CN102604138A - Method for preparing chitosan substrate film by self-deposition of micron gel - Google Patents
Method for preparing chitosan substrate film by self-deposition of micron gel Download PDFInfo
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Abstract
The invention discloses a method for preparing a chitosan substrate film by self-deposition of micron gel. The method comprises the following steps: dissolving chitosan into a diluted acid aqueous solution to prepare a chitosan acid solution; carrying out ultrasonic oscillation, and simultaneously dropwise adding a chitosan precipitating agent so as to separate out chitosan hydrogel; washing the chitosan hydrogel with deionized water until pH value is 7.4; and filtering to obtain chitosan micron hydrogel; and soaking the chitosan micron hydrogel into a glycerol aqueous solution or a glycerol aqueous solution containing a thrombin medicament or an antibacterial active matter, filtering, centrifuging, injecting into a mould, and drying under a vacuum condition. The method disclosed by the invention is simple in preparation process; the prepared chitosan film is loose in structure and has high water permeability and high compliance, and does not curl when contacting water; and various hemostatic or antibacterial medicament active components can be conveniently loaded in chitosan, and the prepared chitosan film is a good medicament carrier.
Description
Technical field
The present invention relates to a kind of preparation method of chitosan basal body film, especially micron gel auto-deposition prepares the method for chitosan basal body film.
Background technology
Chitosan (Chitosan); Formal name used at school (1; 4)-2-amino-2-deoxidation-β-D-glucose; Be a kind of biopolymer that after deacetylated reaction, is obtained chitin (N-acetyl-2-acetylaminohydroxyphenylarsonic acid D-glucose is formed by connecting with the 1-4 glycosidic link), contain two kinds of structural units of N-acetamido glucose and N-GS in its molecular chain usually, both ratios are different with the difference of degree of deacetylation.
Chitin (chitin) derives from ocean shell and algae, chitosan be chitin take off the acetyl product.A kind of natural weakly alkaline biomass sugar of chitosan has excellent biocompatibility, and is nontoxic, has function
antibiotic, that stop blooding, promote wound healing.At present Application of Chitosan is day by day extensive, comprises fields such as medical, agriculture, makeup.Wherein the application in medical field causes people's attention in recent years day by day.The chitosan tourniquet bandage of U.S. Hemcon company (Chitosan Bandages) for example is mainly used in the on-the-spot hemostatic treatment of acute traumatic hemorrhage and bullet wound, as the indispensable first-aid appliance of US soldiers staff; (2006 through the FDA authentication of the U.S. and the CE authentication of European Union for " CELOX " styptic powder of Britain; 2010 through the authentication of Chinese food Drug Administration).
Chitosan structure is tight, has higher percent crystallinity, and no fusing point is difficult to prepare moulding with methods such as ordinary method such as fusion injection mouldings.Breaking through a chitosan machine-shaping difficult problem is the effective way that enlarges the chitosan Application Areas.The molding mode of chitosan comprises the spinning of static electricity, solution stretch spinning at present, and the main at present solution casting method that adopts of the preparation of chitosan film is about to chitosan and is dissolved in advance in acid or the alkali solvent, is poured into the moulding of mould after drying.Mainly contain following several kinds: method one, convection drying film forming behind the solution injection mould; Method two, solution inject mould after drying film forming, then with alkali or acid neutralization, wash to the neutrality drying and forming-film again; Method three, solution are injected mould, and progressively neutralizing with alkali lye or acid solution obtains tabular gel, wash to the neutrality drying and forming-film again.What method one obtained is the film that contains acid or alkali, is unfavorable for prolonged preservation; What the two kinds of methods in back obtained is the neutral film.What these three kinds of methods obtained at last all is dense film, and it is curling when suction, all can to expand, and is unfavorable for using.Method two prepares and promptly is easy to cause curling of film in the process.Method three is similar to the original position precipitation method, and in neutral process progressively, chitosan gel rubber can form layering, and gel can deform even curls in the drying process.Therefore, the preparation technology of chitosan film is still waiting to improve.
