CN105457076A - Chitosan oligosaccharide-nano-silver antimicrobial dressing and preparing method thereof - Google Patents

Chitosan oligosaccharide-nano-silver antimicrobial dressing and preparing method thereof Download PDF

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CN105457076A
CN105457076A CN201510890699.8A CN201510890699A CN105457076A CN 105457076 A CN105457076 A CN 105457076A CN 201510890699 A CN201510890699 A CN 201510890699A CN 105457076 A CN105457076 A CN 105457076A
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oligochitosan
chitosan
nano
silver
prepared
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Inventor
李沉纹
卢来春
王庆
崔欢欢
吴国菻
胡大强
向明凤
徐靖
宋宏宇
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Third Military Medical University TMMU
Third Affiliated Hospital of TMMU
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Third Affiliated Hospital of TMMU
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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
    • A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
    • A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
    • A61L15/18—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing inorganic 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
    • A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
    • A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
    • A61L15/22—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing macromolecular materials
    • A61L15/225—Mixtures of macromolecular compounds
    • 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
    • A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
    • A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
    • A61L15/42—Use of materials characterised by their function or physical properties
    • A61L15/46—Deodorants or malodour counteractants, e.g. to inhibit the formation of ammonia or bacteria
    • 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
    • A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
    • A61L2300/10—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing inorganic materials
    • A61L2300/102—Metals or metal compounds, e.g. salts such as bicarbonates, carbonates, oxides, zeolites, silicates
    • A61L2300/104—Silver, e.g. silver sulfadiazine
    • 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
    • A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
    • A61L2300/40—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a specific therapeutic activity or mode of action
    • A61L2300/404—Biocides, antimicrobial agents, antiseptic agents

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  • Health & Medical Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Epidemiology (AREA)
  • Hematology (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • Inorganic Chemistry (AREA)
  • Materials For Medical Uses (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)

Abstract

The invention relates to nano-silver antimicrobial dressing. A preparing method of the dressing includes the following steps that 1, a chitosan oligosaccharide-nano-silver composition is prepared; 2, the chitosan oligosaccharide-nano-silver antimicrobial dressing is prepared by the adoption of the electrospinning technology. Chitosan oligosaccharide is prepared through the following method including the steps that a chitosan acetic acid solution is prepared, wherein 70-90g of chitosan is dissolved in 1.5-3.5 L of a 2% acetic acid; hydrogen peroxide is added into the prepared chitosan acetic acid solution by a mass ratio of the chitosan acetic acid; hydrogen peroxide=(25-30):(3-4) for treatment; at the temperature of 70 DEG C, a treated product is hydrolyzed for 80-100 min, vacuum concentration is carried out at the temperature of 40 DEG C-60 DEG C, and solid matter obtained through suction filtration is neutralized with NaOH, and freeze-dried at vacuum to obtain chitosan oligosaccharide powder. The prepared chitosan oligosaccharide-nano-silver antimicrobial dressing is high in biosecurity and antimicrobial activity, good in air permeability, capable of accelerating wound healing, promoting tissue repairing and regeneration and capable of being widely applied to infectious wounds.

Description

A kind of oligochitosan-nano silver antibiotic dressing and preparation method thereof
Invention field
The present invention relates to a kind of dressing and preparation method thereof, specifically relate to a kind of oligochitosan-nano silver antibiotic dressing and preparation method thereof.
Background technology
Dressing is because having protection, absorbing exudate, suppressing external infected by microbes and promote the functions such as skin healing and be widely used in wound surface nursing.Wound dressing should possess bio-compatibility and biological degradability, can wound healing, can absorb unnecessary exudate and swelling, has the characteristics such as high porosity and breathability.But traditional dressing materials such as binder, cotton yarn, lint, non-woven fabrics etc., except Swelling Capacity and breathability can not meet the demands, also do not possess the characteristics such as treatment and wound repairing, therefore far can not meet the requirement of wound care.
Its structure of nano fibrous membrane prepared by electrostatic spinning technique and n cell are organized close, have that specific surface area is large, good permeability, moisture retention strong, can the advantage such as wound healing, thus very applicablely make Wound dressing.Have been reported the electrostatic spinning technique that to be combined with polyvinyl alcohol (PVA) by oligochitosan (COS) improves nanofiber uniformity for the preparation of nanofiber dressing.(PVA) as a kind of biodegradable resin, be widely used in biomedical materials field, the PVA nanofiber adopting electrostatic spinning technique to prepare can be used for wound surface nursing.Oligochitosan (COS) is the oligomer that chitosan generates through hydrolysis, this quasi-oligomer has higher dissolubility, good biocompatibility, there is the characteristics such as antibacterial, hemostasis, antiinflammatory, promotion blood coagulation and wound healing, the network structure of wound tissue can be increased, strengthen wound tensile strength, can activating macrophage, produce somatomedin such as TGF-β 1 grade, promote that fibroblast proliferation and collagen are formed, thus wound healing.It is high that nano silver particles (AgNP) has safety, antibacterial range is wide, the Continuous sterilization time is long, the advantages such as the strong surface area of penetration power is large, can fully contact comprehensively and attack pathogen, thus play stronger biological effect, simultaneously, compared with other antibiotic, nanometer silver has spectrum antibacterial effect and the advantage such as to have no drug resistance.The comprehensive above-mentioned fact, in the nanofiber containing oligochitosan (COS) and polyvinyl alcohol (PVA), be incorporated into nano silver particles AgNP will become a kind of Wound dressing material of tool prospect.
