CN109550073A - A kind of photo-thermal anti-bacterial hydrogel dressing and preparation method thereof - Google Patents
A kind of photo-thermal anti-bacterial hydrogel dressing and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of medical material, a kind of photo-thermal anti-bacterial hydrogel dressing and preparation method thereof is disclosed.Method: (1) by tungsten disulfide ultrasonic disperse in sodium alginate soln in, mixed solution is obtained;(2) mixed solution is mixed with acrylamide, crosslinking agent, initiator, obtains pre-polymerization liquid;(3) pre-polymerization liquid is subjected to plastic, obtains photo-thermal anti-bacterial hydrogel dressing.Present invention ultrasound removing tungsten disulfide, effect for removing dispersion in sodium alginate soln is good;By being used in combination tungsten disulfide and sodium alginate and acrylamide, obtained aerogel dressing not only has excellent mechanical property, while having excellent photo-thermal antibacterial effect.Method of the invention is simple, and aerogel dressing yield is big and stablizes.
Description
Technical field
The invention belongs to the technical fields of biomaterial for medical purpose, and in particular to a kind of photo-thermal antiseptic dressing and its preparation side
Method.
Background technique
Skin is to protect internal organ from external environmental interference and the important natural barrier organ for preventing from being dehydrated in vivo, after damage
Its protection mechanism can be lost.The wound infection as caused by bacterium is one of postoperative most common complication.In case of this feelings
Condition, microorganism are easy to invade and initially form bacterium colony, so as to cause serious wound infection, hinder agglutination, or even cause
The complication of threat to life.In addition, serious wounds dehydration can interfere preferably wet healing environment and delay wound healing.Cause
This, is making great efforts to develop for protecting damaged skin from the new material that infects and be dehydrated.Traditional dry dressing such as cotton, day
So or bandage and gauze are synthesized for being initially important wound healing phase, but they are dry and cannot provide tide
Wet environment, and they are also often susceptible to adhere to dry wound surface and finally cause wound after its removal.In order to gram
These disadvantages are taken, have been grown up various wet dressings by the researcher that wet wound healing concept inspires.Wherein, it especially closes
Gel is filled the water, because they can keep moist environment in wound interface, allows gas exchanges, plays the barrier to microorganism
Effect, removes excessive exudate, has excellent biocompatibility, promotes the quick healing of wound, easily remove hurtless measure.
Conventional hydrogel is made of natural or synthetic polymer, and typically exhibits the mechanical performance of relative mistake and small
Balance-swelling ratio, which has limited their practical applications as dressing.
Dressing of the invention is aerogel dressing, has excellent elasticity and tensile property, can be bonded wound well, and
Synchronous body movement;And under the irradiation of near infrared light, good photo-thermal antibacterial effect is shown, prevents the bacterium sense of wound
Dye.The present invention causes plastic using heat, and process is simple, easy to operate, and yield is big and stablizes, excellent in mechanical performance, photo-thermal antibacterial
Effect is obvious, solves defect and deficiency of the existing technology.
Summary of the invention
In order to overcome the shortcomings and deficiencies of the prior art, the purpose of the present invention is to provide a kind of photo-thermal anti-bacterial hydrogels to apply
The preparation method of material.The present invention is obtained two-dimensional material and is uniformly dispersed by the thinned tungsten disulfide of ultrasound in sodium alginate soln
Sodium alginate soln, by heat cause, preparation doping tungsten disulfide two-dimensional material sodium alginate-acrylamide gel apply
Material.Prepared aerogel dressing has good mechanical property and good light thermal property.Aerogel dressing pair of the invention
Wound has extraordinary antibacterial effect, while having excellent biocompatibility, promotes the quick healing of wound, easily removes
Hurtless measure, and there is excellent mechanical property.
Another object of the present invention is to provide the hydrogels prepared by the above method with photo-thermal anti-microbial property
Dressing.Hydrogel of the invention has elasticity and tensile property well, can be bonded wound, and synchronous body movement well,
Under the irradiation of near infrared light, good photo-thermal antibacterial effect is shown, the bacterium infection of wound is prevented.Photo-thermal of the invention is anti-
Bacterium aerogel dressing can prevent wound postoperative infection.
