CN106178079A - A kind of antibacterial chitosan dressing containing nanometer gold and preparation method thereof - Google Patents
A kind of antibacterial chitosan dressing containing nanometer gold and preparation method thereof Download PDFInfo
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- 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
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- 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
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- 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
- A61L15/28—Polysaccharides or their derivatives
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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
- 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
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- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/20—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing organic materials
- A61L2300/23—Carbohydrates
- A61L2300/232—Monosaccharides, disaccharides, polysaccharides, lipopolysaccharides
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- 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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Abstract
The present invention provides a kind of antibacterial chitosan dressing containing nanometer gold, and it is the chitosan fabric containing gold nano grain comprising and/or being attached with and have antibacterial action.The antibacterial chitosan dressing containing nanometer gold that the present invention prepares will have the broad spectrum antibacterial of excellence, without bacterial drug resistance, the antimicrobial nano gold that human body cell toxicity is little is added in chitosan dressing, it is made to have the broad spectrum antibacterial of nanometer gold concurrently and to the good promoting healing of the little effect of human body cell toxicity and chitosan, hemostasis, the biodegradable compatibility, can be used for the treatment of wounds of clinic, and treat the various traumatic infections such as various burn, scald, decubital ulcer infection, it is the most excellent a kind of medical dressing.Present invention also offers the preparation method and application of this antibacterial chitosan dressing.
Description
Technical field
The present invention relates to a kind of antibacterial chitosan dressing, particularly relate to a kind of antibacterial chitosan dressing containing nanometer gold, with
And the preparation of this antibacterial chitosan dressing and application.
Background technology
Chitosan is a kind of degradable biological compatibility material, and chitosan can provide non-protein substrate to promote in wound
Cell proliferation, tissue growth.Chitosan with positive charge, can with electronegative erythrocyte binding, promote erythrocyte aggregation and
Contribute to hemostasis.Chitosan dressing is the dressing made with biomaterial of a class excellent performance.
Simple chitosan dressing does not have preferable bactericidal effect.In chitosan dressing, add antibacterial will carry
The antibiotic property of this dressing high, more improves its function.Nanometer silver has stronger anti-microbial property, but due to the instability of nanometer silver
Property and relatively big to the toxicity of human body cell, U.S. FDA the most clearly forbids nanometer silver use in terms of medical treatment, China CFDA
The use of nanometer silver is limited at some medical aspect.
In recent years, stability is more preferably, gradually reported as the research of antibacterial the less nanometer gold of human body cell toxicity
Road.(Zhao Y, Tian Y, Cui Y, the et al.Small molecule-capped gold such as Zhao yuyun
nanoparticles as potent antibacterial agents that target gram-negative
bacteria[J].Journal of the American Chemical Society,2010,132(35):12349-
12356；Zhao Y,Chen Z,Chen Y,et al.Synergy of non-antibiotic drugs and
pyrimidinethiol on gold nanoparticles against superbugs[J].Journal of the
American Chemical Society, 2013,135 (35): 12940-12943. and Zhao Y, Ye C, Liu W, et
al.Tuning the composition of AuPt bimetallic nanoparticles for antibacterial
application[J].Angewandte Chemie International Edition,2014,53(31):8127-
8131.) the nanometer gold antibacterial of the double-component drug modification of the aminopyrimidine reported or aminopyrimidine/containing the little molecule of amino and receiving
Rice gold platinum bimetallic antibacterial has the strongest broad spectrum antibacterial, has the strongest killing action especially to Multidrug resistant bacteria, and it is to people
Somatic toxicity is well below nanometer silver, and will not produce bacterial drug resistance, is the most promising antibacterial of class.
Anna Regiel-Futyra(Regiel-Futyra A,M,Sebastian V,et
al.Development of Noncytotoxic Chitosan–Gold Nanocomposites as Efficient
Antibacterial Materials[J].ACS applied materials&interfaces,2015,7(2):1087-
1099.) nanometer gold of the chitosan complex reported also has the antibiotic property of excellence and the toxicity low to human body cell.
The nanometer gold of above-mentioned report synthesis needs dialysis treatment, and technique is more complicated, and technique needs to be simplified further；Simple
Nano-Au solution is not readily used for Wound healing and bone regeneration and the reparation of clinic, and anti-microbial property needs to be improved further.
At present, there is no what the nanometer gold that open source literature report is added with broad spectrum antibacterial and cytotoxicity is little made both at home and abroad
Antibacterial chitosan dressing.
Summary of the invention
Therefore, defect based on prior art, it is an object of the invention to provide one and there is broad spectrum antibacterial and to carefully
The antibacterial chitosan dressing containing nanometer gold that cellular toxicity is little, additionally provides the preparation of the described antibacterial chitosan dressing containing nanometer gold
Method and application thereof.
To achieve these goals, the invention provides a kind of antibacterial chitosan dressing containing nanometer gold, described antibacterial shell
Polysaccharide dressing is the chitosan fabric containing gold nano grain comprising and/or being attached with and have antibacterial action.
