the small filter or the two filters are vibrated, the chitosan powder remaining in a space between the two filters is collected.
  • the collected chitosan powder has a particle size of 20 ⁇ 250 ⁇ m.
  • the screening step is carried out to satisfy the size requirements of the chitosan powder according to the present invention. Specifically, the screening step may be carried out before or after the lyophilization step, depending on the powdering processes.
  • the present invention suggests various processes for producing an injectable solid chitosan powder. These processes of the present invention can be selected depending on the used chitosan powder production equipments and production conditions. In particular, automated processes allow the solid chitosan powder to be mass-produced with uniform quality, which is economically advantageous.
  • a 'purified solid chitosan was added to a mixture of acetic acid and caustic soda to prepare an aqueous chitosan solution.
  • the aqueous chitosan solution was frozen to obtain an ice lump of chitosan at a temperature below 0 °C .
  • the ice lump of chitosan was grinded into fine particles using an abraser (or miller). After the fine particles of chitosan were passed through a dual filter to screen fine particles having a particle size of 20 ⁇ 250 ⁇ m, the screened fine particles were lyophilized to produce a chitosan powder.
  • the apparent size of the chitosan powder thus produced was determined during grinding into fine particles, and the structure of the chitosan powder was determined during lyophilizing. That is, fine air bubbles were formed inside the solid chitosan powder from which water was escaped during lyophilizing, thereby achieving a sponge structure of the solid chitosan powder.
  • the size of the fine air bubbles can be controlled by lyophilization temperature. In this Example, the fine air bubbles had a size of 10-50 ⁇ m,
  • a purified and neutralized aqueous chitosan solution was frozen to obtain an ice lump of chitosan at a temperature below 0°C.
  • the ice lump of chitosan was grinded into fine particles using an abraser (or miller). After the fine particles were lyophilized to produce a crude solid chitosan powder, the crude solid chitosan powder was passed through a dual filter to screen a solid chitosan powder having a particle size of 20-250 ⁇ m.
  • Example 3 The process of this Example was carried out in the same manner as in Example 1, except that lyophilizing was carried out prior to screening.
  • a purified and neutralized aqueous chitosan solution was frozen to obtain an ice lump of chitosan at a temperature below 0°C.
  • the ice lump of chitosan was lyophilized to prepare a sponge-structured chitosan lump, and grinded into fine particles using an abraser (or miller).
  • the fine particles were passed through a dual filter to screen a solid chitosan powder having a particle size of 20-250 ⁇ m.
  • the process of this Example is advantageous in terms of its simplicity. That is, the solid chitosan powder is produced by lyophilizing an ice lump of chitosan, followed by grinding and screening. However, the process has a disadvantage of a relatively long lyophilization time.
  • the solid chitosan powder produced in this Example can be usefully utilized in a variety of medicinal applications, e.g., cell culture, using crude chitosan powder.
  • the spray of the aqueous chitosan solution and nitrogen gas was carried out using an ultrasonic vibrator or sprayer.
  • the sprayed aqueous chitosan solution with nitrogen gas was diffused and condensed to form a crystal structure such as a snow crystal, and contacted with an isopropyl alcohol solution.
  • the isopropyl alcohol solution having a low melting point acts on freezing chitosan particles, instead of dissolving them, the chitosan particles are deposited in a frozen state. Specifically, the fine chitosan particles can be frozen and deposited while maintaining the isopropyl alcohol solution at a temperature of -70 .
  • the deposited chitosan particles have higher specific gravity than the isopropyl alcohol solution, they are deposited at the bottom.
  • the deposited chitosan particles were collected in the form of ice powder.
  • the solid chitosan powders of Examples 1 to 3 containing fine air bubbles therein and the solid chitosan powder of Example 4 having a crystal structure consisting of fine frames and branching pods can provide gaps (voids) between the solid chitosan particles when formulated into an injection by kneading.
  • the gaps act as spaces where cells can grow and human tissues are generated.

Abstract

Disclosed herein is a process for producing an injectable solid chitosan powder which can substitute human soft tissues. The process is carried out by any one of the following processes: a process including freezing an aqueous chitosan solution, grinding the frozen chitosan solution, and lyophilizing the grinded chitosan solution; a process including freezing an aqueous chitosan solution, lyophilizing the chitosan solution to form a lump of chitosan with a sponge structure, and grinding the lump of chitosan into fine particles; a process including scattering an aqueous chitosan solution to make a mist form using an ultrasonic vibrator, cooling the chitosan mist to obtain ice powder of chitosan, and lyophilizing the ice powder of chitosan; and a process including scattering an aqueous chitosan solution using an ultrasonic vibrator or a sprayer, dipping the scattered chitosan in isopropyl alcohol at low temperature to obtain chitosan precipitates, and lyophilizing the chitosan precipitates.