In order to achieve the purpose that invention, the technical solution adopted by the present invention is that:
A kind of preparation method of photo-thermal anti-bacterial hydrogel dressing, includes the following steps:
(1) by tungsten disulfide ultrasonic disperse in sodium alginate soln, mixed solution is obtained;
(2) mixed solution is mixed with acrylamide, crosslinking agent, initiator, obtains pre-polymerization liquid;
(3) pre-polymerization liquid is subjected to plastic, obtains photo-thermal anti-bacterial hydrogel dressing.
Ultrasonic condition described in step (1) is 80~800W, and 20~100Hz, ultrasonic time is 1~100h.
The dosage of tungsten disulfide described in step (1) meets the following conditions: tungsten disulfide accounts for mixed solution gross mass
0.075%~1.5%.
The concentration of sodium alginate is 0.02wt%~5wt% in sodium alginate soln described in step (1).
Mixed solution described in step (1) specifically refers to tungsten disulfide ultrasound removing the low speed in sodium alginate soln
Centrifugation, removes unstripped material, then high speed centrifugation, disperses precipitating in sodium alginate soln again, obtains mixed solution;
The concentration of sodium alginate of the tungsten disulfide ultrasound removing in sodium alginate soln is 0.02wt%~0.2wt%;By precipitating weight
The concentration for being newly scattered in the sodium alginate soln in sodium alginate soln is 1.5wt%~4.8wt%.
The revolving speed of the low-speed centrifugal is 800-2000r/min;The ultracentrifugal revolving speed is 5000-12000r/
Min, the time of low-speed centrifugal are 10-60min, and the ultracentrifugal time is 10~60min.
The dosage of acrylamide described in step (2) is the 6%~18.7% of mixed solution and acrylamide gross mass.
Crosslinking agent described in step (2) is N, N- methylene-bisacrylamide, N hydroxymethyl acrylamide, the initiator
For ammonium persulfate or potassium peroxydisulfate.
The dosage of crosslinking agent described in step (2) is the 0.04%~1.2% of acrylamide quality;The dosage of initiator is
The 0.05%~0.2% of acrylamide quality.
The temperature of plastic described in step (3) is 40~70 DEG C, and gelation time is 1~5h.
Hydrogel described in step (3) forms in a mold, and plastic is after demoulding with a thickness of 1~3 millimeter.
The photo-thermal anti-bacterial hydrogel dressing is prepared by above-mentioned method.
Photo-thermal antibacterial effect may be implemented in the photo-thermal antiseptic dressing under the conditions of near-infrared, is used for wound dressing.
Present invention ultrasound removing tungsten disulfide, effect for removing dispersion in sodium alginate soln is good;By by curing
Tungsten and sodium alginate and acrylamide are used in combination, and obtained aerogel dressing not only has excellent mechanical property, simultaneously
With excellent photo-thermal antibacterial effect.Hydrogel of the invention has elasticity and tensile property well, can be bonded wound well
Mouthful, and synchronous body movement, under conditions of near-infrared, antibacterial prevents the bacterium infection of wound.Method of the invention is simple,
Aerogel dressing yield is big and stablizes, excellent in mechanical performance, and photo-thermal antibacterial effect is obvious.
The invention has the following advantages that
(1) aerogel dressing of the invention has excellent photo-thermal antibacterial effect, realizes the quick antibacterial of wound surface;
(2) method of the invention is simple, and cost is relatively low, can be with large scale preparation and production;
(3) aerogel dressing stable components prepared by, quickly, method safety, yield is big and stablizes, and mechanical property is excellent for sterilization
Different, photo-thermal effect is obvious, durable antibacterial effect.
Detailed description of the invention
Fig. 1 is the scanning electron microscopic picture in embodiment 1 with photo-thermal anti-bacterial hydrogel dressing;
Fig. 2 is the cyclic tension figure in embodiment 1 with photo-thermal anti-bacterial hydrogel dressing;
Fig. 3 is that sodium alginate-acrylamide gel (left side) is added and has photo-thermal in embodiment 1 under illumination condition
The optical photograph that anti-bacterial hydrogel dressing (right side) is coated with the plate of the bacterium solution after bacterium co-cultivation afterwards;
Fig. 4 is that sodium alginate-acrylamide gel (left side) is added and has photo-thermal in embodiment 2 under illumination condition
The optical photograph that anti-bacterial hydrogel dressing (right side) is coated with the plate of the bacterium solution after bacterium co-cultivation afterwards;
Fig. 5 is that sodium alginate-acrylamide gel (left side) is added and has photo-thermal in embodiment 3 under illumination condition
The optical photograph that anti-bacterial hydrogel dressing (right side) is coated with the plate of the bacterium solution after bacterium co-cultivation afterwards;
Fig. 6 is that sodium alginate-acrylamide gel (left side) is added and has photo-thermal in embodiment 4 under illumination condition
The optical photograph that anti-bacterial hydrogel dressing (right side) is coated with the plate of the bacterium solution after bacterium co-cultivation afterwards.