According to the antibacterial chitosan dressing of the present invention, wherein, described chitosan fabric can be adhesive-bonded fabric, woven fabric
Or knitting fabric.
According to the antibacterial chitosan dressing of the present invention, wherein, described described antibacterial chitosan dressing is accounted for containing gold nano grain
0.01～3 mass %, it may be preferred to be 0.01～1 mass %.
According to the antibacterial chitosan dressing of the present invention, wherein, the described mean diameter containing gold nano grain is below 50nm,
2～10nm can be preferably, such as 4～6nm.
According to the antibacterial chitosan dressing of the present invention, wherein, there is described in the nano-particle containing nanometer gold of anti-microbial property
Selected from nanometer gold, one-component or multicomponent small-molecule drug or the macromole nanometer gold modified and containing nanometer gold double groups
One or more in part or multicomponent metal nanoparticle.
Preferably, the described nanometer gold modified by one-component or multicomponent small-molecule drug or macromole is with phonetic containing amino
Nanogold particle that pyridine micromolecular is modified as one-component or using containing aminopyrimidine micromolecular/amino micromolecular as double
The nanogold particle that component is modified, the described molar content containing aminopyrimidine micromolecular and gold element ratio for 0.5:1～2:1,
The molar content of described amino micromolecular and gold element is than for 0.5:1～2:1.Most preferably, described little containing Aminopyrimidines
Molecule is 4,6-2 amino-2-mercapto phenyl formic pyrimidine, and amino micromolecular is metformin or 1-(3-chlorophenol) biguanide.
Or preferably, described double-component containing nanometer gold or multicomponent metal nanoparticle are that nanometer gold-platinum bimetallic is received
Rice grain.Most preferably, described nanometer gold-platinum duplex metal nano granule is by the gold of 80% atomic percent and 20% atomic percent
The platinum composition of ratio.
Present invention also offers the preparation method of the above-mentioned antibacterial chitosan dressing containing nanometer gold, described method includes following
Step:
(1) dissolve chitosan in acetic acid solution, obtain chitosan acetic acid solution；
(2) the chitosan acetic acid solution that nano-Au solution obtains with step (1) is mixed homogeneously, stand froth breaking, then use
Acetic acid regulation solution ph is 4.5～5.5, obtains nanometer gold chitosan spinning liquid；Described nano-Au solution is containing described tool
There is the dispersion liquid containing gold nano grain of antibacterial action；
(3) the nanometer gold chitosan spinning liquid that step (2) obtains is extruded by spinneret cap, enter in solidification liquid and coagulate
Gu, obtain the antibacterial chitin fiber containing nanometer gold；
(4) carry out the antibacterial chitin fiber containing nanometer gold that step (3) obtains stretching, being dried, obtain containing nanometer gold
Antibacterial chitosan long fibre, be then prepared as the described antibacterial chitosan dressing containing nanometer gold.
By add in chitosan spinning liquid have antibacterial action containing gold nano grain, spinning obtains containing receiving the most again
The antibacterial chitin fiber of meter Jin, is then prepared as the chitosan dressing (such as chitosan fabric) containing nanometer gold, can make to contain
Gold nano grain (it should be readily apparent to one skilled in the art that fiber surface also may be used in being distributed in chitin fiber the most securely
Can be attached with containing gold nano grain) so that chitosan fabric comprise and/or be attached with have antibacterial action containing gold nano
Grain.
The described antibacterial chitosan long fibre containing nanometer gold can be prepared as chitosan fabric by conventional means, such as nonwoven
Fabric, woven fabric or knitting fabric etc..Such as, the antibacterial chitosan long fibre containing nanometer gold is through shredding, one-tenth net, acupuncture system
Obtain adhesive-bonded fabric.
Obtained chitosan dressing can through cutting further, packing, the operation such as sterilizing prepare dressing finished product with on-demand.
The preparation method of the antibacterial chitosan dressing according to the present invention, wherein, the concentration of described acetic acid solution be 0.3～
0.9mol/L。
The preparation method of the antibacterial chitosan dressing according to the present invention, wherein, described solidification liquid comprises selected from sodium hydroxide
One or more in solution, potassium hydroxide solution and alkalescence ammoniacal solutions, preferably sodium hydroxide solution.It is highly preferred that institute
The concentration stating sodium hydroxide solution is 0.5～1.2mol/L.It is further preferred that described solidification liquid also comprises organic solvent, institute
State organic solvent and be preferably ethanol.
The preparation method of the antibacterial chitosan dressing according to the present invention, wherein, is stretched as 2～5 times described in step (4)
Stretching, described in be stretching at 60～90 DEG C and carry out.Preferably, the temperature being dried described in step (4) is 60～90 DEG C, and the time is
1～5h.