" InternationalJournalofNanomedicine " International Periodicals discloses " nanometer silver/oligochitosan/polyvinyl alcohol nano is as the preclinical study of antiseptic dressing ".This research for carrier with polyvinyl alcohol (PVA), has been prepared a kind of nano fibrous membrane PVA/COS-AgNP containing nano silver particles by electrostatic spinning technique and has been used as antiseptic dressing.Find that prior art mainly exists following 2 point defects with analysis after deliberation: although 1 polyvinyl alcohol (PVA) has been widely used in producing nano-fiber medical dressing, containing potential sensitization composition; 2, the commercially available oligochitosan weight average molecular weight that the nanofiber that prepared by prior art adopts is at more than 3000Da, there is molecular weight higher, the shortcoming that molecular weight distributing index is wide, the nanofiber causing it to prepare is partially long, silver particles granule is bigger than normal, water absorption and the breathability of made dressing are not good enough, cannot better meet medical requirement.
Summary of the invention
For overcoming the deficiencies in the prior art, the invention provides a kind of preparation method of oligochitosan-nanometer silver Wound dressing of improvement.
The technical scheme realizing the object of the invention is as follows:
A kind of method preparing nano silver antibiotic dressing provided by the invention, described dressing comprises the oligochitosan-nano-ag composite obtained by oligochitosan and silver nitrate, and its improvements are that described oligochitosan is what prepare by the following method:
1) chitosan-acetic acid solution is prepared:
70-90g chitosan is dissolved in the acetum of 2% of 1.5-3.5L;
2) in step 1) add the hydrogen peroxide treatment counted in mass ratio in the chitosan-acetic acid solution prepared:
Chitosan-acetic acid solution: hydrogen peroxide=25 ~ 30:3 ~ 4;
3) at 70 DEG C, by step 2) process product hydrolysis 80-100min, 40-60 DEG C at vacuum concentration, in the solid content NaOH of sucking filtration and after, vacuum lyophilization obtains described oligochitosan powder.
In first optimal technical scheme provided by the invention, the preparation method of described oligochitosan-nano-ag composite comprises the steps:
1) nanometer silver-oligochitosan complex is prepared:
Under stirring, at 30-80 DEG C, reacted by the silver nitrate solution of oligochitosan described in 0.5-2.0g and 0.1M, use acetone and washing with alcohol successively, at 100 DEG C, vacuum drying 24h obtains nanometer silver-oligochitosan complex;
2) nanometer silver-oligochitosan complex spinning liquid is prepared:
Under room temperature, nanometer silver-oligochitosan complex described in 3-5 mass parts is by mass percentage mixed with the polyvidone of the 95-97 mass parts of 30-50% (w/v);
3) electrostatic spinning: under voltage 10-20KV, 0.2-0.6mL/h flow velocity and 9-16cm receiving range, with syringe to step 2) obtained spinning liquid spinning, the oligochitosan obtained-nanometer silver nanofiber;
4) nano silver antibiotic dressing is obtained through 60Coradiation sterilizing.
In second optimal technical scheme provided by the invention,
1) described step 1) in:
70-80g chitosan is dissolved in the acetum of 2% of 2.0-3.5L;
2) described step 2) in: chitosan-acetic acid solution: hydrogen peroxide=25:4.
In 3rd optimal technical scheme provided by the invention, described step 1) in: acetum 80g chitosan being dissolved in 2% of 2.5L; Described step 2) in: chitosan-acetic acid solution: hydrogen peroxide=28:3.
In 4th optimal technical scheme provided by the invention, described step 3) in, after hydrolysis 90-100min, vacuum concentration at 40-50 DEG C, sucking filtration, in solid content NaOH and after, vacuum lyophilization obtains described oligochitosan powder.
In 5th optimal technical scheme provided by the invention, described hydrolysis time is vacuum concentration at 95-100min, 45-50 DEG C.
In 6th optimal technical scheme provided by the invention, described step 1) in, obtained 1.0-2.0g oligochitosan and the silver nitrate solution of 0.1M react at 70-80 DEG C; Described step 3) in, voltage 15-20KV and 0.2-0.4mL/h flow velocity.
In 7th optimal technical scheme provided by the invention, the volume of described acetone is 40 ~ 80mL.