Specific embodiment
Below with reference to embodiment and attached drawing, the present invention is described in further detail, but embodiments of the present invention are unlimited
In this.
Embodiment 1
(1) tungsten disulfide is added in the sodium alginate soln that concentration is 0.025wt% and is mixed, it is then ultrasonic
12h (power 300W, frequency 45Hz) is centrifuged 30min with 1500 revs/min of revolving speeds, takes supernatant, then with 8000 revs/min
Clock revolving speed is centrifuged 30min, collects precipitating;Then it disperses precipitating in the sodium alginate soln that concentration is 1.5wt%, is mixed
Close solution;Tungsten disulfide concentration in mixed solution is 0.075wt%;
(2) acrylamide is added into mixed solution (acrylamide accounts for mixed solution and acrylamide gross mass
12.5%), be uniformly mixed, be added relative acrylamide's mass 0.06% crosslinking agent N, N- methylene-bisacrylamide and
0.09% thermal initiator ammonium persulfate is uniformly mixed, and obtains pre-polymerization liquid;
(3) pre-polymerization liquid is poured into 5 centimetres of length, it is 5 centimetres wide, with a thickness of in 2 millimeters of molds, the mold of pre-polymerization liquid will be poured into
Be put into baking oven, at 50 DEG C, react 2.5 hours plastics, demoulding obtain good mechanical properties with photo-thermal anti-microbial property
Aerogel dressing.
Fig. 1 is the low power scanning electron microscope (SEM) photograph in embodiment 1 with photo-thermal anti-bacterial hydrogel dressing;Fig. 2 is light in embodiment 1
The mechanical property of hot anti-bacterial hydrogel dressing is assessed, the cyclic tension figure of aerogel dressing.Fig. 3 is in embodiment 1 in illumination item
Under part, sodium alginate-acrylamide gel (left side) is added and has photo-thermal anti-bacterial hydrogel dressing (right side) afterwards and Escherichia coli
The optical photograph of the plate coating of bacterium solution after co-cultivation.
Photo-thermal anti-bacterial hydrogel dressing manufactured in the present embodiment is under conditions of illumination, antibiotic rate 100%;And alginic acid
Antibiotic rate is 0% to sodium-acrylamide gel (no tungsten disulfide) under light illumination.Two in aerogel dressing manufactured in the present embodiment
Tungsten sulfide extent of exfoliation is high, evenly dispersed in aerogel dressing matrix, and performance, which is stablized, has long acting antibiotic effect.
The mechanical experimental results of aerogel dressing manufactured in the present embodiment are as shown in table 1.
The mechanical property parameters of the aerogel dressing of 1 embodiment 1 of table preparation
Embodiment 2
(1) tungsten disulfide is added in the sodium alginate soln that concentration is 0.05wt% and is mixed, then ultrasound 10h
(power 500W, frequency 45Hz) is centrifuged 30min with 1500 revs/min of revolving speeds, takes supernatant, then turn with 8000 revs/min
Speed centrifugation 30min, collects precipitating;Then it disperses precipitating in the sodium alginate soln that concentration is 1.75wt%, is mixed
Solution;Tungsten disulfide concentration in mixed solution is 0.1wt%;
(2) acrylamide is added into mixed solution (acrylamide accounts for mixed solution and acrylamide gross mass
15%) it, is uniformly mixed, crosslinking agent N, the N- methylene-bisacrylamide and 0.09% of relative acrylamide's mass 0.06% is added
Thermal initiator ammonium persulfate, be uniformly mixed, obtain pre-polymerization liquid;
(3) pre-polymerization liquid is poured into 5 centimetres of length, it is 5 centimetres wide, with a thickness of in 2 millimeters of molds, the mold of pre-polymerization liquid will be poured into
Be put into baking oven, at 50 DEG C, react 2.5 hours plastics, demoulding obtain good mechanical properties with photo-thermal anti-microbial property
Aerogel dressing.Fig. 4 is that sodium alginate-acrylamide gel (left side) is added and has light in embodiment 2 under illumination condition
The optical photograph that hot anti-bacterial hydrogel dressing (right side) is coated with the plate of the bacterium solution after Escherichia coli co-cultivation afterwards.