The preparation method of the antibacterial chitosan dressing according to the present invention, wherein, described nano-Au solution is by following step
Rapid prepared:
(a) according to proportioning, by chlorauric acid solution with containing aminopyrimidine micromolecular and/or the solution of amino micromolecular or
Potassium chloroplatinate solution mixes, and obtains mixed solution；
B () under agitation rapidly joins reducing agent in described mixed solution, fully i.e. obtain described nanometer gold after reaction
Solution；
Wherein, the joining day of described reducing agent is less than 5 minutes, preferably more than 1 minute, more preferably 5～60 seconds, enters
One step preferably 5～30 seconds, such as 25 seconds.
Preferably, the solution containing aminopyrimidine micromolecular and/or amino micromolecular described in step (a) can also wrap
Include organic acid or mineral acid.It is preferably acetic acid, propanoic acid or hydrochloric acid.It is highly preferred that the percent mass that acid is in described mixed solution
Ratio is 0.01%～10%.
Preferably, contain in the solution of aminopyrimidine micromolecular and/or amino micromolecular all right described in step (a)
Including nonionic surfactant.It is preferably tween or Polyethylene Glycol.It is highly preferred that nonionic surfactant is in described mixing
Mass percent in solution is 0.005～10%, preferably 0.005～0.01%.
Preferably, reducing agent described in step (b) can be selected from sodium borohydride, sodium citrate and sodium ascorbate
Plant or multiple.Described in step (b), abundant reaction temperature can be below room temperature or room temperature, such as, can be less than 25 DEG C, time
Between can be 0.5～3 hour, for example, 1 hour.
Preferably, the concentration in described nano-Au solution containing the nano-particle of nanometer gold described in step (b) be 10～
4000ppm, preferably 400～4000ppm, more preferably 800～4000ppm.It is further preferred that described reducing agent and chlorine
The mol ratio of the mol ratio of auric acid or described reducing agent and gold chloride and potassium chloroplatinate is 0.5～10:1, preferably 0.5～3:
1.Wherein, 1ppm generally can be scaled 1mg/L.
It is highly preferred that the preparation method of described nano-Au solution does not comprise the step of nano-Au solution described in purification；Enter one
Preferably, the step of nano-Au solution described in purification includes processing with bag filter dialysis treatment or centrifugal filtration step.In other words, originally
Invention production method need not carry out purified nanotubes gold solution by modes such as bag filter dialysis treatment or centrifugal filtration process.As more
Further limiting, the preparation method of above-mentioned nano-Au solution can also be expressed as being made up of step (a) and step (b).
It should be readily apparent to one skilled in the art that the gold chloride raw material used when preparing chlorauric acid solution can be four hydrations
Gold chloride.
Present invention also offers the above-mentioned antibacterial chitosan dressing containing nanometer gold or according to the method described above and prepare containing receiving
The antibacterial chitosan dressing of meter Jin is used for treating the application in the medicine that burn, scald or decubital ulcer infect in preparation.
The antibacterial chitosan dressing containing nanometer gold that the present invention prepares is by having the broad spectrum antibacterial of excellence, without bacterial resistance
Property, the antimicrobial nano gold that human body cell toxicity is little is added in chitosan dressing, makes it have the broad spectrum antibacterial of nanometer gold concurrently
And to the good promoting healing of the little effect of human body cell toxicity and chitosan, hemostasis, the biodegradable compatibility.Can be used for clinic
Treatment of wounds, and treat the various traumatic infections such as various burn, scald, decubital ulcer infection, be a kind of the most excellent medical
Dressing.And, the present invention use in chitosan spinning liquid add antimicrobial nano gold, then spinning obtain the shell containing nanometer gold gather
Sugar dressing, can make nanometer gold the most firmly be distributed in chitin fiber, and antibacterial effect is more preferably.
In the preparation method of the antimicrobial nano gold that prior art has been reported, reducing agent is to add in the way of dropping, for
Industrialized production, the dropping mode of background report is the most oversize, it is impossible to realize, and the system of the nano-Au solution provided in the present invention
In Preparation Method, reducing agent, for be disposably added rapidly to described mixed solution, the most more saves the time, contributes to promoting producing and imitates
Rate.
The nano-Au solution of background report needs with bag filter dialysis or centrifugation after completion of the reaction, for industrialization
Producing, the post-processing approach of background report is complicated, apparatus expensive.And the present invention provide nano-Au solution preparation method not
Needing dialysis or centrifugation to process, therefore technique is the simplest, reduces production cost, improves production efficiency further.
Being proved by testing inspection, the antibacterial effect of the nano-Au solution prepared by preparation method that the present invention provides is the most excellent
In reducing agent dropping and/or through the nano-Au solution prepared by dialysis treatment.The present invention provides receiving prepared by preparation method
The cytotoxicity of rice gold solution is significantly lower than nanometer silver solution and silver nitrate solution.Additionally, the present invention provide containing nanometer gold
Antibacterial chitosan dressing is compared with the nanometer gold antiseptic solution containing the same mass percent of same type, and antibacterial effect is more excellent.