Summary of the invention
The purpose of this invention is to provide the method that the simple micron of a kind of preparation technology gel auto-deposition prepares the chitosan basal body film, to obtain loose and to meet the unconvoluted film of water.
For achieving the above object, micron gel auto-deposition of the present invention prepares the method for chitosan basal body film, may further comprise the steps:
The first step:
Chitosan is dissolved in the dilute acid solution; Be mixed with the chitosan acid solution of mass concentration 2%, remove by filter insoluble substance, sonic oscillation; In solution, dropwise add the agent of chitosan precipitating simultaneously; Separate out chitosan gel rubber, sonic oscillation control chitosan gel rubber particle diameter makes the chitosan micron hydrogel suspension between 100～500 μ m;
Second step:
Chitosan micron hydrogel suspension use deionized water wash to the pH value that the first step is made is 7.4, filters, and obtains the chitosan micron hydrogel;
The 3rd step:
It is in 0.5%～10% the glycerin solution behind 30-60min that the second chitosan micron hydrogel that make of step is immersed mass concentration, filters, and obtains USP Kosher plastifying chitosan micron hydrogel;
The 4th step:
USP Kosher plastifying chitosan micron hydrogel is centrifugal, and control USP Kosher plastifying chitosan micron hydrogel water ratio is 100%～500% of a chitosan mass; Then USP Kosher plastifying chitosan micron hydrogel is injected mould, under vacuum or condition of normal pressure,, obtain the chitosan basal body film in 45～80 ℃ of oven dry.
Among the present invention, the deacetylation of said chitosan is 50%～100%, and molecular weight is 100000～500000.The account form of deacetylation is like the 846th～848 page of " analytical chemistry research notes " 2002 the 7th phase, " the soda acid Conductometric Titration Method deacetylating degree of chitosan " that Jia Zhishen, the Li Xiu tinkling of pieces of jade are write.
Have hemostasis or antimicrobial function in order to give the chitosan basal body film, can in glycerin solution, add Ox-Dapro, CaCl
2Or the tranexamic acid blood-clotting agent, perhaps add terramycin or nanometer silver antimicrobial active substance.The add-on of medicine is selected as required.
Among the present invention, used mould can be petridish etc. similar have uncovered, the vessel of other position sealing; Also can be that sub-sieve etc. is similar has uncoveredly, and the bottom has the utensil of porous gauze.
Among the present invention, described diluted acid is that mass concentration is that 1%～5% aqueous formic acid, mass concentration are that 1%～5% acetic acid aqueous solution or mass concentration are 1%～5% aqueous hydrochloric acid.
Among the present invention, the agent of described chitosan precipitating can be that mass concentration is that 5% the NaOH aqueous solution, mass concentration are that 5% the KOH aqueous solution, mass concentration are that 5% NaOH ethanolic soln or mass concentration are 5% KOH ethanolic soln.
The present invention has advantage and effect:
1, the present invention utilizes capillary force and Van der Waals force between the chitosan micron hydrogel particle to interconnect; Drying and moulding need not add linking agent, only needs once washing; Simplify preparation technology greatly, can prepare smooth, regular chitosan film fast.
2, the chitosan film of the present invention's preparation, short texture has high water permeability, meets water and does not curl, and compliance is high, can be attached at various surfaces easily.
3, the present invention uses neutral chitosan micron hydrogel, can conveniently in chitosan, load various hemostasis or antimicrobial active constituents of medicine, is a kind of excellent drug carrier.