Photo-thermal anti-bacterial hydrogel dressing manufactured in the present embodiment is under conditions of illumination, antibiotic rate 100%;And alginic acid
Antibiotic rate is 0% to sodium-acrylamide gel (no tungsten disulfide) under light illumination.Two in aerogel dressing manufactured in the present embodiment
Tungsten sulfide extent of exfoliation is high, evenly dispersed in aerogel dressing matrix, and performance, which is stablized, has long acting antibiotic effect.
The mechanical experimental results of aerogel dressing manufactured in the present embodiment are as shown in table 2.
The mechanical property parameters of the aerogel dressing of 2 embodiment 2 of table preparation
Embodiment 3
(1) tungsten disulfide is added in the sodium alginate soln that concentration is 0.1wt% and is mixed, then ultrasound 8h
(power 600W, frequency 45Hz) is centrifuged 30min with 1500 revs/min of revolving speeds, takes supernatant, then turn with 8500 revs/min
Speed centrifugation 30min, collects precipitating;Then it disperses precipitating in the sodium alginate soln that concentration is 2wt%, it is molten to obtain mixing
Liquid;Tungsten disulfide concentration in mixed solution is 0.125wt%;
(2) acrylamide is added into mixed solution (acrylamide accounts for mixed solution and acrylamide gross mass
16%) it, is uniformly mixed, crosslinking agent N, the N- methylene-bisacrylamide and 0.1% of relative acrylamide's mass 0.08% is added
Thermal initiator ammonium persulfate, be uniformly mixed, obtain pre-polymerization liquid;
(3) pre-polymerization liquid is poured into 5 centimetres of length, it is 5 centimetres wide, with a thickness of in 2 millimeters of molds, the mold of pre-polymerization liquid will be poured into
Be put into baking oven, at 50 DEG C, react 2.5 hours plastics, demoulding obtain good mechanical properties with photo-thermal anti-microbial property
Aerogel dressing.Fig. 5 is that sodium alginate-acrylamide gel (left side) is added and has light in embodiment 3 under illumination condition
The optical photograph that hot anti-bacterial hydrogel dressing (right side) is coated with the plate of the bacterium solution after Escherichia coli co-cultivation afterwards.
Photo-thermal anti-bacterial hydrogel dressing manufactured in the present embodiment is under conditions of illumination, antibiotic rate 100%;And alginic acid
Antibiotic rate is 0% to sodium-acrylamide gel (no tungsten disulfide) under light illumination.Two in aerogel dressing manufactured in the present embodiment
Tungsten sulfide extent of exfoliation is high, evenly dispersed in aerogel dressing matrix, and performance, which is stablized, has long acting antibiotic effect.
The mechanical experimental results of aerogel dressing manufactured in the present embodiment are as shown in table 3.
The mechanical property parameters of the aerogel dressing of 3 embodiment 3 of table preparation
Embodiment 4
(1) tungsten disulfide is added in the sodium alginate soln that concentration is 0.15wt% and is mixed, then ultrasound 8h
(power 800W, frequency 45Hz) is centrifuged 30min with 1500 revs/min of revolving speeds, takes supernatant, then turn with 8500 revs/min
Speed centrifugation 30min, collects precipitating;Then it disperses precipitating in the sodium alginate soln that concentration is 2.25wt%, is mixed
Solution;Tungsten disulfide concentration in mixed solution is 0.15wt%;
(2) acrylamide is added into mixed solution (acrylamide accounts for mixed solution and acrylamide gross mass
18%) it, is uniformly mixed, crosslinking agent N, the N- methylene-bisacrylamide and 0.1% of relative acrylamide's mass 0.08% is added
Thermal initiator ammonium persulfate, be uniformly mixed, obtain pre-polymerization liquid;
(3) pre-polymerization liquid is poured into 5 centimetres of length, it is 5 centimetres wide, with a thickness of in 2 millimeters of molds, the mold of pre-polymerization liquid will be poured into
It is put into baking oven, at 50 DEG C, reacts 2.5 hours plastics.Demoulding obtain good mechanical properties with photo-thermal anti-microbial property
Aerogel dressing.Fig. 6 is that sodium alginate-acrylamide gel (left side) is added and has light in embodiment 4 under illumination condition
The optical photograph that hot anti-bacterial hydrogel dressing (right side) is coated with the plate of the bacterium solution after Escherichia coli co-cultivation afterwards.