Accompanying drawing explanation
Hereinafter, describe embodiment of the present invention in detail in conjunction with accompanying drawing, wherein:
Fig. 1 shows embodiment 1 nanometer gold and is purchased nanometer silver transmission electron microscope (TEM) figure；
Fig. 2 show embodiment 1 nanometer gold, be purchased nanometer silver, the cytotoxicity that is purchased silver nitrate compares.
Detailed description of the invention
The present invention is further illustrated below by specific embodiment, it should be understood, however, that, these embodiments are only
It is used for specifically describing in more detail, and is not to be construed as limiting in any form the present invention.
This part to the present invention test used in material and test method carry out general description.Although it is
Realize many materials that the object of the invention used and operational approach is to it is known in the art that but the present invention still uses up at this
May describe in detail.It will be apparent to those skilled in the art that within a context, if not specified, material therefor of the present invention and behaviour
It is well known in the art as method.
The reagent and the instrument that use in following example are as follows:
Reagent:
Instrument:
Inductively coupled plasma atomic emission spectrometer (ICP-OES)；Model iCAP 6300；It is purchased from: U.S. Thermo
Scientific company
Transmission electron microscope (TEM)；Model Tecnai G2 20S-TWIN；It is purchased from: FEI Co. of the U.S.
Embodiment 1
The present embodiment is for antibacterial chitosan dressing containing nanometer gold that the present invention is described and preparation method thereof.
(1) 50g chitosan is dissolved in the 0.90mol/L acetic acid solution of 1000mL, obtains chitosan acetic acid solution；
(2) nanometer gold that the 4,6-2 amino-2-mercapto phenyl formic pyrimidine/metformin containing 1.5g is modified as double-component
The chitosan acetic acid solution that the nano-Au solution of grain obtains with step (1) is mixed homogeneously, and stands froth breaking, then molten with acetic acid regulation
Liquid pH value is 5, obtains nanometer gold chitosan spinning liquid；
(3) the nanometer gold chitosan spinning liquid that step (2) obtains is extruded by spinneret cap, enter the hydrogen-oxygen of 1.2mol/L
Change in sodium solution and solidify, obtain the antibacterial chitin fiber containing nanometer gold；
(4) carry out the antibacterial chitin fiber containing nanometer gold that step (3) obtains stretching (2 times of stretchings at 60 DEG C),
It is dried (at 60 DEG C, being dried 5h), obtains the antibacterial chitosan long fibre containing nanometer gold, then this antibacterial chitosan long fibre is entered
Row shredding, one-tenth net, acupuncture, make the chitosan adhesive-bonded fabric containing nanometer gold, can be as the antibacterial chitosan dressing containing nanometer gold；
(5) adhesive-bonded fabric can also be cut as dressing sheet, carry out subsequently packing, sterilizing, become containing nanometer gold is antibacterial
Chitosan dressing finished product.
The preparation method of above-mentioned nano-Au solution is:
A the four hydration gold chlorides of 3g are dissolved in the deionized water of 0.75L by (), obtain chlorauric acid solution.By a certain amount of
4,6-2 amino-2-mercapto phenyl formic pyrimidines and metformin are dissolved in the deionized water of 0.75L, are additionally added a certain amount of Tween 80 and second
Acid, is completely dissolved in water helping lend some impetus to aminopyrimidine micromolecular and amino micromolecular, obtains containing Aminopyrimidines
Little molecule and/or the solution of amino micromolecular.By two solution mixing, obtain mixed solution.
B a certain amount of sodium ascorbate is dissolved in the deionized water of 0.325L by (), under agitation by above-mentioned ascorbic acid
Sodium solution rapidly join (used time 30s) in above-mentioned mixed solution, 1 hour stirred below of room temperature to fully reaction, be not required to adopt
With purifying process such as dialysis, i.e. obtain the concentration of about 1.875L be about (the calculating according to rate of charge) of 800ppm containing above-mentioned 4,
The nano-Au solution of the nanogold particle that 6-2 amino-2-mercapto phenyl formic pyrimidine/metformin is modified as double-component.
According to rate of charge, the molar content of 4,6-2 amino-2-mercapto phenyl formic pyrimidines and gold element ratio is for 2:1, metformin and gold
The molar content of element is than for 0.5:1, and the molar content of reducing agent sodium ascorbate and gold chloride is than for 0.5:1, and acetic acid accounts for be received
The mass percent of rice gold solution is 0.01%, and surface active agent tween 80 accounts for the mass percent of nano-Au solution and is
0.005%.
In this antibacterial chitosan dressing containing nanometer gold, measuring through ICP-OES, the gold content of every chitosan dressing is
3 mass %.Through 200KV lanthanum hexaboride determination of transmission electron microscopy, the mean diameter of the nanogold particle in this dressing is
5nm。
Comparative example 1
The nanometer gold antiseptic solution of comparative example 1 is prepared according to preparation method same as in Example 1, then by room temperature solvent
Evaporation of water, is configured to the nanometer gold antiseptic solution of variable concentrations, wherein, applies including with the nanometer gold chitosan in embodiment 1
Material has the nano-Au solution of identical nanometer gold weight/mass percentage composition.