Embodiment
Below in conjunction with embodiment the present invention is further described:
Embodiment 1:
(1) get 2g deacetylation 95%, the chitosan of molecular weight 100,000, adding the 200ml mass concentration is 2% acetic acid aqueous solution, stirring at room is mixed with the chitosan acetic acid aqueous solution of 1% (m/v), standing and defoaming to dissolving fully; Above-mentioned solution is filtered; Sonic oscillation in the ultra-sonic dispersion device dropwise adds 5% aqueous sodium hydroxide solution simultaneously in solution, until precipitating fully; Make the chitosan micron hydrogel suspension, the particle diameter of the chitosan micron gel of gained is between 300～500 μ m;
(2) with deionized water rinsing chitosan micron hydrogel suspension to neutral pH=7.4, filter, obtain the chitosan micron hydrogel;
(3) the chitosan micron hydrogel that makes is immersed in the USP Kosher solution of mass concentration 1%, behind the 30min, filter, obtain USP Kosher plastifying chitosan micron hydrogel;
(4) carry out USP Kosher plastifying chitosan micron hydrogel centrifugal; Remove unnecessary water; Control USP Kosher plastifying chitosan micron hydrogel water ratio is 100% of a chitosan mass; Then USP Kosher plastifying chitosan micron hydrogel is injected mould, in 60 ℃ of oven dry, obtain the chitosan basal body film under the condition of normal pressure.This chitosan film has high water permeability, meets water and does not curl.
Embodiment 2:
(1) get 2g deacetylation 85%, the chitosan of molecular weight 200,000, adding the 200ml mass concentration is 2% aqueous hydrochloric acid, stirring at room is mixed with the chitosan salt aqueous acid of 1% (m/v), standing and defoaming to dissolving fully; Above-mentioned solution is filtered; Sonic oscillation in the ultra-sonic dispersion device dropwise adds 5% potassium hydroxide aqueous solution simultaneously in solution, until precipitating fully; Make the chitosan micron hydrogel suspension, the particle diameter of the chitosan micron gel of gained is between 100～300 μ m;
(2) with deionized water rinsing chitosan micron hydrogel to neutral pH=7.4, filter, obtain the chitosan micron hydrogel;
(3) the chitosan micron hydrogel immersion that makes is contained mass concentration 1% USP Kosher, 0.5%CaCl
2In 1% Ox-Dapro solution, the 30min after-filtration obtains containing CaCl
2USP Kosher plasticising chitosan micron hydrogel with Ox-Dapro;
(4) (3) step contained CaCl
2Carry out centrifugally with the USP Kosher plasticising chitosan micron hydrogel of Ox-Dapro, remove unnecessary water, control chitosan micron hydrogel water ratio is 100% of a chitosan mass, will contain CaCl then
2Inject mould with the USP Kosher plasticising chitosan micron hydrogel of Ox-Dapro, under vacuum condition,, obtain containing CaCl in 45 ℃ of oven dry
2With the USP Kosher plastifying chitosan film of Ox-Dapro, this film can be used for quick-acting haemostatic powder.
Embodiment 3:
(1) get 2g deacetylation 75%, the chitosan of molecular weight 500,000, adding the 200ml mass concentration is 2% acetic acid aqueous solution, stirring at room is mixed with the chitosan acetic acid aqueous solution of 1% (m/v), standing and defoaming to dissolving fully; Above-mentioned solution is filtered; Sonic oscillation in the ultra-sonic dispersion device dropwise adds 5% aqueous sodium hydroxide solution simultaneously in solution, until precipitating fully; Make the chitosan micron hydrogel suspension, the particle diameter of the chitosan micron gel of gained is between 100～300 μ m;
(2) with deionized water rinsing chitosan micron hydrogel to neutral pH=7.4, filter, obtain the chitosan micron hydrogel;
(3) the chitosan micron hydrogel immersion that makes is contained in the aqueous solution of mass concentration 1% USP Kosher, 1% Ox-Dapro and 0.5% nanometer silver, behind the 30min, filter, obtain containing the USP Kosher plastifying chitosan micron hydrogel of Ox-Dapro and nanometer silver;
The USP Kosher plastifying chitosan micron hydrogel that (4) will contain Ox-Dapro and nanometer silver carries out centrifugal; Remove unnecessary water; Control chitosan micron hydrogel water ratio is 200% of a chitosan mass; The USP Kosher plastifying chitosan micron hydrogel that will contain Ox-Dapro and nanometer silver then injects mould, under vacuum condition, in 80 ℃ of oven dry, obtains containing the chitosan film of Ox-Dapro and nanometer silver.This chitosan film has the function of antibacterial anti hemorrhagic.
