CN109908394A - Degradable medical antibacterial leakage protection film and preparation method thereof - Google Patents
Degradable medical antibacterial leakage protection film and preparation method thereof Download PDFInfo
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- CN109908394A CN109908394A CN201910140095.XA CN201910140095A CN109908394A CN 109908394 A CN109908394 A CN 109908394A CN 201910140095 A CN201910140095 A CN 201910140095A CN 109908394 A CN109908394 A CN 109908394A
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Abstract
The invention discloses a kind of degradable medical antibacterial leakage protection films and preparation method thereof.After cellulose is carried out oxidation processes by the method, it is added in alginate solution after homogeneous and forms suspension and carried out spin coating, be immersed in Ca after dry2+Drying and forming-film after being crosslinked it in solion, it is finally that film is compound with chitosan solution, obtain the medical protective film of antiseep of biodegradable and anti-microbial property fine and close soft and with certain mechanical strength.Raw material sources of the present invention are safe and environment-friendly; product has very excellent biocompatibility; protective film obtained is soft fine and close; with stronger mechanical strength and excellent anti-microbial property; and pattern and intensity can degrade after maintaining a period of time in vivo, for the leakage protection at wound suture position suitable for performing the operation.
Description
Technical field
The present invention relates to a kind of degradable medical antibacterial leakage protection films and preparation method thereof, belong to bio-medical material
Technical field.
Background technique
Complication, including hematobilia and gallbladder leakage etc. are often accompanied by liver or kidney surgery.Complication can generate serious
Consequence, including surgical effect is influenced, delay Rehabilitation, may result in second operation and risk is high, serious person's even meeting
Lead to death.The control method of existing hepatobiliary surgery complication includes antibiotic treatment, insertion drainage tube, second operation etc.,
Its failure rate is high, and risk is big, and can cause considerable distress to patient, it is, thus, sought for the method for new control leakage.?
The surface of a wound wraps up one layer of absorbable bio-medical protective film to prevent the leakage of bile or blood from can dramatically avoid
The generation of complication.
Alginate is a kind of natural anionic polymer, due to its good biocompatibility and low cell toxicant
Property, it is widely studied and applied in the fields of biomedicine such as wound dressing and medical gel.Especially calcium ion with
Alginate can form the calcium with " nucleocapsid " structure under cation interaction and induce gel.Alginate dressing can absorb
A large amount of Wound exudates provide physiology wet microenvironment for wound healing.But poor chemical stability, the machine of pure alginate film
Tool intensity is weak and structural degradation is uncontrollable, limits its further applying on medical dressing.Chitosan is that one kind derives from
The natural polysaccharide of the renewable resources such as crab shell, shrimp shell has good biocompatibility and antibiotic property.But pure chitosan dressing
There is also hygroscopicity is poor and the uncontrollable problem of degrading.
Cellulose especially bacteria cellulose (BC) have splendid biocompatibility, and it is with high purity, nontoxic, without dirt
Dye.More importantly bacteria cellulose also has many high molecular excellent performances of synthesis, such as good mechanical property, height simultaneously
Modulus, chemical stability and hydrophily etc..The oxidation of cellulose is to prepare new medical material such as pharmaceutical carrier, can absorb only
The important means of blood gauze etc..Cellulose oxidation reaction is usually the oxidation reaction of 3 hydroxyls of cellulose glucose unit, can
Aldehyde radical, ketone group and carboxyl are generated, not only can change the structure of cellulose, while giving many new objects of cellulose after oxidation
Physical chemistry characteristic is greatly expanded the application range of cellulosic material.Have using the aldehyde radical of cellulose, carboxyl etc. after oxidation
The group of reactivity, can by oxycellulose carry out functional modification or with other function Material cladding, formed simultaneously
Composite material with bioactivity and functionalization.
Summary of the invention
The purpose of the present invention is to provide the controllable degradable medical antibacterial antiseeps of a kind of mechanical property and degradation property
Protective film and preparation method thereof.
