CN1434072A - High-strength antimicrobial dialdehyde starch crosslinked chitosan membane and preparation method and use thereof - Google Patents
High-strength antimicrobial dialdehyde starch crosslinked chitosan membane and preparation method and use thereof Download PDFInfo
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Abstract
The present invention relates to a high-strength antimirobial dialdehyde starch cross-linked chitosan film, its production method and application. It is made up by using 1-3 wt% of chitosan acetic acid aqueos solution and 2-7 wt% of dialdehyde starch and adopting the processes of fully stirring, mixing, centrifugal defoaming, film-making, washing with acid, washing with water, drying by airing to obtain the invented product dried film. Said chitosan cross-linked film has excellent mechanical strength, flexibility and good antibacterial function, and has no toxic side effect for human body. Said chitosan cross-linked film has good bacteria-inhibiting action, can be used as clinical medical material for reducing infection of wound.
Description
Technical field
The present invention relates to a kind of high strength germ resistance dialdehyde starch crosslinked chitosan film and method for making and purposes.
Background technology
(Chitosan is β-(1 → 4)-2-amino-D-pyrans dextran CS) to chitosan, has biological functions such as good biological activity, biocompatibility, biodegradability and antibiotic, hemostasis, anti-inflammatory and promotion wound healing.The thread-like molecule chain structure of chitosan makes it have good film-forming properties, and its mould material can be used as artificial skin, hemostatic material and wound dressing material etc.Up to the present, almost also do not have chitosan film to obtain the practical, commercial of suitability for industrialized production, one of most important reason is that chitosan is membranous crisp, and mechanical property is relatively poor, and the physical strength that therefore improves the chitosan film material just becomes expands its key in application.Adopt at present extensively linking agent such as epoxy chloropropane, glutaraldehyde, dibasic acid anhydride and chitosan crosslinked method can improve the mechanical property of chitosan film, but these linking agents itself are exactly the stronger material of toxicity, harmful to HUMAN HEALTH, its application as medical material is restricted.
Summary of the invention
The objective of the invention is to overcome the problem of the deficiencies in the prior art and existence, and then a kind of high strength germ resistance dialdehyde starch crosslinked chitosan film and method for making and purposes that human body is had no side effect is provided.
Technical scheme provided by the invention is: high strength germ resistance dialdehyde starch crosslinked chitosan film, chitosan aqueous acetic acid with 1-3% (weight ratio), fully mix with the dialdehyde starch aqueous solution of 2-7% (weight ratio), evacuation and centrifugal degassing, the system film, deacidification, wash, dry, dry film is dialdehyde starch crosslinked chitosan film required for the present invention.
The present invention also provides the method for making of above-mentioned high strength germ resistance dialdehyde starch crosslinked chitosan film, and chitosan is dissolved in the aqueous acetic acid of 1-4% (volume ratio), filter, the chitosan solution of 1-3% (weight ratio); Dialdehyde starch is dissolved in 60 ℃ the water, filter the dialdehyde starch aqueous solution of 2-7% (weight ratio).With the above-mentioned chitosan solution and the dialdehyde starch aqueous solution is 100 by weight: the ratio of 1-10 fully mixes, and evacuation and centrifugal degassing is straight Glass tubing knifing on the sheet glass of cleaning of copper wire then with two ends, the infrared lamp oven dry.Above-mentioned sheet glass is put into the NaOH aqueous solution and the residual acid that weight percentage is 1-5%.Take off film, flowing water fully washes, and dries with distilled water wash again, and dry film is the dialdehyde starch crosslinked chitosan film of the present invention's preparation.
The chitose crosslinked membrane of the present invention's preparation has excellent mechanical strength, snappiness and good antimicrobial property, and human body is had no side effect.(Dialdehyde Starch is a kind of natural polymer dialdehyde DAS) to dialdehyde starch, also is a kind of linking agent of excellent performance, and human body is had no side effect, and is widely used in fields such as weaving, medicine, food.The present invention proposes with dialdehyde starch chitosan to be carried out crosslinked, has significantly improved the physical strength and the snappiness of chitosan film; Simultaneously, the present invention also simulates the condition of human body physiological pH value (7.2-7.6), prepared a series of chitose crosslinked membranes have been carried out antibacterial experiment to two kinds of common representative bacteriums (streptococcus aureus and intestinal bacteria), the result shows that prepared a series of chitose crosslinked membranes all have good bacteriostatic action, and it is applied to the clinical probability that will reduce wound infection as bio-medical material.
Embodiment
Embodiment 1: with deacetylation is 90.2%, and viscosity-average molecular weight is 5.0 * 10
5Chitosan be dissolved in the aqueous acetic acid of 2% (volume ratio), filter, the chitosan solution of 3% (weight ratio); With oxidisability is that 63.5% dialdehyde starch is dissolved in 60 ℃ the water, filter the dialdehyde starch aqueous solution of 5% (weight ratio).Above-mentioned chitosan solution and the dialdehyde starch aqueous solution ratio in 99: 1 (weight ratio) is fully mixed, and evacuation and centrifugal degassing is straight Glass tubing knifing on the sheet glass of cleaning of copper wire then with two ends, the infrared lamp oven dry.Above-mentioned sheet glass is put into NaOH solution and the residual acid that weight percentage is 1-5%.Take off film, flowing water fully washes, and dries the dialdehyde starch crosslinked chitosan film CSD-1 that obtains containing 1% (weight ratio) dialdehyde starch with distilled water wash again.