In 8th optimal technical scheme provided by the invention, described fibre diameter 100nm; Nano-Ag particles particle diameter 10nm,
In 9th optimal technical scheme provided by the invention, the weight average molecular weight of described oligochitosan is 1000 ~ 2000.
With immediate prior art ratio, technical scheme provided by the invention has following excellent effect:
1. the Wound dressing preparation method prepared of the present invention, except the aspect of choosing of the weight average molecular weight from the preparation method of oligochitosan, oligochitosan has been done and improved preparation aspect that is outer, electrostatic spinning liquid and done outside improvement, its fibre diameter 100nm, significantly lower than the fibre diameter 130nm of described immediate prior art, therefore nanofiber distribution is more even; Nano-Ag particles diameter 10nm, compared to existing technology nano-Ag particles diameter 15.7nm, less nano-Ag particles contributes to nano-particle evenly be attached on nanofiber.
2. the Wound dressing that prepared by the present invention has good fungistatic effect (inhibition zone reaches 10 ~ 25mm) to gram positive bacteria and negative bacterium (staphylococcus aureus, micrococcus scarlatinae, Pseudomonas aeruginosa, escherichia coli);
3. the antiseptic dressing that prepared by the present invention has the advantages that swellability is high, breathability is strong: swelling ratio reaches 652% ~ 706%, and breathability reaches 10.86 ~ 12.04 × 10 -6gh -1cm -3mmHg -1, antiseptic dressing prepared by the present invention is all significantly increased in breathability and swelling ratio.
4. Wound dressing provided by the invention is to human normal cell, as L929 (human skin fibroblast), does not have toxicity (it is suitable with blank group that mtt assay detects 24h cell survival rate);
5. Wound dressing provided by the invention can accelerate rat machinery wound healing, at the 7th day healing percentage rate height 20-28%.
Accompanying drawing explanation
The SEM photo of the oligochitosan-nano silver antibiotic dressing of Fig. 1 prepared by the embodiment of the present invention 1;
The TEM photo of the oligochitosan-nano silver antibiotic dressing of Fig. 2 prepared by the embodiment of the present invention 1;
Fig. 3 is the result of embodiment of the present invention 1-3 cytotoxicity test;
Fig. 4 is Rat Wound Healing test photo, is from left to right followed successively by the healing state of wound surface after blank group, embodiment 1 and the antiseptic dressing process prepared by embodiment 3.
Detailed description of the invention
Be described in further detail specific embodiment below in conjunction with accompanying drawing 1-4, be clearly and completely described technical scheme of the present invention, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
Embodiment 1
Prepare oligochitosan: acetum 70g chitosan powder body being dissolved in 2% of 1.75L, according to mass ratio meter, chitosan-acetic acid solution: the ratio of hydrogen peroxide=25:3 adds hydrogen peroxide, vacuum concentration at 40 DEG C is hydrolyzed after 80min at 70 DEG C, sucking filtration, obtains oligochitosan powder with final vacuum lyophilization in solid content NaOH.
Prepare oligochitosan-nano-ag composite: take 0.5g oligochitosan powder, add the silver nitrate solution of 20mL0.1mol/L, stirring reaction 4h at 30 DEG C.Add 40mL acetone precipitation product, washing with alcohol, at 100 DEG C after vacuum drying 24h and get final product.
Prepare oligochitosan-nano silver antibiotic dressing:
By obtained 0.5g nanometer silver-oligochitosan complex, add in 10g30% (w/v=300g/L) polyvidone, divide after being uniformly mixed and add in syringe needle, use electrostatic spinning machine spinning.Spinning parameter: voltage 12KV, flow velocity 0.2mL/h, receiving range 10cm.The oligochitosan obtained-nanometer silver nanofiber is cut to 3cm × 3cm, with 3KGy absorbed dose through 60Coradiation sterilizing and get final product.
Test the oligochitosan-nano silver antibiotic dressing product prepared by the present embodiment by SEM, its structure as shown in Figure 1.As seen from the figure, antiseptic dressing nanofiber is evenly distributed, and diameter is about 100nm.
Test the oligochitosan-nano silver antibiotic dressing product prepared by the present embodiment by TEM, its structure as shown in Figure 2.As seen from the figure, nanometer silver is attached on fiber equably, and particle diameter is about 10nm.
Embodiment 2
The preparation of oligochitosan: acetum 70g chitosan powder body being dissolved in 2% of 1.75L, count in mass ratio, chitosan-acetic acid solution: the amount of hydrogen peroxide=25:3 adds hydrogen peroxide, vacuum concentration at 40 DEG C is hydrolyzed after 80min at 70 DEG C, with NaOH neutralization after sucking filtration, vacuum lyophilization obtains water-soluble chitosan oligosaccharide powder.
Prepare oligochitosan-nano-ag composite:
0.5g oligochitosan is added in the silver nitrate solution of 30mL0.1mol/L, after stirring and dissolving, 60 DEG C of stirring reaction 5h.Add 40mL acetone precipitation product, washing with alcohol product, namely 100 DEG C of vacuum drying 24h obtain oligochitosan-nano-ag composite.