Description

DESCRIPTION
Title of the Invention Process for preparing an injection type solid chitosan powder
Fields of the Invention
The present invention relates to a process for producing an injectable solid chitosan powder which can substitute human soft tissues.
Background Art
Korean Patent Laid-Open No. 10-2002-0012004 discloses a solid chitosan capable of being used as an injection for replacing the human soft tissues and a process for producing the solid chitosan.
According to this patent publication, the solid chitosan can be used as an injectable material for filling the volume of soft tissues, like a bag used in augmentation mammoplasty. In addition, the solid chitosan has a sponge structure. The process for producing the solid chitosan is carried out by any one of the following processes^ a vacuum expansion process including heating a chitosan powder to form a high-pressure state, and depressurizing for a short time to form fine air bubbles inside the chitosan particles! a spray scatter-lyophilization process including mixing chitosan particles and distilled water, rapidly cooling while spraying the mixture using a sprayer, and freeze-drying the cooled mixture; and an ultrasonic scatter-lyophilization process including mixing chitosan particles and distilled water, rapidly cooling while ultrasonically vibrating to scatter the tnixture, and freeze-drying the cooled mixture.
The solid chitosan has a particle size of 50~250μm sufficient to pass through a syringe needle. However, the size of the solid chitosan is too large to be ingested by macrophages. In addition, the solid chitosan having this size range can form fine air bubbles inside the chitosan particles. The fine air bubbles provide spaces for cell growth within the chitosan particles, thereby substituting human soft tissues. The solid chitosan can be produced by the vacuum expansion process, the spray scatter-lyophilization process and the ultrasonic scatter- lyophilization process as discussed above.
The above processes are characterized by including vacuum expanding a chitosan powder or spraying a solution of the chitosan powder in distilled water. The chitosan powder is obtained by grinding a lump of chitosan to a particle size of 25-41μm. The lyophilization step is carried out to form fine air bubbles inside the chitosan particles. These processes have an advantage that the vacuum expanding or spraying step and lyophilizing step require simple equipments. However, they have problems that each step is separately carried out and thus mass -production of the chitosan powder is limited.
Detailed Description of the Invention
Therefore, the present invention has been made in view of the above problems of the conventional processes for producing a chitosan powder, and it is an object of the present invention to provide a process for producing an injectable solid chitosan powder in which the screening of chitosan particles is possible, the quality of the solid chitosan powder is uniform, unnecessary steps are eliminated and mass -production of the chitosan powder is possible.
In order to accomplish the above object of the present invention, there is provided a process for producing an injectable solid chitosan powder which comprises the steps of freezing an aqueous chitosan solution, lyophilizing and screening, the solid chitosan powder having a particle size of 250μm or smaller and having fine air bubbles formed inside the chitosan particles.
The solid chitosan powder can be used as an injectable material for filling the volume of soft tissues, such as injection, cell culture and bags for breast augmentation.
Specifically, the solid chitosan powder is produced by purifying and neutralizing an aqueous chitosan solution and powdering the aqueous chitosan solution to form air bubbles inside the chitosan particles and screening the chitosan particles having a particle size of 250μm or less.
Said aqueous chitosan solution is obtained in accordance with a known process. The aqueous chitosan solution is obtained by dissolving a lump of chitosan in acetic acid, adding caustic soda to the chitosan solution, and purifying and completely neutralizing the mixture. In order to powder the aqueous chitosan solution to form air bubbles inside the chitosan particles, any one of the following processes is used: a process including freezing an aqueous chitosan solution, grinding the frozen chitosan solution, and lyophilizing the grinded chitosan solution; a process including freezing an aqueous chitosan solution, lyophilizing the chitosan solution to form a lump of chitosan with a sponge structure, and grinding the lump of chitosan into fine particles; a process including scattering an aqueous chitosan solution to make a mist form using an ultrasonic vibrator, cooling the chitosan mist to obtain ice powder of chitosan, and lyophilizing the ice powder of chitosan; and a process including scattering an aqueous chitosan solution using an ultrasonic vibrator or a sprayer, dipping the scattered chitosan in isopropyl alcohol at low temperature to obtain chitosan precipitates, and lyophilizing the chitosan precipitates.
The screening of the chitosan powder is carried out to obtain chitosan powder having a particle size of 20-250μm with fine air bubbles formed therein. Specifically, the chitosan powder is passed through a dual filter. The dual filter consists of a pair of a large filter and a small filter spaced each other. The chitosan powder having a particle size exceeding 250μm cannot pass through the large filter, and the chitosan powder having a particle size exceeding 20μm cannot pass through the small filter. After the chitosan powder is shot toward the large filter and the small filter or the two filters are vibrated, the chitosan powder remaining in a space between the two filters is collected. The collected chitosan powder has a particle size of 20~250μm.
Since macrophages can ingest particles having a size smaller than about 50μm, some of the chitosan articles may be ingested. However, since the chitosan powder having a particle size smaller than 50μm is mixed with chitosan powder having a particle size exceeding 50μm, there is a low possibility that macrophages can ingest the chitosan powder having a particle size smaller than 50μm. This screening step has an advantage in terms of high production throughput.