Embodiment 2: change the blending ratio of the above-mentioned chitosan solution and the dialdehyde starch aqueous solution into 97: 3 (weight ratio), all the other obtain containing the dialdehyde starch crosslinked chitosan film CSD-2 of 3% (weight ratio) dialdehyde starch with embodiment 1.
Embodiment 3: change the blending ratio of the above-mentioned chitosan solution and the dialdehyde starch aqueous solution into 95: 5 (weight ratio), all the other obtain containing the dialdehyde starch crosslinked chitosan film CSD-3 of 5% (weight ratio) dialdehyde starch with embodiment 1.
Embodiment 4: change the blending ratio of the above-mentioned chitosan solution and the dialdehyde starch aqueous solution into 93: 7 (weight ratio), all the other obtain containing the dialdehyde starch crosslinked chitosan film CSD-4 of 7% (weight ratio) dialdehyde starch with embodiment 1.
Embodiment 5: change the blending ratio of the above-mentioned chitosan solution and the dialdehyde starch aqueous solution into 91: 9 (weight ratio), all the other obtain containing the dialdehyde starch crosslinked chitosan film CSD-5 of 9% (weight ratio) dialdehyde starch with embodiment 1.
Comparative example: with deacetylation is 90.2%, and viscosity-average molecular weight is 5.0 * 10
5Chitosan be dissolved in the aqueous acetic acid of 2% (volume ratio), filter, the chitosan solution of 3% (weight ratio); With above-mentioned chitosan solution evacuation and centrifugal degassing, be straight Glass tubing knifing on the sheet glass of cleaning of copper wire then with two ends, the infrared lamp oven dry.Above-mentioned sheet glass is put into NaOH solution and the residual acid that massfraction is 1-5%.Take off film, flowing water fully washes, and dries with distilled water wash to obtain chitosan film CS again.
Tensile strength (σ according to ISO6239-1986 (E) standard testing dialdehyde starch crosslinked chitosan film CSD-1, CSD-2, CSD-3, CSD-4, CSD-5 and chitosan film CS
b) and elongation at break (ε
b), speed of experiment is 5mm/min, repeats five times and averages.Test result is listed in table 1.
Table 1: the mechanical property of dialdehyde starch crosslinked chitosan film
Sample tensile strength/MPa elongation at break/%
CS 46.0 16.9
CSD-1 84.5 19.5
CSD-2 106.1 23.7
CSD-3 113.1 27.0
CSD-4 101.8 21.3
CSD-5 86.9 11.5
Can find from table: along with dialdehyde starch content increases, the tensile strength of cross linking membrane increases rapidly, reaches maximum value when dialdehyde starch content is 5%, and its value is 113.1MPa, has improved 145.7% than the tensile strength (46.0MPa) of pure chistosan film CS.The elongation at break variation tendency of chitose crosslinked membrane is similar to the variation tendency of its tensile strength, reaches maximum value when dialdehyde starch content is 5%, and its value is 27.0%, has improved 59.8% than the elongation at break (16.9%) of pure chistosan film.
The bacteriostatic action mechanism more complicated of chitosan, major cause may be: chitosan is a cationic polymers, contains positively charged amino on its molecular chain, bacterium can be bonded together, and stops its diffusion, thereby makes chitosan have bacteriostatic action.
Table 2: the anti-microbial property of dialdehyde starch crosslinked chitosan film
Colony number (CFU/cm
2)
Sample
Staphylococcus aureus e coli
CSD-1 5.6×10
3 6.4×10
3
CSD-2 1.0×10
4 9.8×10
3
CSD-3 3.5×10
4 5.1×10
4
CSD-4 6.2×10
4 7.8×10
4
CSD-5 7.0×10
4 9.3×10
4
Contrast 4.6 * 10
57.8 * 10
5
Table 2 shows the external fungistatic effect of dialdehyde starch crosslinked chitosan film, and control sample is the blank sample of blooming not.Can find that prepared a series of chitose crosslinked membranes all have certain bacteriostatic action from table, it is applied to the clinical probability that will reduce wound infection as bio-medical material.
Claims (3)
1. a high strength germ resistance dialdehyde starch crosslinked chitosan film by the chitosan aqueous acetic acid of 1-3% (weight percent), makes with the dialdehyde starch aqueous solution of 2-7% (weight percent).