Prepare oligochitosan-nano silver antibiotic dressing:
0.5g nanometer silver-oligochitosan complex is added in 10g40% (w/v=400g/L) polyvidone, adds after being uniformly mixed in syringe needle, spinning in electrostatic spinning machine.Spinning parameter: voltage 13KV, flow velocity 0.2mL/h, receiving range 12cm.The oligochitosan obtained-nanometer silver nanofiber is cut to 3cm × 3cm, with 3KGy absorbed dose through 60Coradiation sterilizing and get final product.
Embodiment 3
The preparation of oligochitosan: 80g chitosan powder body is dissolved in the acetum of 2% of 1.75L, according to mass ratio range, chitosan-acetic acid solution: the amount of hydrogen peroxide=25:3 adds hydrogen peroxide, vacuum concentration at 40 DEG C is hydrolyzed after 80min at 70 DEG C, sucking filtration, finally with NaOH neutralization, then vacuum lyophilization obtains water-soluble chitosan oligosaccharide powder.
The preparation of oligochitosan-nano-ag composite: 0.5g oligochitosan is added in the silver nitrate solution of 30mL0.1mol/L, 50mL acetone precipitation product is added after stirring reaction 5h at 60 DEG C, washing with alcohol product, at 100 DEG C, namely vacuum drying 24h obtains oligochitosan-nano-ag composite.
The preparation of oligochitosan-nano silver antibiotic dressing: 0.5g nanometer silver-oligochitosan complex is added in 10g40% (w/v=400g/L) polyvidone, adds after being uniformly mixed in syringe needle, spinning in electrostatic spinning machine.Spinning parameter: voltage 14KV, flow velocity 0.2mL/h, receiving range 12cm.The oligochitosan obtained-nanometer silver nanofiber is cut to 3cm × 3cm, namely obtains oligochitosan-nano-ag composite in 3KGy absorbed dose through 60Coradiation sterilizing.
Embodiment 4
The preparation of oligochitosan: 80g chitosan powder body is dissolved in the acetum of 2% of 1.75L, according to mass ratio range, chitosan-acetic acid solution: the amount of hydrogen peroxide=25:3 adds hydrogen peroxide, vacuum concentration at 40 DEG C is hydrolyzed after 80min at 70 DEG C, sucking filtration, finally with NaOH neutralization, then vacuum lyophilization obtains water-soluble chitosan oligosaccharide powder.
The preparation of oligochitosan-nano-ag composite: 0.5g oligochitosan is added in the silver nitrate solution of 30mL0.1Mol/L, stirring reaction 6h at 60 DEG C.Add 50mL acetone precipitation product, washing with alcohol, namely 100 DEG C of vacuum drying 24h obtain oligochitosan-nano-ag composite.
The preparation of oligochitosan-nano silver antibiotic dressing: 0.5g nanometer silver-oligochitosan complex is added in 10g40% (w/v=400g/L) polyvidone, adds after being uniformly mixed in syringe needle, electrostatic spinning machine spinning.Spinning parameter: voltage 15KV, flow velocity 0.3mL/h, receiving range 12cm.The oligochitosan obtained-nanometer silver nanofiber is cut to 3cm × 3cm, namely obtains oligochitosan-nano-ag composite in 3KGy absorbed dose through 60Coradiation sterilizing.
Embodiment 5
The preparation of oligochitosan: 80g chitosan powder body is dissolved in the acetum of 2% of 2.0L, according to mass ratio meter, chitosan-acetic acid solution: the amount of hydrogen peroxide=25:4 adds hydrogen peroxide, after being hydrolyzed 90min at 70 DEG C, vacuum concentration at 50 DEG C again, sucking filtration, finally with NaOH neutralization, then vacuum lyophilization obtains water-soluble chitosan oligosaccharide powder.
The preparation of oligochitosan-nano-ag composite: 1.0g oligochitosan is added in the silver nitrate solution of 30mL0.1Mol/L, stirring reaction 6h at 60 DEG C.Add 55mL acetone precipitation product, washing with alcohol product, namely 100 DEG C of vacuum drying 24h obtain oligochitosan-nano-ag composite.
The preparation of oligochitosan-nano silver antibiotic dressing: 0.4g nanometer silver-oligochitosan complex is added in 10g40% (w/v=400g/L) polyvidone, adds after being uniformly mixed in syringe needle, electrostatic spinning machine spinning.Spinning parameter: voltage 15KV, flow velocity 0.3mL/h, receiving range 14cm.The oligochitosan obtained-nanometer silver nanofiber is cut to 3cm × 3cm, in 3KGy absorbed dose through 60Coradiation sterilizing and get final product.