The screening step is carried out to satisfy the size requirements of the chitosan powder according to the present invention. Specifically, the screening step may be carried out before or after the lyophilization step, depending on the powdering processes. The present invention suggests various processes for producing an injectable solid chitosan powder. These processes of the present invention can be selected depending on the used chitosan powder production equipments and production conditions. In particular, automated processes allow the solid chitosan powder to be mass-produced with uniform quality, which is economically advantageous.
Best Mode for carrying out the Invention
Hereinafter, the present invention will be described in more detail with reference to the following Examples.
Example 1
First, a 'purified solid chitosan was added to a mixture of acetic acid and caustic soda to prepare an aqueous chitosan solution. The aqueous chitosan solution was frozen to obtain an ice lump of chitosan at a temperature below 0 °C . The ice lump of chitosan was grinded into fine particles using an abraser (or miller). After the fine particles of chitosan were passed through a dual filter to screen fine particles having a particle size of 20~250μm, the screened fine particles were lyophilized to produce a chitosan powder.
The apparent size of the chitosan powder thus produced was determined during grinding into fine particles, and the structure of the chitosan powder was determined during lyophilizing. That is, fine air bubbles were formed inside the solid chitosan powder from which water was escaped during lyophilizing, thereby achieving a sponge structure of the solid chitosan powder. The size of the fine air bubbles can be controlled by lyophilization temperature. In this Example, the fine air bubbles had a size of 10-50μm,
Since the process of this Example uses an aqueous chitosan solution and a series of steps consisting of preparation of an ice lump of chitosan, grinding, screening and lyophilization is continuously carried out, mass -production of chitosan powder is possible and the size of the chitosan powder can be easily controlled. In addition, since the process uses an ice lump of chitosan which can be easily grinded, a solid chitosan powder with uniform quality can be produced.
Example 2
First, a purified and neutralized aqueous chitosan solution was frozen to obtain an ice lump of chitosan at a temperature below 0°C. The ice lump of chitosan was grinded into fine particles using an abraser (or miller). After the fine particles were lyophilized to produce a crude solid chitosan powder, the crude solid chitosan powder was passed through a dual filter to screen a solid chitosan powder having a particle size of 20-250μm.
The process of this Example was carried out in the same manner as in Example 1, except that lyophilizing was carried out prior to screening. Example 3
First, a purified and neutralized aqueous chitosan solution was frozen to obtain an ice lump of chitosan at a temperature below 0°C. The ice lump of chitosan was lyophilized to prepare a sponge-structured chitosan lump, and grinded into fine particles using an abraser (or miller). The fine particles were passed through a dual filter to screen a solid chitosan powder having a particle size of 20-250μm.
The process of this Example is advantageous in terms of its simplicity. That is, the solid chitosan powder is produced by lyophilizing an ice lump of chitosan, followed by grinding and screening. However, the process has a disadvantage of a relatively long lyophilization time. The solid chitosan powder produced in this Example can be usefully utilized in a variety of medicinal applications, e.g., cell culture, using crude chitosan powder.
Example 4
First, after a purified and neutralized aqueous chitosan solution was sprayed using nitrogen gas to contact an isopropyl alcohol solution, fine precipitates in the form of ice were obtained. The fine precipitates were separated and then lyophilized. The lyophilized chitosan powder was passed through a dual filter to screen a solid chitosan powder having a particle size of 20-250μm.
The spray of the aqueous chitosan solution and nitrogen gas was carried out using an ultrasonic vibrator or sprayer. The sprayed aqueous chitosan solution with nitrogen gas was diffused and condensed to form a crystal structure such as a snow crystal, and contacted with an isopropyl alcohol solution.
Since the isopropyl alcohol solution having a low melting point acts on freezing chitosan particles, instead of dissolving them, the chitosan particles are deposited in a frozen state. Specifically, the fine chitosan particles can be frozen and deposited while maintaining the isopropyl alcohol solution at a temperature of -70 .
Since the deposited chitosan particles have higher specific gravity than the isopropyl alcohol solution, they are deposited at the bottom. In this Example, the deposited chitosan particles were collected in the form of ice powder.
When the frozen chitosan powder was lyophilized, water which assumes the form of ice contained in the powder was sublimed in the form of water vapor to form many fine air bubbles inside the chitosan particles. The outside of the chitosan particles was crystallized to form a crystal structure consisting of fine frames and branching pods.
Accordingly, the solid chitosan powders of Examples 1 to 3 containing fine air bubbles therein and the solid chitosan powder of Example 4 having a crystal structure consisting of fine frames and branching pods, can provide gaps (voids) between the solid chitosan particles when formulated into an injection by kneading. The gaps act as spaces where cells can grow and human tissues are generated.
Although the preferred embodiments of the present invention have been disclosed for illustrative purposes, those skilled in the art will appreciate that various modifications, additions and substitutions are possible, without departing from the scope and spirit of the invention as disclosed in the accompanying claims.