2. the method for making of the described dialdehyde starch crosslinked chitosan film of claim 1 is characterized in that: chitosan is dissolved in the aqueous acetic acid of 1-4% (volume percent), filters, the chitosan solution of 1-3% (weight percent); Dialdehyde starch is dissolved in 60 ℃-80 ℃ the water, filter the dialdehyde starch aqueous solution of 2-7% (weight percent); With the above-mentioned chitosan solution and the dialdehyde starch aqueous solution is 100 by weight: the ratio of 1-10 fully mixes, and evacuation and centrifugal degassing is straight Glass tubing knifing on the sheet glass of cleaning of copper wire then with two ends, the infrared lamp oven dry; Above-mentioned sheet glass is put into the NaOH aqueous solution and the residual acid that weight percent is 1-5%; Take off film, flowing water fully washes, again with distilled water wash, dry, dry film is the dialdehyde starch crosslinked chitosan film of the present invention preparation.
3. the described dialdehyde starch crosslinked chitosan film of claim 1 is as bio-medical material.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB031185355A CN1168766C (en) | 2003-01-27 | 2003-01-27 | High-strength antimicrobial dialdehyde starch crosslinked chitosan membane and preparation method and use thereof |
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|---|---|---|---|
| CNB031185355A CN1168766C (en) | 2003-01-27 | 2003-01-27 | High-strength antimicrobial dialdehyde starch crosslinked chitosan membane and preparation method and use thereof |
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| CN1434072A true CN1434072A (en) | 2003-08-06 |
| CN1168766C CN1168766C (en) | 2004-09-29 |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102206223A (en) * | 2010-03-29 | 2011-10-05 | 清华大学 | Optical probe film and special-purposed organic dye for micro determination of copper ion content in water sample |
| CN105885068A (en) * | 2014-12-08 | 2016-08-24 | 北京服装学院 | Crosslinked chitosan membrane and application thereof |
| CN106046400A (en) * | 2016-06-20 | 2016-10-26 | 江南大学 | Preparation method of dialdehyde cellulose cross-linked chitosan film |
| CN109260504A (en) * | 2018-10-08 | 2019-01-25 | 青岛博益特生物材料股份有限公司 | A kind of amino sugar hemostasis medical material and its preparation method and application |
| CN109289074A (en) * | 2018-10-08 | 2019-02-01 | 青岛博益特生物材料股份有限公司 | A kind of wound healing material and its preparation method and application |
| CN109364287A (en) * | 2018-10-08 | 2019-02-22 | 中国海洋大学 | A kind of polysaccharide bleeding-stopping dressing and its preparation method and application |
| CN110089562A (en) * | 2019-05-15 | 2019-08-06 | 东南大学 | A kind of preparation method of fruit anti-mildew fresh-keeping coating |
| CN110423456A (en) * | 2019-08-13 | 2019-11-08 | 湖南工业大学 | A kind of preparation method of high intensity dual network biomass membrane material |
| CN113207946A (en) * | 2020-12-05 | 2021-08-06 | 西北农林科技大学 | Preparation method of high-water-absorptivity aerogel pad with bacteriostatic function and application of high-water-absorptivity aerogel pad in chilled meat preservation |
| CN117186503A (en) * | 2022-11-15 | 2023-12-08 | 青岛健康海洋生物制药有限公司 | Preparation method and application of chitosan material suitable for mucosal administration |
-
2003
- 2003-01-27 CN CNB031185355A patent/CN1168766C/en not_active Expired - Fee Related
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102206223A (en) * | 2010-03-29 | 2011-10-05 | 清华大学 | Optical probe film and special-purposed organic dye for micro determination of copper ion content in water sample |
| CN105885068A (en) * | 2014-12-08 | 2016-08-24 | 北京服装学院 | Crosslinked chitosan membrane and application thereof |
| CN106046400A (en) * | 2016-06-20 | 2016-10-26 | 江南大学 | Preparation method of dialdehyde cellulose cross-linked chitosan film |
| CN109260504A (en) * | 2018-10-08 | 2019-01-25 | 青岛博益特生物材料股份有限公司 | A kind of amino sugar hemostasis medical material and its preparation method and application |
| CN109289074A (en) * | 2018-10-08 | 2019-02-01 | 青岛博益特生物材料股份有限公司 | A kind of wound healing material and its preparation method and application |
| CN109364287A (en) * | 2018-10-08 | 2019-02-22 | 中国海洋大学 | A kind of polysaccharide bleeding-stopping dressing and its preparation method and application |
| CN110089562A (en) * | 2019-05-15 | 2019-08-06 | 东南大学 | A kind of preparation method of fruit anti-mildew fresh-keeping coating |
| CN110423456A (en) * | 2019-08-13 | 2019-11-08 | 湖南工业大学 | A kind of preparation method of high intensity dual network biomass membrane material |
| CN113207946A (en) * | 2020-12-05 | 2021-08-06 | 西北农林科技大学 | Preparation method of high-water-absorptivity aerogel pad with bacteriostatic function and application of high-water-absorptivity aerogel pad in chilled meat preservation |
| CN117186503A (en) * | 2022-11-15 | 2023-12-08 | 青岛健康海洋生物制药有限公司 | Preparation method and application of chitosan material suitable for mucosal administration |
| CN117186503B (en) * | 2022-11-15 | 2024-04-30 | 青岛健康海洋生物制药有限公司 | Preparation method and application of chitosan material suitable for mucosal administration |
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|---|---|
| CN1168766C (en) | 2004-09-29 |
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