Embodiment 6
The preparation of oligochitosan: 85g chitosan powder body is dissolved in the acetum of 2% of 2.0L, according to mass ratio range, chitosan-acetic acid solution: the amount of hydrogen peroxide=25:4 adds hydrogen peroxide, vacuum concentration at 50 DEG C is again hydrolyzed after 90min at 70 DEG C, sucking filtration, finally with NaOH neutralization, then vacuum lyophilization obtains water-soluble chitosan oligosaccharide powder.
The preparation of oligochitosan-nano-ag composite: obtained 1.0g oligochitosan is added in the silver nitrate solution of 30mL0.1Mol/L, after stirring and dissolving, stirring reaction 6h at 70 DEG C.Add 55mL acetone precipitation product, washing with alcohol product, namely 100 DEG C of vacuum drying 24h obtain oligochitosan-nano-ag composite.
The preparation of oligochitosan-nano silver antibiotic dressing: 0.4g nanometer silver-oligochitosan complex is added in 10g40% (w/v=400g/L) polyvidone, adds after being uniformly mixed in syringe needle, electrostatic spinning machine spinning.Spinning parameter: voltage 15KV, flow velocity 0.3mL/h, receiving range 14cm.The oligochitosan obtained-nanometer silver nanofiber is cut to 3cm × 3cm, namely obtains oligochitosan-nano-ag composite in 3KGy absorbed dose through 60Coradiation sterilizing.
Embodiment 7
The preparation of oligochitosan: 85g chitosan powder body is dissolved in the acetum of 2% of 2.2L, according to mass ratio range, chitosan-acetic acid solution: the amount of hydrogen peroxide=25:4 adds hydrogen peroxide, vacuum concentration at 50 DEG C be again hydrolyzed 90min at 70 DEG C after, sucking filtration, finally with NaOH neutralization, then vacuum lyophilization obtains water-soluble chitosan oligosaccharide powder.
The preparation of oligochitosan-nano-ag composite: obtained 1.0g oligochitosan is added in the silver nitrate solution of 40mL0.1Mol/L, after stirring and dissolving, stirring reaction 6h at 70 DEG C.Add 55mL acetone precipitation product, washing with alcohol product, 100 DEG C of vacuum drying 24h and get final product.
The preparation of oligochitosan-nano silver antibiotic dressing: take 0.4g nanometer silver-oligochitosan complex, adds in 10g45% (w/v=450g/L) polyvidone, is uniformly mixed; Said components is added in syringe needle, in electrostatic spinning machine, carry out spinning.Spinning parameter: voltage 15KV, flow velocity 0.4mL/h, receiving range 14cm.The oligochitosan obtained-nanometer silver nanofiber is cut to 3cm × 3cm, in 3KGy absorbed dose through 60Coradiation sterilizing and get final product.
Embodiment 8
The preparation of oligochitosan: 85g chitosan powder body is dissolved in the acetum of 2% of 2.2L, according to mass ratio meter, chitosan-acetic acid solution: the amount of hydrogen peroxide=25:4 adds hydrogen peroxide, at 70 DEG C of hydrolysis 90min, then at 50 DEG C of vacuum concentration, sucking filtration, finally with NaOH neutralization, then vacuum lyophilization obtains water-soluble chitosan oligosaccharide powder.
The preparation of oligochitosan-nano-ag composite: take 1.0g oligochitosan, adds the silver nitrate solution of 40mL0.1Mol/L, after stirring and dissolving, and 70 DEG C of stirring reaction 7h.Add 60mL acetone precipitation product, washing with alcohol product, 100 DEG C of vacuum drying 24h and get final product.
The preparation of oligochitosan-nano silver antibiotic dressing: take 0.4g nanometer silver-oligochitosan complex, adds in 10g45% (w/v=450g/L) polyvidone, is uniformly mixed; Said components is added in syringe needle, in electrostatic spinning machine, carry out spinning.Spinning parameter: voltage 15KV, flow velocity 0.4mL/h, receiving range 15cm.The oligochitosan obtained-nanometer silver nanofiber is cut to 3cm × 3cm, in 3KGy absorbed dose through 60Coradiation sterilizing and get final product.
Embodiment 9
The preparation of oligochitosan: 90g chitosan powder body is dissolved in the acetum of 2% of 2.3L, according to mass ratio meter, chitosan-acetic acid solution: the amount of hydrogen peroxide=25:4 adds hydrogen peroxide, vacuum concentration at 60 DEG C again after lower 70 DEG C of hydrolysis 100min, sucking filtration, finally with NaOH neutralization, then vacuum lyophilization obtains the water-soluble chitosan oligosaccharide powder of weight average molecular weight 2000.
The preparation of oligochitosan-nano-ag composite: 1.5g oligochitosan is added in the silver nitrate solution of 40mL0.1Mol/L, after stirring and dissolving, stirring reaction 7h at 70 DEG C.Add 60mL acetone precipitation product, washing with alcohol product, 100 DEG C of vacuum drying 24h and get final product.