The foregoing description only for letting the personage who is familiar with this technology can understand content of the present invention and enforcement according to this, can not limit protection scope of the present invention with this.All equivalences that spirit is done according to the present invention change or modify, and all should be encompassed within protection scope of the present invention.
Claims (5)
1. a micron gel auto-deposition prepares the method for chitosan basal body film, it is characterized in that may further comprise the steps:
The first step:
Chitosan is dissolved in the dilute acid solution; Be mixed with the chitosan acid solution of mass concentration 2%, remove by filter insoluble substance, sonic oscillation; In solution, dropwise add the agent of chitosan precipitating simultaneously; Separate out aquagel, sonic oscillation control chitosan gel rubber particle diameter makes the chitosan micron hydrogel suspension between 100～500 μ m;
Second step:
Chitosan micron hydrogel suspension use deionized water wash to the pH value that the first step is made is 7.4, filters, and obtains the chitosan micron hydrogel;
The 3rd step:
It is in 0.5%～10% the glycerin solution behind 30-60min that the second chitosan micron hydrogel that make of step is immersed mass concentration, filters, and obtains USP Kosher plastifying chitosan micron hydrogel;
The 4th step:
USP Kosher plastifying chitosan micron hydrogel is centrifugal, and control USP Kosher plastifying chitosan micron hydrogel water ratio is 100%～500% of a chitosan mass; Then USP Kosher plastifying chitosan micron hydrogel is injected mould, under vacuum or condition of normal pressure,, obtain the chitosan basal body film in 45～80 ℃ of oven dry.
2. micron gel auto-deposition according to claim 1 prepares the method for chitosan basal body film, and it is characterized in that: the deacetylation of said chitosan is 50%～100%, and molecular weight is 100000～500000.
3. micron gel auto-deposition according to claim 1 prepares the method for chitosan basal body film, it is characterized in that: the 3rd step added Ox-Dapro, CaCl in glycerin solution
2Or the tranexamic acid blood-clotting agent, perhaps add terramycin or nanometer silver antimicrobial active substance.
4. micron according to claim 1 gel auto-deposition prepares the method for chitosan basal body film, it is characterized in that: diluted acid is that mass concentration is that 1%～5% aqueous formic acid, mass concentration are that 1%～5% acetic acid aqueous solution or mass concentration are 1%～5% aqueous hydrochloric acid.
5. micron according to claim 1 gel auto-deposition prepares the method for chitosan basal body film, it is characterized in that: the agent of chitosan precipitating is that mass concentration is that 5% the NaOH aqueous solution, mass concentration are that 5% the KOH aqueous solution, mass concentration are that 5% NaOH ethanolic soln or mass concentration are 5% KOH ethanolic soln.