Realize that the technical solution of the object of the invention is as follows:
The preparation method of degradable medical antibacterial leakage protection film, the specific steps are as follows:
Step 1, cellulose is pre-processed, placing it in oxidation processes in oxidation system is oxidized to its surface hydroxyl
Carboxyl or aldehyde radical；
Step 2,0.5~10% sodium alginate aqueous solution is mixed with 0.5~10% oxycellulose suspension
It is even, pour into casting film and the drying at 10~60 DEG C in mold；
Step 3, the material after drying is immersed in 0.1~10%CaCl2Ethanol/water solution in, stand 0.5~48h,
React it sufficiently, it is dry at 10~60 DEG C；
Step 4, film step 3 obtained is immersed in 0.5~20% chitosan solution, is impregnated 0.5~72h, is made film
Carboxyl or aldehyde radical in middle calcium alginate and oxycellulose are sufficiently reacted with the amido on chitosan surface, are done in 10~60 DEG C
Dry film forming obtains degradable medical antibacterial leakage protection film.
In step 1, the cellulose can be native cellulose, synthetic cellulose etc..Cellulose pattern can be wadding
Shape, membranaceous, whisker, powder etc..The cellulose can be bacteria cellulose, can be the cotton-shaped bacterium that dynamic cultivation obtains
Cellulose is also possible to the powder obtained after the membranaceous cellulose, or both that static culture obtains is ground, or
It is the whisker etc. obtained after hydrolyzing.
In step 1, the oxidizability of the oxycellulose is 0.5~30%.The oxidation system is selected from titanium dioxide
Nitrogen systems, TEMPO class system, laccase system, hypochlorite system or sodium metaperiodate system, but not limited to this.
In step 2, the mass ratio of the sodium alginate and oxycellulose is 1:0.1~20.
In step 3, the mass ratio of the ethyl alcohol and water is 1:1~99.
In step 4, the molecular weight of chitosan is 50,000~400,000, and the solvent of chitosan solution is acetic acid/water solution,
The volume ratio of acetic acid and water is 0.5~5%.
Compared with prior art, the invention has the following advantages that
The present invention uses safe and non-toxic natural polymer fibers element as raw material, will using a series of physical chemical method
Each component is connected in the form of covalent bond or non-covalent bond, gives full play to the excellent properties of each component, and fills up mechanics
Performance is poor, and pattern is held time the defects of shorter.Medical wounded surface Protective coatings of the invention have excellent mechanical property
With controllable degradation property, degradable performance can exempt operation after more change dressings when caused by surface of a wound secondary injury and
A possibility that reducing infection, and its moist environment created is conducive to the healing of the surface of a wound, has as postoperative protective film potential
Application prospect.
Detailed description of the invention
Fig. 1 is degradable medical antibacterial leakage protection film pictorial diagram of the invention.
Fig. 2 is the mechanical strength comparison of one month front and back of degradable medical antibacterial leakage protection membrane degradation of the invention
Figure.
Fig. 3 is membrane degradation one month mass change figure of degradable medical antibacterial leakage protection of the invention.
Fig. 4 is the mechanical property figure of degradable medical antibacterial leakage protection film of the invention.
Specific embodiment
Below with reference to embodiment and attached drawing, the invention will be further described.
Embodiment 1
Step 1, cellulose is pre-processed, places it in phosphate buffer magnetic agitation 30 minutes at 60 DEG C
So that it is uniformly dispersed, sequentially add TEMPO, sodium chlorite, sodium hypochlorite, the magnetic stirrer over night at 60 DEG C uses acid base titration
It is 8% that method, which measures its oxidizability,；
Step 2, by the oxycellulose suspension of the sodium alginate aqueous solution of 3% (g/mL) of preparation and 3% (g/mL)
It is uniformly mixed with the ratio of 1:9, is poured into casting film and the drying at 25 DEG C in mold；
Step 3, resulting materials are immersed in 3% (g/mL) CaCl2Ethanol/water (5:95, g/g) solution in, stand 12h
React it sufficiently, it is dry at 25 DEG C；
Step 4, above-mentioned film is soaked in the chitosan solution that molecular weight that concentration is 4% (g/mL) is 50,000 for 24 hours, is made
Carboxyl in film in calcium alginate and oxycellulose is sufficiently reacted with the amido on chitosan surface, the drying and forming-film at 25 DEG C.