The preparation of oligochitosan-nano silver antibiotic dressing: 0.3g nanometer silver-oligochitosan complex is added in 10g50% (w/v=500g/L) polyvidone, adds after being uniformly mixed in syringe needle, electrostatic spinning machine spinning.Spinning parameter: voltage 20KV, flow velocity 0.4mL/h, receiving range 15cm.The oligochitosan obtained-nanometer silver nanofiber is cut to 3cm × 3cm, in 3KGy absorbed dose through 60Coradiation sterilizing and get final product.
Embodiment 10
The preparation of oligochitosan: 90g chitosan powder body is dissolved in the acetum of 2% of 2.5L, according to mass ratio meter, chitosan-acetic acid solution: the amount of hydrogen peroxide=28:3 adds hydrogen peroxide, be hydrolyzed 100min at 70 DEG C after, again in lower 60 DEG C of vacuum concentration, sucking filtration, finally with NaOH neutralization, vacuum lyophilization obtains the water-soluble chitosan oligosaccharide powder of weight average molecular weight 1000.
The preparation of oligochitosan-nano-ag composite: the silver nitrate solution obtained 1.5g oligochitosan being added 40mL0.1Mol/L, after stirring and dissolving, 80 DEG C of stirring reaction 8h.Add 60mL acetone precipitation product, washing with alcohol product, 100 DEG C of vacuum drying 24h and get final product.
The preparation of oligochitosan-nano silver antibiotic dressing: 0.3g nanometer silver-oligochitosan complex is added in 10g50% (w/v=500g/L) polyvidone, adds after being uniformly mixed in syringe needle, electrostatic spinning machine spinning.Spinning parameter: voltage 20KV, flow velocity 0.5mL/h, receiving range 16cm.The oligochitosan obtained-nanometer silver nanofiber is cut to 3cm × 3cm, in 3KGy absorbed dose through 60Coradiation sterilizing and get final product.
Embodiment 11
The preparation of oligochitosan: 90g chitosan powder body is dissolved in the acetum of 2% of 2.5L, according to mass ratio meter, chitosan-acetic acid solution: the amount of hydrogen peroxide=28:4 adds hydrogen peroxide, after 70 DEG C of hydrolysis 100min, vacuum concentration at 60 DEG C again, sucking filtration, finally with NaOH neutralization, then vacuum lyophilization obtains the water-soluble chitosan oligosaccharide powder of weight average molecular weight 2000.
The preparation of oligochitosan-nano-ag composite: by 2.0g oligochitosan, adds the silver nitrate solution of 40mL0.1Mol/L, after stirring and dissolving, and 80 DEG C of stirring reaction 8h.Add 60mL acetone precipitation product, washing with alcohol product, 100 DEG C of vacuum drying 24h and get final product.
The preparation of oligochitosan-nano silver antibiotic dressing: 0.3g nanometer silver-oligochitosan complex is added in 10g50% (w/v=500g/L) polyvidone, adds after being uniformly mixed in syringe needle, carry out spinning in electrostatic spinning machine.Spinning parameter: voltage 20KV, flow velocity 0.5mL/h, receiving range 16cm.The oligochitosan obtained-nanometer silver nanofiber is cut to 3cm × 3cm, in 3KGy absorbed dose through 60Coradiation sterilizing and get final product.
Embodiment 12
The preparation of oligochitosan: acetum 90g chitosan powder body being dissolved in 2% of 2.7L, according to mass ratio meter, chitosan-acetic acid solution: the amount of hydrogen peroxide=30:3 adds hydrogen peroxide, at 70 DEG C of hydrolysis 100min, then at 60 DEG C of vacuum concentration, sucking filtration, finally with NaOH neutralization, then vacuum lyophilization obtains the oligochitosan powder of water solublity weight average molecular weight 1000.
The preparation of oligochitosan-nano-ag composite: by 2.0g oligochitosan, adds the silver nitrate solution of 40mL0.1Mol/L, after stirring and dissolving, and 80 DEG C of stirring reaction 8h.Add 60mL acetone precipitation product, washing with alcohol product, 100 DEG C of vacuum drying 24h and get final product.
The preparation of oligochitosan-nano silver antibiotic dressing: by 0.3g nanometer silver-oligochitosan complex, adds in 10g50% (w/v=500g/L) polyvidone, adds in syringe needle after being uniformly mixed, spinning in electrostatic spinning machine.Spinning parameter: voltage 20KV, flow velocity 0.5mL/h, receiving range 16cm.The oligochitosan obtained-nanometer silver nanofiber is cut to 3cm × 3cm, in 3KGy absorbed dose through 60Coradiation sterilizing and get final product.
Embodiment 13
The preparation of oligochitosan: 90g chitosan powder body is dissolved in the acetum of 2% of 2.7L, according to mass ratio meter, chitosan-acetic acid solution: the amount of hydrogen peroxide=30:4 adds hydrogen peroxide, be hydrolyzed 100min at 70 DEG C after, vacuum concentration at 60 DEG C again, sucking filtration, finally with NaOH neutralization, then vacuum lyophilization obtains the water-soluble chitosan oligosaccharide powder of weight average molecular weight 1000.