Comparative example 1.1
The nanometer gold antiseptic solution of comparative example 1.1 is prepared according to the preparation method similar to comparative example 1.In comparative example 1.1
The mode of reductant solution dropping joins in reaction solution, and it is anti-to use the dialysis treatment mode of 24 hours to obtain nanometer gold
Bacterium solution, adds purified water so that it is have identical nanometer gold weight/mass percentage composition with the nanometer gold antiseptic solution in comparative example 1.
Test example 1
By the antibacterial experiment in test example 1, it was demonstrated that the nanometer gold antiseptic solution of comparative example 1 is better than comparative example 1.1
Nanometer gold antiseptic solution.Antibacterial effect is shown in Table 1.
Comparative approach is as follows: uses minimal inhibitory concentration MIC (mg/L) to weigh, uses micropore dilution process
(National Committee for Clinical Laboratory Standards., Methodsfor determining
Bactericidal activity of antimicrobial agents, M26-A, 1999.), by 100 μ L variable concentrations
The nano-Au solution of comparative example 1 and comparative example 1.1 is added separately in 96 microwell plates, 10 μ L same concentrations (104CFU/mL)
Inoculum adds in each micropore, 37 DEG C cultivate 24 hours after observe, in the micropore of the bacterial growth that not can be seen that
Few concentration is minimal inhibitory concentration (MIC).
Test result is shown in Table 1.From test result, the antibacterial effect of the nanometer gold antiseptic solution of comparative example 1 is much better than
The antibacterial effect of the nanometer gold antiseptic solution of comparative example 1.1.Illustrate to use the nano-Au solution identical with comparative example 1 preparation method
The antibacterial chitosan dressing containing nanometer gold of preparation, its antibacterial effect also should be much better than employing and comparative example 1.1 preparation method phase
Antibacterial chitosan dressing containing nanometer gold prepared by same nano-Au solution.
The anti-microbial property of the nanometer gold antiseptic solution of table 1 comparative example 1 and comparative example 1.1 compares
Embodiment 2
The present embodiment is for antibacterial chitosan dressing containing nanometer gold that the present invention is described and preparation method thereof.
(1) 30g chitosan is dissolved in the 0.30mol/L acetic acid solution of 1000mL, obtains chitosan acetic acid solution；
(2) using 4,6-2 amino-2-mercapto phenyl formic pyrimidine/1-(3-chlorophenol) biguanide containing 0.003g as the little molecule of double-component
The chitosan acetic acid solution that the nano-Au solution of the nanogold particle modified obtains with step (1) is mixed homogeneously, and stands froth breaking, so
Regulating solution ph with acetic acid afterwards is 4.5, obtains nanometer gold chitosan spinning liquid；
(3) the nanometer gold chitosan spinning liquid that step (2) obtains is extruded by spinneret cap, enter the hydrogen-oxygen of 0.5mol/L
Change in sodium solution and solidify, obtain the antibacterial chitin fiber containing nanometer gold；
(4) carry out the antibacterial chitin fiber containing nanometer gold that step (3) obtains stretching (5 times of stretchings at 90 DEG C),
It is dried (at 90 DEG C, being dried 1h), obtains the antibacterial chitosan long fibre containing nanometer gold, then this antibacterial chitosan long fibre is entered
Row shredding, one-tenth net, acupuncture, make the chitosan adhesive-bonded fabric containing nanometer gold, can be as the antibacterial chitosan dressing containing nanometer gold；
(5) adhesive-bonded fabric can also be cut as dressing sheet, carry out subsequently packing, sterilizing, become containing nanometer gold is antibacterial
Chitosan dressing finished product.
The preparation method of above-mentioned nano-Au solution is:
A the four hydration gold chlorides of 0.27g are dissolved in the deionized water of 0.067L by (), obtain chlorauric acid solution.Will be certain
The 4 of amount, 6-2 amino-2-mercapto phenyl formic pyrimidine and 1-(3-chlorophenol) biguanide are dissolved in the deionized water of 0.067L, are additionally added a certain amount of
Tween 80 and acetic acid, be completely dissolved in water helping lend some impetus to aminopyrimidine micromolecular and amino micromolecular, contained
Aminopyrimidine micromolecular and/or the solution of amino micromolecular.By two solution mixing, obtain mixed solution.
B a certain amount of sodium ascorbate is dissolved in the deionized water of 0.033L by (), under agitation by above-mentioned ascorbic acid
Sodium solution rapidly join (used time 5s) in above-mentioned mixed solution, 1 hour stirred below of room temperature to fully reaction, be not required to use
The purifying process such as dialysis, the concentration i.e. obtaining about 0.167L is about (the calculating according to rate of charge) of 800ppm containing above-mentioned 4,6-
The nano-Au solution of the nanogold particle that 2 amino-2-mercapto phenyl formic pyrimidines/1-(3-chlorophenol) biguanide is modified as double-component.