Fig. 1 is the degradable medical antibacterial leakage protection film of preparation.Fig. 2 is the degradable medical antibacterial antiseep of preparation
Protective film carries out the mechanical strength comparison diagram of the front and back of external degradation one month, and material is still after degrading one month as seen from the figure
With certain mechanical strength, the package surface of a wound can satisfy up to the actual demand of its healing.
Embodiment 2
Step 1, cellulose is pre-processed, with CCl4As inertia catalyzing enzyme, NO is used2(N2O4) as at oxidant
Reason makes its surface hydroxyl be oxidized to carboxyl, is after reaction overnight 30% with its oxidizability of determination of acid-basetitration；
Step 2, by 0.5% sodium alginate aqueous solution of preparation with 0.5% oxycellulose suspension with 10:1's
Ratio is uniformly mixed, and is poured into casting film and the drying at 60 DEG C in mold；
Step 3, resulting materials are immersed in 0.1%CaCl2Ethanol/water (1:99, g/g) solution in, stand 48h make it
Sufficiently reaction, makes it dry at 60 DEG C；
Step 4, above-mentioned film is soaked in 72h in the chitosan solution that molecular weight that concentration is 0.5% is 400,000 makes in film
Carboxyl in calcium alginate and oxycellulose is sufficiently reacted with the amido on chitosan surface, the drying and forming-film at 60 DEG C.
Embodiment 3
Step 1, cellulose is pre-processed, places it in phosphate buffer magnetic agitation 30 minutes at 60 DEG C
So that it is uniformly dispersed, sequentially add TEMPO, sodium chlorite, sodium hypochlorite, the magnetic stirrer over night at 60 DEG C uses acid base titration
It is 8% that method, which measures its oxidizability,；
Step 2, by 3% sodium alginate aqueous solution of preparation with 3% oxycellulose suspension with the mass ratio of 3:7
It is uniformly mixed, is poured into casting film and the drying at 25 DEG C in mold；
Step 3, resulting materials are immersed in 3%CaCl2Ethanol/water (1:1, g/g) solution in, standing fill it for 24 hours
Divide reaction, is made it dry at 60 DEG C；
Step 4, above-mentioned film is soaked in 0.5h in the chitosan solution that molecular weight that concentration is 20% is 220,000 makes in film
Carboxyl or aldehyde radical in calcium alginate and oxycellulose are sufficiently reacted with the amido on chitosan surface, are dried at 60 DEG C
Film.
Embodiment 4
Step 1, cellulose is pre-processed, places it in phosphate buffer magnetic agitation 30 minutes at 60 DEG C
So that it is uniformly dispersed, sequentially add TEMPO, sodium chlorite, sodium hypochlorite, the magnetic stirrer over night at 60 DEG C uses acid base titration
It is 8% that method, which measures its oxidizability,；
Step 2, the oxycellulose suspension of 3% sodium alginate aqueous solution of preparation and 3% is mixed with the ratio of 1:1
It closes uniformly, is poured into casting film and the drying at 40 DEG C in mold；
Step 3, resulting materials are immersed in 3%CaCl2Ethanol/water (5:95, g/g) solution in, stand 36h fill it
Divide reaction, is made it dry at 40 DEG C；
Step 4, by above-mentioned film be soaked in 36h in the chitosan solution that molecular weight that concentration is 5% is 100,000 make it is extra large in film
Carboxyl in calcium alginate and oxycellulose is sufficiently reacted with the amido on chitosan surface, the drying and forming-film at 40 DEG C.