The preparation of oligochitosan-nano-ag composite: by 2.0g oligochitosan, adds the silver nitrate solution of 40mL0.1Mol/L, after stirring and dissolving, and 80 DEG C of stirring reaction 8h.Add 60mL acetone precipitation product, washing with alcohol product, 100 DEG C of vacuum drying 24h and get final product.
The preparation of oligochitosan-nano silver antibiotic dressing: 0.3g nanometer silver-oligochitosan complex is added in 10g50% (w/v=500g/L) polyvidone, adds after being uniformly mixed in syringe needle, spinning in electrostatic spinning machine.Spinning parameter: voltage 20KV, flow velocity 0.5mL/h, receiving range 16cm.The oligochitosan obtained-nanometer silver nanofiber is cut to 3cm × 3cm, in 3KGy absorbed dose through 60Coradiation sterilizing and get final product.
Below by the detection of swellability, breathability, swellability and the breathability of oligochitosan-nano silver antibiotic dressing described in embodiment of the present invention 1-13 is described.Detection method is as follows: 37 DEG C by dressing in phosphate buffer (pH7.4) soak 24h, according to swelling ratio formulae discovery swelling ratio.Result is as shown in table 1.Result shows that the swelling ratio of oligochitosan-nano silver antibiotic dressing provided by the invention and breathability are significantly higher than closest to prior art.
Table 1: the swellability of oligochitosan-nano silver antibiotic dressing, breathability
The antibacterial activity of antiseptic dressing detects
Inhibition zone method is adopted to investigate oligochitosan-nano silver antibiotic dressing to the antimicrobial effect of gram positive bacteria, gram negative bacteria (staphylococcus aureus, Pseudomonas aeruginosa, escherichia coli, bacillus subtilis).Detection method is as follows: the bacterium liquid of configuration 106CFU/mL, also coating is even on LB solid medium to add 100 μ L, being that the circular Wound dressing of 1cm is affixed on solid medium being cut into diameter, putting into biochemical cultivation case 37 DEG C and cultivating 24h, observing the size of inhibition zone.The anti-bacterial result is as shown in table 2, finds do not have antibacterial activity containing the Wound dressing of nanometer silver, and adds three groups of samples of nanometer silver, can be observed obvious inhibition zone.Antibacterial experiment in vitro shows that oligochitosan-nano silver antibiotic dressing all has stronger inhibitory action to wound surface encountered pathogenic bacteria growing.
The inhibition zone testing result (unit: mm) of table 2 oligochitosan-nano silver antibiotic dressing of the present invention
The cytotoxicity of antiseptic dressing detects
Adopt mtt assay test oligochitosan-nano silver antibiotic dressing to the safety of human normal cell.Detection method is as follows: collect logarithmic (log) phase L929 (human skin fibroblast) cell, adjustment concentration of cell suspension is 1 × 105/mL, every hole adds 100 μ L, and bed board makes cell to be measured adjust density to 1000 hole (the aseptic PBS of edge hole fills).5%CO 2, hatch for 37 DEG C, be paved with (96 hole flat underside) at the bottom of hole to cell monolayer, what add embodiment 1-3 is cut into the circular Wound dressing that diameter is 1cm, and often group adds and establishes 5 multiple holes.5%CO 2, hatch 24 hours for 37 DEG C, observe under inverted microscope.Every hole adds 20 μ LMTT solution (5mg/ml, i.e. 0.5%MTT), continues to cultivate 4h.Stop cultivating, carefully suck culture fluid in hole.Every hole adds 150ul dimethyl sulfoxide, puts low-speed oscillation 10min on shaking table, crystal is fully dissolved.The light absorption value in each hole is measured at enzyme-linked immunosorbent assay instrument OD490nm place.Zeroing hole (culture medium, MTT, dimethyl sulfoxide) is set simultaneously, control wells (the dressing dissolve medium of cell, same concentrations, culture fluid, MTT, dimethyl sulfoxide).As shown in Figure 3, compared with blank group, the equal well-grown of cell of embodiment 1-3 group, does not demonstrate cytotoxicity to result.Result shows, oligochitosan-nano silver antibiotic dressing provided by the invention does not have toxicity to human normal cell, and biological safety is good.
Adopt rat wound model test oligochitosan-nano silver antibiotic dressing to the facilitation of wound healing.Detection method is as follows: SD rat back sets up the circular skin trauma model that diameter is 1cm.Give the Wound dressing of blank's example, embodiment 1 and embodiment 3 respectively, then fixed with nonirritant adhesive plaster and binder.Within 0,7,14 day, wound diameter is observed after causing injury.Result shows, and after causing injury 7 days, compared with blank's example 1, embodiment 1 dressing can produce better wound healing effect, and result as shown in Figure 4.
Not containing nanometer silver in blank's example 1.