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| CN104707238A (en) * | 2015-03-11 | 2015-06-17 | 浙江大学 | Epidural-subcutaneous buried type analgesia pump with anti-infection function |
| CN104910404A (en) * | 2015-06-24 | 2015-09-16 | 武汉工程大学 | Chitosan-glycerol-nano silver sponge as well as preparation method and application of chitosan-glycerol-nano silver sponge |
| CN106049057A (en) * | 2016-05-31 | 2016-10-26 | 东华大学 | Preparation method of hydrophilic and antistatic polyester fiber |
| CN107050524A (en) * | 2016-12-23 | 2017-08-18 | 江南大学 | A kind of preparation method of novel antibacterial composite biological material |
| CN108066813A (en) * | 2016-11-18 | 2018-05-25 | 南京理工大学 | A kind of preparation method for carrying medicine chitosan film |
| CN110079884A (en) * | 2019-05-08 | 2019-08-02 | 东华大学 | A kind of preparation method of high-specific surface area polyimides fibrid |
| CN111467576A (en) * | 2020-04-29 | 2020-07-31 | 上海市东方医院（同济大学附属东方医院） | Artificial gallbladder wall synthetic material, preparation method and application thereof, and artificial gallbladder wall |
| CN111944366A (en) * | 2020-07-08 | 2020-11-17 | 中山大学 | Preparation method and application of high-adhesion hydrogel coating |
| CN113425889A (en) * | 2021-06-25 | 2021-09-24 | 延安大学 | Antibacterial hemostatic sponge and preparation method and application thereof |
| CN113440643A (en) * | 2021-06-10 | 2021-09-28 | 武汉大学 | Surface antibacterial treatment method of absorbable surgical material |
| CN114685823A (en) * | 2021-12-13 | 2022-07-01 | 河南健康广济生物技术有限公司 | Anti-curling chitosan hydrogel film, preparation method thereof and chronic wound dressing |
| CN115010981A (en) * | 2022-06-24 | 2022-09-06 | 遵义医科大学附属口腔医院 | Solid product containing amino insoluble polymer, preparation method and application thereof |
| CN115252879A (en) * | 2022-07-13 | 2022-11-01 | 肖地生 | Preparation method and application of chitosan hemostatic material |
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| CN104707238A (en) * | 2015-03-11 | 2015-06-17 | 浙江大学 | Epidural-subcutaneous buried type analgesia pump with anti-infection function |
| CN104910404A (en) * | 2015-06-24 | 2015-09-16 | 武汉工程大学 | Chitosan-glycerol-nano silver sponge as well as preparation method and application of chitosan-glycerol-nano silver sponge |
| CN104910404B (en) * | 2015-06-24 | 2018-04-27 | 武汉工程大学 | A kind of chitosan-glycerine-nano silver sponge and its preparation method and application |
| CN106049057A (en) * | 2016-05-31 | 2016-10-26 | 东华大学 | Preparation method of hydrophilic and antistatic polyester fiber |
| CN108066813A (en) * | 2016-11-18 | 2018-05-25 | 南京理工大学 | A kind of preparation method for carrying medicine chitosan film |
| CN107050524A (en) * | 2016-12-23 | 2017-08-18 | 江南大学 | A kind of preparation method of novel antibacterial composite biological material |
| CN110079884B (en) * | 2019-05-08 | 2021-11-02 | 东华大学 | Preparation method of polyimide fibrid with high specific surface area |
| CN110079884A (en) * | 2019-05-08 | 2019-08-02 | 东华大学 | A kind of preparation method of high-specific surface area polyimides fibrid |
| CN111467576A (en) * | 2020-04-29 | 2020-07-31 | 上海市东方医院（同济大学附属东方医院） | Artificial gallbladder wall synthetic material, preparation method and application thereof, and artificial gallbladder wall |
| CN111944366A (en) * | 2020-07-08 | 2020-11-17 | 中山大学 | Preparation method and application of high-adhesion hydrogel coating |
| CN113440643A (en) * | 2021-06-10 | 2021-09-28 | 武汉大学 | Surface antibacterial treatment method of absorbable surgical material |
| CN113425889A (en) * | 2021-06-25 | 2021-09-24 | 延安大学 | Antibacterial hemostatic sponge and preparation method and application thereof |
| CN114685823A (en) * | 2021-12-13 | 2022-07-01 | 河南健康广济生物技术有限公司 | Anti-curling chitosan hydrogel film, preparation method thereof and chronic wound dressing |
| CN114685823B (en) * | 2021-12-13 | 2024-02-09 | 河南健康广济生物技术有限公司 | Anti-curling chitosan hydrogel film, preparation method thereof and chronic wound dressing |
| CN115010981A (en) * | 2022-06-24 | 2022-09-06 | 遵义医科大学附属口腔医院 | Solid product containing amino insoluble polymer, preparation method and application thereof |
| CN115010981B (en) * | 2022-06-24 | 2023-12-05 | 遵义医科大学附属口腔医院 | Solid product containing amino indissolvable polymer, preparation method and application thereof |
| CN115252879A (en) * | 2022-07-13 | 2022-11-01 | 肖地生 | Preparation method and application of chitosan hemostatic material |
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