Embodiment 5
Step 1, cellulose is pre-processed, places it in phosphate buffer magnetic agitation 30 minutes at 60 DEG C
So that it is uniformly dispersed, sequentially add TEMPO, sodium chlorite, sodium hypochlorite, the magnetic stirrer over night at 60 DEG C uses acid base titration
It is 8% that method, which measures its oxidizability,；
Step 2, the oxycellulose suspension of 3% sodium alginate aqueous solution of preparation and 3% is mixed with the ratio of 7:3
It closes uniformly, is poured into casting film and the drying at 25 DEG C in mold；
Step 3, resulting materials are immersed in 5%CaCl2Ethanol/water (5:95, g/g) solution in, standing fill it for 24 hours
Divide reaction, is made it dry at 25 DEG C；
Step 4, above-mentioned film is soaked in the chitosan solution that molecular weight that concentration is 10% is 50,000 make for 24 hours it is extra large in film
Carboxyl in calcium alginate and oxycellulose is sufficiently reacted with the amido on chitosan surface, the drying and forming-film at 25 DEG C.
Embodiment 6
Step 1, cellulose is pre-processed, sodium metaperiodate is used to make its surface hydroxyl as oxidizing processing cellulose
Base is oxidized to aldehyde radical, is 0.5% with its oxidizability of determination of acid-basetitration；
Step 2, by 10% sodium alginate aqueous solution of preparation and 10% oxycellulose suspension with the ratio of 3:7
It is uniformly mixed, is poured into casting film and the drying at 10 DEG C in mold；
Step 3, resulting materials are immersed in 0.1%CaCl2Ethanol/water (5:95, g/g) solution in, stand 1h make it
Sufficiently reaction, makes it dry at 10 DEG C；
Step 4, by above-mentioned film be soaked in 48h in the chitosan solution that molecular weight that concentration is 10% is 400,000 make it is extra large in film
Carboxyl in calcium alginate and oxycellulose is sufficiently reacted with the amido on chitosan surface, the drying and forming-film at 10 DEG C.
Comparative example 1
Step 1,3% sodium alginate aqueous solution of preparation is poured into casting film and the drying at 25 DEG C in mold；
Step 2, resulting materials are immersed in 3%CaCl2Ethanol/water (5:95, g/g) solution in, standing fill it for 24 hours
Divide reaction, is made it dry at 40 DEG C；
Step 3, above-mentioned film is soaked in 0.5h in the chitosan solution that molecular weight that concentration is 20% is 220,000, at 40 DEG C
Lower drying and forming-film.
Comparative example 2
Step 1, cellulose is pre-processed, places it in phosphate buffer magnetic agitation 30 minutes at 60 DEG C
So that it is uniformly dispersed, sequentially add TEMPO, sodium chlorite, sodium hypochlorite, the magnetic stirrer over night at 60 DEG C uses acid base titration
It is 8% that method, which measures its oxidizability,；
Step 2, by 0.1% sodium alginate aqueous solution of preparation with 0.1% oxycellulose suspension with the ratio of 1:1
Example is uniformly mixed, and is poured into after mold and CaCl2Solution can not form a film.
Resulting material will be prepared according to sodium alginate and oxidizing bacteria cellulose in comparative example 1 and embodiment 1,3,4,5
Mass ratio be denoted as TOBC/SA-0, TOBC/SA-10, TOBC/SA-30, TOBC/SA-50 and TOBC/SA-70 respectively.Fig. 3 is
Mass change figure during this several groups of resulting materials are degraded one month in PBS buffer solution.As seen from Figure 3, alginic acid
The variation of the mass ratio of salt and oxidizing bacteria cellulose can cause large effect to the degradation property of material.Fig. 4 is to prepare institute
The mechanical property figure of the material obtained, the variation of alginate and oxidizing bacteria fiber quality ratio also can be to material as seen from Figure 4
Mechanical strength produce bigger effect.In conclusion may be implemented by the mass ratio of control alginate and oxycellulose
Regulation to material mechanical performance and degradation rate.