According to rate of charge, the molar content of 4,6-2 amino-2-mercapto phenyl formic pyrimidines and gold element is than for 0.5:1,1-(3-chlorophenol)
The molar content of biguanide and gold element is than for 2:1, and the molar content of reducing agent sodium ascorbate and gold chloride is than for 3:1, acetic acid
The mass percent accounting for nano-Au solution is 0.01%, and surface active agent tween 80 accounts for the mass percent of nano-Au solution and is
0.01%.
In this antibacterial chitosan dressing containing nanometer gold, measuring through ICP-OES, the gold content of every chitosan dressing is
0.01 mass %.Through 200KV lanthanum hexaboride determination of transmission electron microscopy, the mean diameter of the nanogold particle in this dressing is
6nm。
Comparative example 2
The nanometer gold antiseptic solution of comparative example 2 is prepared according to preparation method same as in Example 2, then by room temperature solvent
Evaporation of water, makes nanometer gold antiseptic solution so that it is have identical nanometer golden with the nanometer gold chitosan dressing in embodiment 2
Amount percentage composition.
Embodiment 3
The present embodiment is for antibacterial chitosan dressing containing nanometer gold that the present invention is described and preparation method thereof.
(1) 50g chitosan is dissolved in the 0.50mol/L acetic acid solution of 1000mL, obtains chitosan acetic acid solution；
(2) by the gold containing 0.5g-platinum bi-component Au80Pt20The nano-Au solution of nano-particle and step (1) obtain
Chitosan acetic acid solution mix homogeneously, stands froth breaking, and then regulating solution ph with acetic acid is 5.5, obtains nanometer gold chitosan
Spinning liquid；
(3) the nanometer gold chitosan spinning liquid that step (2) obtains is extruded by spinneret cap, enter the hydrogen-oxygen of 0.8mol/L
Change in sodium solution and solidify, obtain the antibacterial chitin fiber containing nanometer gold；
(4) carry out the antibacterial chitin fiber containing nanometer gold that step (3) obtains stretching (3 times of stretchings at 70 DEG C),
It is dried (at 70 DEG C, being dried 3h), obtains the antibacterial chitosan long fibre containing nanometer gold, then this antibacterial chitosan long fibre is entered
Row shredding, one-tenth net, acupuncture, make the chitosan adhesive-bonded fabric containing nanometer gold, can be as the antibacterial chitosan dressing containing nanometer gold；
(5) adhesive-bonded fabric can also be cut as dressing sheet, carry out subsequently packing, sterilizing, become containing nanometer gold is antibacterial
Chitosan dressing finished product.
The above-mentioned preparation method containing the nano-Au solution of nanometer gold-platinum duplex metal nano granule is:
A () is by the four hydration gold chloride (HAuCl of 0.825g4·4H2And 0.175g potassium chloroplatinate (K O)2PtCl6) be dissolved in
In the deionized water of 0.2L, obtain mixed solution.
B a certain amount of sodium borohydride is dissolved in the deionized water of 0.05L by (), under agitation by above-mentioned sodium borohydride solution
Rapidly join (used time 25s) in above-mentioned mixed solution, 1 hour stirred below of room temperature to fully reaction, be not required to use dialysis
Deng purifying process, the nanometer gold that the concentration about 800ppm i.e. obtaining about 0.25L contains nanometer gold-platinum duplex metal nano granule is molten
Liquid.
According to rate of charge, the molar content of borane reducing agent sodium hydride and gold chloride and potassium chloroplatinate is than for 3:1, the atom of platinum
Percentage ratio is 20%, and therefore this gold-Pt nanoparticle is represented by Au80Pt20Nano-particle.
In this antibacterial chitosan dressing containing nanometer gold, measuring through ICP-OES, the gold content of every chitosan dressing is
1 mass %.Through 200KV lanthanum hexaboride determination of transmission electron microscopy, the mean diameter of the nanogold particle in this dressing is
4nm。
Comparative example 3
The nanometer gold antiseptic solution of comparative example 3 is prepared according to preparation method same as in Example 3, then by room temperature solvent
Evaporation of water so that it is have identical nanometer gold weight/mass percentage composition with the nanometer gold chitosan dressing in embodiment 3.
Test example 2
The nanometer gold that 4,6-2 amino-2-mercapto phenyl formic pyrimidine/metformin embodiment 1 used is modified as double-component resists
Bacterium solution, compared with the anti-microbial property of the commercially available antiseptic solution (purchased from Zhangjiagang Nai Er nanosecond science and technology company) containing nanometer silver, is said
The antibacterial chitosan dressing containing nanometer gold of the bright present invention also should have good anti-microbial property.