Just the specific embodiment of the present invention of above description, the present invention is not limited thereto.Those of ordinary skill in the field read description can to before described detailed description of the invention make an amendment, within the protection domain of the claim that these amendments are all awaited the reply in application.

Claims (10)

1. prepare a method for nano silver antibiotic dressing, described dressing comprises the oligochitosan-nano-ag composite obtained by oligochitosan and silver nitrate, and it is characterized in that, described oligochitosan is what obtain by the following method:
1) chitosan-acetic acid solution is prepared:
70-90g chitosan is dissolved in the acetum of 2% of 1.5-3.5L;
2) in step 1) add the hydrogen peroxide counted in mass ratio in the chitosan-acetic acid solution prepared and process:
Chitosan-acetic acid solution: hydrogen peroxide=25 ~ 30:3 ~ 4;
3) at 70 DEG C, by step 2) process product hydrolysis 80-100min, 40-60 DEG C at vacuum concentration, in the solid content NaOH of sucking filtration gained and after, vacuum lyophilization obtains described oligochitosan powder.
2. a kind of method preparing nano silver antibiotic dressing according to claim 1, is characterized in that, the preparation method of described oligochitosan-nano-ag composite comprises the steps:
1) nanometer silver-oligochitosan complex is prepared:
Under stirring, at 30-80 DEG C, reacted by the silver nitrate solution of oligochitosan described in 0.5-2.0g and 0.1M, use acetone and washing with alcohol successively, at 100 DEG C, vacuum drying 24h obtains nanometer silver-oligochitosan complex;
2) nanometer silver-oligochitosan complex spinning liquid is prepared:
Under room temperature, nanometer silver-oligochitosan complex described in 3-5 mass parts is by mass percentage mixed with the polyvidone of the 95-97 mass parts of 30-50% (w/v);
3) electrostatic spinning: under voltage 10-20KV, 0.2-0.6mL/h flow velocity and 9-16cm receiving range, with syringe to step 2) obtained spinning liquid spinning, the oligochitosan obtained-nanometer silver nanofiber;
4) nano silver antibiotic dressing is obtained through 60Coradiation sterilizing.
3. the method preparing nano silver antibiotic dressing according to claim 1, is characterized in that,
1) described step 1) in:
70-80g chitosan is dissolved in the acetum of 2% of 2.0-3.5L;
2) described step 2) in: chitosan-acetic acid solution: hydrogen peroxide=25:4.
4. the method preparing nano silver antibiotic dressing according to claim 1, is characterized in that, described step 1) in: acetum 80g chitosan being dissolved in 2% of 2.5L; Described step 2) in: chitosan-acetic acid solution: hydrogen peroxide=28:3.
5. the method preparing nano silver antibiotic dressing according to claim 1, is characterized in that, described step 3) in, after hydrolysis 90-100min, vacuum concentration at 40-50 DEG C, sucking filtration, in solid content NaOH and after, vacuum lyophilization obtains described oligochitosan powder.
6. the method preparing nano silver antibiotic dressing according to claim 5, is characterized in that, described hydrolysis time is vacuum concentration at 95-100min, 45-50 DEG C.
7. the method preparing nano silver antibiotic dressing according to claim 2, is characterized in that, described step 1) in, obtained 1.0-2.0g oligochitosan and the silver nitrate solution of 0.1M react at 70-80 DEG C; Described step 3) in, voltage 15-20KV and 0.2-0.4mL/h flow velocity.
8. the method preparing nano silver antibiotic dressing according to claim 2, is characterized in that, the volume of described acetone is 40 ~ 80mL.
9. the method preparing nano silver antibiotic dressing according to claim 2, is characterized in that, described nanofiber diameter 100nm, nano-Ag particles particle diameter 10nm.
10. the method preparing nano silver antibiotic dressing according to claim 1, is characterized in that, the weight average molecular weight of described oligochitosan is 1000 ~ 2000.
CN201510890699.8A 2015-12-04 2015-12-04 Chitosan oligosaccharide-nano-silver antimicrobial dressing and preparing method thereof Pending CN105457076A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107802527A (en) * 2017-12-12 2018-03-16 中国药科大学 Muffin prepared using edible mushroom source combine dressing and preparation method thereof
CN108465123A (en) * 2018-03-29 2018-08-31 青岛翰兴知识产权运营管理有限公司 A kind of compound hemostatic material and preparation method thereof
CN113981617A (en) * 2021-10-18 2022-01-28 南京医科大学 Nano antibacterial material and its preparation method and use

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107802527A (en) * 2017-12-12 2018-03-16 中国药科大学 Muffin prepared using edible mushroom source combine dressing and preparation method thereof
CN108465123A (en) * 2018-03-29 2018-08-31 青岛翰兴知识产权运营管理有限公司 A kind of compound hemostatic material and preparation method thereof
CN113981617A (en) * 2021-10-18 2022-01-28 南京医科大学 Nano antibacterial material and its preparation method and use

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