Claims (10)
1. the preparation method of degradable medical antibacterial leakage protection film, which is characterized in that specific step is as follows:
Step 1, cellulose is pre-processed, placing it in oxidation processes in oxidation system makes its surface hydroxyl be oxidized to carboxyl
Or aldehyde radical；
Step 2,0.5~10% sodium alginate aqueous solution is uniformly mixed with 0.5~10% oxycellulose suspension,
Enter casting film and the drying at 10~60 DEG C in mold；
Step 3, the material after drying is immersed in 0.1~10%CaCl2Ethanol/water solution in, stand 0.5~48h, make it
Sufficiently reaction, it is dry at 10~60 DEG C；
Step 4, film step 3 obtained is immersed in 0.5~20% chitosan solution, impregnates 0.5~72h, is made extra large in film
Carboxyl or aldehyde radical in calcium alginate and oxycellulose are sufficiently reacted with the amido on chitosan surface, are dried in 10~60 DEG C
Film obtains degradable medical antibacterial leakage protection film.
2. preparation method according to claim 1, which is characterized in that in step 1, the cellulose is native cellulose
Or synthetic cellulose.
3. preparation method according to claim 2, which is characterized in that in step 1, the cellulose be it is cotton-shaped, it is membranaceous,
Whisker or powder.
4. preparation method according to claim 2, which is characterized in that in step 1, the cellulose obtains for dynamic cultivation
The membranaceous cellulose or cotton-shaped bacteria cellulose or membranaceous cellulose that the cotton-shaped bacteria cellulose or static culture arrived obtains are ground
The bacteria cellulose whisker that the bacteria cellulose powder or bacteria cellulose obtained after mill processing hydrolyzes.
5. preparation method according to claim 1, which is characterized in that in step 1, the oxidizability of the oxycellulose
It is 0.5~30%.
6. preparation method according to claim 1, which is characterized in that in step 1, the oxidation system is selected from titanium dioxide
Nitrogen systems, TEMPO class system, laccase system, hypochlorite system or sodium metaperiodate system.
7. preparation method according to claim 1, which is characterized in that in step 2, the sodium alginate and oxidized fibre
The mass ratio of element is 1:0.1~20.
8. preparation method according to claim 1, which is characterized in that in step 3, the mass ratio of the ethyl alcohol and water is
1:1~99.
9. preparation method according to claim 1, which is characterized in that in step 4, the molecular weight of chitosan is 50,000
~40 ten thousand, the solvent of chitosan solution is acetic acid/water solution, and the volume ratio of acetic acid and water is 0.5~5%.
10. degradable medical antibacterial leakage protection film made from -9 any preparation methods according to claim 1.
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Cited By (3)
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| CN110585485A (en) * | 2019-10-29 | 2019-12-20 | 湖南师范大学 | Novel bamboo fiber/hydroxyapatite/chitosan composite membrane and preparation method thereof |
| CN112618777A (en) * | 2020-12-24 | 2021-04-09 | 无锡中科光远生物材料有限公司 | Alginic acid biological membrane and preparation method thereof |
| CN113082299A (en) * | 2021-03-18 | 2021-07-09 | 浙江农林大学 | Degradable porous PVA/starch biological membrane and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110585485A (en) * | 2019-10-29 | 2019-12-20 | 湖南师范大学 | Novel bamboo fiber/hydroxyapatite/chitosan composite membrane and preparation method thereof |
| CN112618777A (en) * | 2020-12-24 | 2021-04-09 | 无锡中科光远生物材料有限公司 | Alginic acid biological membrane and preparation method thereof |
| CN113082299A (en) * | 2021-03-18 | 2021-07-09 | 浙江农林大学 | Degradable porous PVA/starch biological membrane and preparation method thereof |
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Application publication date: 20190621 |