Comparative approach is as follows: uses minimal inhibitory concentration MIC (mg/L) to weigh, uses micropore dilution process
(National Committee for Clinical Laboratory Standards., Methodsfor determining
Bactericidal activity of antimicrobial agents, M26-A, 1999.), by 100 μ L variable concentrations
Nanometer gold or nanometer silver join in 96 microwell plates, 10 μ L same concentrations (104CFU/mL) inoculum adds each micro-
Kong Zhong, cultivates for 37 DEG C and observes after 24 hours, nanometer gold minimum in the micropore of the bacterial growth that not can be seen that or nanometer silver
Concentration is minimal inhibitory concentration (MIC).Test result is shown in Table 2.
From test result, the 4 of embodiment 1 employing, 6-2 amino-2-mercapto phenyl formic pyrimidine/metformin is repaiied as double-component
The escherichia coli of nanometer gold antiseptic solution and the MIC of bacillus pyocyaneus of decorations are both less than the commercially available MIC containing nano-silver antiseptic solution, by
This explanation, embodiment 1 is better than the commercially available antiseptic solution containing nanometer silver to the anti-microbial property of escherichia coli and bacillus pyocyaneus.
The nano-Au solution of table 2 embodiment 1 and the anti-microbial property comparative result of the commercially available antiseptic solution containing nanometer silver
Test example 3
By the dressing Bactericidal test of different nanometer gold content, antibacterial chitosan dressing containing this nanometer gold is described
Bacteriostatic activity.
Test, to embodiment 1-3 and comparative example according to " medicine Micro biological Tests handbook " the 18th chapter Section 1 cup-plate method
1-3 carries out inhibition zone test.Result of the test is shown in Table 3.The inhibition zone of blank chitosan is 10mm, and inhibition zone size is chitosan sample
The original size of product, does not has fungistatic effect.
Test result is visible, although the nanometer gold mass percent of each embodiment is different with type, but all can be observed bright
Aobvious inhibition zone, illustrates that escherichia coli, staphylococcus aureus and bacillus pyocyaneus are all had good by the chitosan dressing containing nanometer gold
Good fungistatic effect.And the inhibition zone of the same type of chitosan dressing containing nanometer gold of same concentration to be all higher than nanometer gold antibacterial
Solution, illustrates that the fungistatic effect of the chitosan dressing containing nanometer gold is better than identical nanometer gold content identical nanometer gold type
Nanometer gold antiseptic solution.
Test example 4 cytotoxicity experiment
Cell toxicity test operating process: Human umbilical vein endothelial cells (HUVEC) is clear containing 10% N of fetal blood
The Eagle culture medium (DMEM) that Dulbecco improves is cultivated.10 are added in each hole of 96 microwell plates4Individual HUVEC cell,
(2-sulfydryl-4,6-di-amino-pyrimidine/metformin bi-component is modified to be separately added into the nano-particle containing variable concentrations in each hole
Nanogold particle) nano-Au solution (being available from comparative example 1), be purchased nanometer silver, be purchased silver nitrate solution 200 microlitre.Micro-
Hole medium is cultivated 48 hours at 37 DEG C, does not add the HUVEC cell of antibacterial as comparison.After having cultivated, in micropore
Solution wash once with phosphate buffer solution (PBS, 0.01mol/L, pH 7.4), add 10% (v/v) CCK-8 solution micro-
In the medium of hole, cultivate 2 hours at 37 DEG C.Various kinds sample wells and the suction of control wells is measured at enzyme-linked immunosorbent assay instrument 450nm
Light value.Calculate each sample well cell relative viability.Each sample porocyte relative activity is defined as: each hole light absorption value/comparison
Light absorption value × 100% in hole.Result of the test is shown in Fig. 2.
Knowable to the result of the test shown in Fig. 2, the present invention use containing gold nano grain cell toxicant under variable concentrations
Property all significantly lower than being purchased nanometer silver and be purchased silver nitrate solution.
Although present invention has been a certain degree of description, it will be apparent that, without departing from the spirit and scope of the present invention
Under the conditions of, the suitable change of each condition can be carried out.It is appreciated that and the invention is not restricted to described embodiment, and be attributed to right
The scope required, it includes the equivalent of described each factor.
Claims (10)
1. the antibacterial chitosan dressing containing nanometer gold, it is characterised in that described antibacterial chitosan dressing is for comprising and/or attached
The chitosan fabric containing gold nano grain with antibacterial action.
Antibacterial chitosan dressing containing nanometer gold the most according to claim 1, it is characterised in that described chitosan fabric is
Adhesive-bonded fabric, woven fabric or knitting fabric.
Antibacterial chitosan dressing containing nanometer gold the most according to claim 1 and 2, it is characterised in that described containing gold nano
Granule accounts for 0.01～3 mass % of described antibacterial chitosan dressing, preferably 0.01～1 mass %.
Antibacterial chitosan dressing containing nanometer gold the most according to any one of claim 1 to 3, it is characterised in that described
Mean diameter containing gold nano grain is below 50nm, preferably 2～10nm.