Claims

WHAT IS CLAIMED IS:
1. A process for producing an injectable solid chitosan powder which can be used as an injectable material for filling the volume of soft tissues, such as injection bags, cell culture bags and bags for breast augmentation, comprising the steps of: powdering a purified and neutralized aqueous chitosan solution to form fine air bubbles inside the chitosan powder; and screening the chitosan powder, wherein the solid chitosan powder has a particle size of 250μm or smaller, and fine air bubbles are formed therein.
2. The process for producing an injectable solid chitosan powder according to claim 1, wherein the powdering and screening steps include the sub-steps of freezing an aqueous chitosan solution at a temperature below 0°C to obtain an ice lump of chitosan, grinding the ice lump of chitosan into fine particles using an abraser (or miller), passing the fine particles of chitosan through a dual filter to screen fine particles having a particle size of 20~250μm, and lyophilizing the screened fine particles to produce a chitosan powder.
3. The process for producing an injectable solid chitosan powder according to claim 1, wherein the powdering and screening steps include the sub-steps of freezing an aqueous chitosan solution at a temperature below 0°C to obtain an ice lump of chitosan, grinding the ice lump of chitosan into fine particles using an abraser (or miller), lyophilizing the fine particles to produce a crude solid chitosan powder, and passing the crude solid chitosan powder through a dual filter to screen a solid chitosan powder having a particle size of 20~250μm.
4. The process for producing an injectable solid chitosan powder according to claim 1, wherein the powdering and screening steps include the sub-steps of freezing an aqueous chitosan solution at a temperature below 0C to obtain an ice lump of chitosan, lyophilizing the ice lump of chitosan to prepare a sponge- structured chitosan lump, grinding the sponge-structured chitosan lump into fine particles using an abraser (or miller), and passing the fine particles through a dual filter to screen a solid chitosan powder having a particle size of 20-250μm.
5. The process for producing an injectable solid chitosan powder according to claim 1, wherein the powdering and screening steps include the sub-steps of diffuse-spraying a mixture of an aqueous chitosan solution and nitrogen gas to bring the mixture into contact with an isopropyl alcohol solution thereby obtaining fine precipitates in the form of ice, separating and lyophilizing the fine precipitates to form a crystal structure consisting of fine frames and branching pods, and passing the crystal-structured chitosan through a dual filter to screen a solid chitosan powder having a particle size of 20~250μm.
PCT/KR2003/000911 2002-05-08 2003-05-07 Process for preparing an injection type solid chitosan powder WO2003094893A1 (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2867073A1 (en) * 2004-03-08 2005-09-09 Europlak Use of a chitosane thread for the preparation of a device, which is implanted under the skin for a cosmetic use to modify the appearance of an individual

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JPH01152104A (en) * 1987-12-08 1989-06-14 Hokkaido Soda Kk Preparation of water-soluble chitosan salt powder
WO1990013780A1 (en) * 1989-05-01 1990-11-15 Enzytech, Inc. Very low temperature casting of controlled release microspheres
JPH0747113A (en) * 1993-08-06 1995-02-21 San Five Kk Therapeutic agent
WO2000016817A1 (en) * 1998-09-24 2000-03-30 Korea Atomic Energy Research Institute Dermal scaffold using neutralized chitosan sponge or neutralized chitosan/collagen mixed sponge
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Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6390507A (en) * 1986-10-03 1988-04-21 Unitika Ltd Chitosan sponge
JPH01152104A (en) * 1987-12-08 1989-06-14 Hokkaido Soda Kk Preparation of water-soluble chitosan salt powder
WO1990013780A1 (en) * 1989-05-01 1990-11-15 Enzytech, Inc. Very low temperature casting of controlled release microspheres
JPH0747113A (en) * 1993-08-06 1995-02-21 San Five Kk Therapeutic agent
US6206930B1 (en) * 1998-08-10 2001-03-27 Charlotte-Mecklenburg Hospital Authority Absorbable tissue expander
WO2000016817A1 (en) * 1998-09-24 2000-03-30 Korea Atomic Energy Research Institute Dermal scaffold using neutralized chitosan sponge or neutralized chitosan/collagen mixed sponge

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2867073A1 (en) * 2004-03-08 2005-09-09 Europlak Use of a chitosane thread for the preparation of a device, which is implanted under the skin for a cosmetic use to modify the appearance of an individual

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KR100553667B1 (en) 2006-02-24

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