Photo-thermal anti-bacterial hydrogel dressing manufactured in the present embodiment is under conditions of illumination, antibiotic rate 100%;And alginic acid
Antibiotic rate is 0% to sodium-acrylamide gel (no tungsten disulfide) under light illumination.Two in aerogel dressing manufactured in the present embodiment
Tungsten sulfide extent of exfoliation is high, evenly dispersed in aerogel dressing matrix, and performance, which is stablized, has long acting antibiotic effect.
The mechanical experimental results of aerogel dressing manufactured in the present embodiment are as shown in table 4.
The mechanical property parameters of the aerogel dressing of 4 embodiment 4 of table preparation
The mechanical property provided from Examples 1 to 4 is it is found that tungsten disulfide extent of exfoliation is high, in aerogel dressing matrix
It is evenly dispersed, and there is no the mechanical properties for reducing hydrogel.
Claims (8)
1. a kind of preparation method of photo-thermal anti-bacterial hydrogel dressing, characterized by the following steps:
(1) by tungsten disulfide ultrasonic disperse in sodium alginate soln, mixed solution is obtained;
(2) mixed solution is mixed with acrylamide, crosslinking agent, initiator, obtains pre-polymerization liquid;
(3) pre-polymerization liquid is subjected to plastic, obtains photo-thermal anti-bacterial hydrogel dressing.
2. the preparation method of photo-thermal anti-bacterial hydrogel dressing according to claim 1, it is characterised in that:
The dosage of tungsten disulfide described in step (1) meets the following conditions: tungsten disulfide accounts for the 0.075% of mixed solution gross mass
~1.5%;
The concentration of sodium alginate is 0.02wt%~5wt% in sodium alginate soln described in step (1).
3. the preparation method of photo-thermal anti-bacterial hydrogel dressing according to claim 1, it is characterised in that: described in step (1)
Mixed solution specifically refers to remove tungsten disulfide ultrasound in sodium alginate soln, and low-speed centrifugal removes unstripped material,
High speed centrifugation again disperses precipitating in sodium alginate soln again, obtains mixed solution.
4. the preparation method of photo-thermal anti-bacterial hydrogel dressing according to claim 3, it is characterised in that: the stripping of tungsten disulfide ultrasound
Concentration from the sodium alginate in sodium alginate soln is 0.02wt%~0.2wt%;It disperses alginic acid again by precipitating
The concentration of sodium alginate soln in sodium solution is 1.5wt%~4.8wt%;
The revolving speed of the low-speed centrifugal is 800-2000r/min;The ultracentrifugal revolving speed is 5000-12000r/min, low
The time of speed centrifugation is 10-60min, and the ultracentrifugal time is 10~60min.
5. the preparation method of photo-thermal anti-bacterial hydrogel dressing according to claim 1, it is characterised in that: described in step (2)
The dosage of acrylamide is the 6%~18.7% of mixed solution and acrylamide gross mass.
6. the preparation method of photo-thermal anti-bacterial hydrogel dressing according to claim 1, it is characterised in that: described in step (2)
Crosslinking agent is N, and N- methylene-bisacrylamide, N hydroxymethyl acrylamide, the initiator is ammonium persulfate or potassium peroxydisulfate;
The dosage of crosslinking agent described in step (2) is the 0.04%~1.2% of acrylamide quality;The dosage of initiator is propylene
The 0.05%~0.2% of amide quality.
7. the preparation method of photo-thermal anti-bacterial hydrogel dressing according to claim 1, it is characterised in that: described in step (1)
The condition of ultrasound is 80~800W, and 20~100Hz, ultrasonic time is 1~100h;
The temperature of plastic described in step (3) is 40~70 DEG C, and gelation time is 1~5h.
8. a kind of photo-thermal anti-bacterial hydrogel dressing obtained by any one of claim 1~7 preparation method.
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