Antibacterial chitosan dressing containing nanometer gold the most according to any one of claim 1 to 4, it is characterised in that described
Have anti-microbial property containing gold nano grain selected from nanometer gold, modified by one-component or multicomponent small-molecule drug or macromole
Nanometer gold and containing one or more in the double-component of nanometer gold or multicomponent metal nanoparticle；
Preferably, the described nanometer gold modified by one-component or multicomponent small-molecule drug or macromole is with containing Aminopyrimidines
Nanogold particle that little molecule is modified as one-component or using containing aminopyrimidine micromolecular/amino micromolecular as double-component
The nanogold particle modified, the described molar content containing aminopyrimidine micromolecular and gold element ratio is for 0.5:1～2:1, described
The molar content of amino micromolecular and gold element is than for 0.5:1～2:1, most preferably, described containing aminopyrimidine micromolecular
Being 4,6-2 amino-2-mercapto phenyl formic pyrimidine, amino micromolecular is metformin or 1-(3-chlorophenol) double arcs；
Or preferably, described double-component containing nanometer gold or multicomponent metal nanoparticle are nanometer gold-platinum bimetal nano
Grain；Most preferably, described nanometer gold-platinum duplex metal nano granule is by the gold of 80% atomic percent and 20% atomic percent
Platinum forms.
6. the preparation method of the antibacterial chitosan dressing containing nanometer gold according to any one of claim 1 to 5, its feature exists
In, said method comprising the steps of:
(1) dissolve chitosan in acetic acid solution, obtain chitosan acetic acid solution；
(2) the chitosan acetic acid solution that nano-Au solution obtains with step (1) is mixed homogeneously, stand froth breaking, then use acetic acid
Regulation solution ph is 4.5～5.5, obtains nanometer gold chitosan spinning liquid；Described nano-Au solution is anti-for having described in containing
The dispersion liquid containing gold nano grain of bacterium effect；
(3) the nanometer gold chitosan spinning liquid that step (2) obtains is extruded by spinneret cap, enters in solidification liquid and solidify,
Obtain the antibacterial chitin fiber containing nanometer gold；
(4) carry out the antibacterial chitin fiber containing nanometer gold that step (3) obtains stretching, being dried, obtain resisting containing nanometer gold
Bacterium chitosan long fibre, is then prepared as the described antibacterial chitosan dressing containing nanometer gold.
The preparation method of the antibacterial chitosan dressing containing nanometer gold the most according to claim 6, it is characterised in that described second
The concentration of acid solution is 0.3～0.9mol/L；Preferably, described solidification liquid comprises selected from sodium hydroxide solution, potassium hydroxide molten
One or more in liquid and alkalescence ammoniacal solutions, preferably sodium hydroxide solution；It is highly preferred that described sodium hydroxide solution
Concentration is 0.5～1.2mol/L；It is further preferred that described solidification liquid also comprises organic solvent, described organic solvent is preferably
Ethanol.
8. according to the preparation method of the antibacterial chitosan dressing containing nanometer gold described in claim 6 or 7, it is characterised in that step
Suddenly be stretched as 2～5 times of stretchings described in (4), described in be stretching at 60～90 DEG C and carry out；Preferably, dry described in step (4)
Dry temperature is 60～90 DEG C, and the time is 1～5h.
9. according to the preparation method of the antibacterial chitosan dressing containing nanometer gold according to any one of claim 6 to 8, its feature
Being, described nano-Au solution is through the following steps that prepare:
(a) according to proportioning, by chlorauric acid solution with containing aminopyrimidine micromolecular and/or the solution of amino micromolecular or chlorine platinum
Acid solution mixes, and obtains mixed solution；
B () under agitation rapidly joins reducing agent in described mixed solution, fully both obtained described nano-Au solution after reaction；
Wherein, the joining day of described reducing agent be less than 5 minutes, preferably more than 1 minute, more preferably 5～60 seconds, further
Preferably 5～30 seconds；
Preferably, the mol ratio of described reducing agent and gold chloride or described reducing agent and gold chloride and the mol ratio of potassium chloroplatinate
It is 0.5～10:1, preferably 0.5～3:1；
It is highly preferred that the preparation method of described nano-Au solution does not comprise the step of nano-Au solution described in purification；The most excellent
Selection of land, the step of nano-Au solution described in purification includes processing with bag filter dialysis treatment or centrifugal filtration.
10. antibacterial chitosan dressing containing nanometer gold according to any one of claim 1 to 5 or use in claim 6 to 9 is appointed
One described preparation method and the antibacterial chitosan dressing containing nanometer gold prepared in preparation for treating burn, scald or decubital ulcer
Application in the medicine infected.
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| CN110292652A (en) * | 2018-03-23 | 2019-10-01 | 国家纳米科学中心 | Mercaptophenyl boronic acid activates gold nano grain, preparation method and application |
| CN111110906A (en) * | 2019-12-24 | 2020-05-08 | 西北农林科技大学 | Preparation of food functional factor modified nano antibacterial material and antibacterial membrane |
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