CN110755669B - Medical collagen wound repair membrane - Google Patents
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Abstract
The invention discloses a medical collagen wound repair film, which has a three-layer structure consisting of a graphene oxide/collagen film and composite gel microspheres, wherein the upper layer and the lower layer are both the graphene oxide/collagen film, and the middle layer is the composite gel microspheres; the graphene oxide/collagen film is prepared by taking graphene oxide, fish scale collagen and garlic extract as raw materials and poly-lysine as a cross-linking agent; the composite gel microspheres are loaded on the graphene oxide/collagen film in an electrostatic spraying mode. The collagen wound repair film has good mechanical strength and good elasticity, is used for wound repair, has good hemostasis and antibacterial properties, has the effect of radiating infrared rays to promote blood circulation on the surface of a wound so as to promote the wound to heal and shorten the wound healing period, and can also avoid the problem of slow wound healing speed caused by secondary wound injury after the wound is subjected to external force again.
Description
Technical Field
The invention relates to the field of medical supplies, in particular to a medical collagen wound repair film.
Background
The skin provides a protective effect for the human body, and once the skin is injured, the skin can greatly influence the physical function; therefore, after the skin is injured, the wound needs to be protected in time to avoid the wound from being infected; the existing common wound repair products comprise gauze, gel dressing, band-aid dressing, sponge dressing and the like, the wound repair products have the effects of protecting and stopping bleeding and promoting wound healing by being pasted on the surface of a wound, and a wound repair material pasted on the surface of the wound has certain oppressibility on the wound, so that the body temperature of the surface of the wound is reduced, discomfort of a patient is caused, and the phenomenon is caused because the wound is coated to influence the blood circulation effect on the surface of the wound and be not beneficial to wound healing, so that the wound repair film has the effect of promoting the blood circulation of the wound and plays an important role in promoting wound repair and shortening the wound healing period; in addition, in actual life, the wound surface is also inevitably damaged by external force, and when the wound surface is touched by the external force, a patient can be caused with huge pain, so that the wound surface dressing has a certain buffering effect, and further has positive significance for reducing the damage of the external force to the wound surface.
At present, a wound repair film only has a protective effect on a wound, and for a serious wound, the wound healing period is long and unavoidable, and the wound can be infected, so that the improvement of the antibacterial performance of the repair film has an important effect on wound repair; on the other hand, there is a problem that an excessive amount of an antibacterial agent (e.g., silver ion) causes side effects to the human body.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a medical collagen wound repair film which has good mechanical strength and good elasticity, is used for wound repair, has good hemostatic and antibacterial properties, has the function of promoting blood circulation on the surface of a wound so as to promote the wound to heal and shorten the healing period of the wound, and can avoid the problem of slow healing speed of the wound caused by secondary injury of the wound due to the external force acting on the wound again.
The technical scheme for solving the technical problems is as follows:
a medical collagen wound repair film has a three-layer structure consisting of a graphene oxide/collagen film and composite gel microspheres, wherein the upper layer and the lower layer of the wound repair film are both the graphene oxide/collagen film, and the middle layer is the composite gel microspheres; the graphene oxide/collagen film is prepared by taking graphene oxide, fish scale collagen and garlic extract as raw materials and polylysine as a cross-linking agent; the composite gel microsphere is prepared from the following raw materials in parts by weight: 4-6 parts of sodium alginate, 4-6 parts of polyethylene glycol, 2-3 parts of polyethyleneimine, 0.2-0.3 part of liquid silicone rubber, 0.4-0.6 part of zeolite, 0.1-0.2 part of medical stone, 0.05-0.1 part of vermiculite, 0.5-1 part of aloe extract, 0.4-0.8 part of alkanna tinctoria root extract and 0.2-0.3 part of bletilla striata extract;
the preparation method of the medical collagen wound repair membrane specifically comprises the following steps:
(1) preparation of graphene oxide/collagen film
1.1) cleaning, removing impurities and drying fish scales, crushing the fish scales into powder, adding an acetic acid solution into the powder, stirring the mixture to react for 12 to 24 hours, filtering the mixture to obtain a fish scale filter material and a filtrate, washing the fish scale filter material for 1 to 3 times by using the acetic acid solution, and transferring the washing solution into the filtrate for later use;
1.2) heating the fish scale filter material washed in the step 1.1) to 90 ℃, sterilizing for 5-10min, adding a mixture of an acetic acid solution and a pepsin solution after cooling, reacting for 24-36h at 36-37 ℃, and performing centrifugal separation to obtain a supernatant collagen enzymolysis liquid;
1.3) adding the garlic extract into the collagenase hydrolyzed solution obtained in the step 1.2), carrying out ultrasonic stirring reaction, adding graphene oxide, carrying out stirring ultrasonic dispersion uniformly, adding xanthan gum, carrying out stirring uniformly to obtain a mixed solution, injecting the mixed solution into a film forming mold, injecting a polylysine solution into the mold, and soaking at the temperature of 2-4 ℃ for 12-24 hours to obtain a wet graphene oxide/collagen film;
(2) preparing a gel microsphere precursor solution:
2.1) dispersing a mixture of sodium alginate, polyethylene glycol, polyethyleneimine and liquid silicone rubber in deionized water to obtain a high-molecular mixed solution;
2.2) taking bletilla striata and alkanna tinctoria root, grinding into powder, adding 75% ethanol solution for soaking, and obtaining an extract through reduced pressure suction filtration; cleaning fresh aloe, cutting, mashing, adding equivalent amount of deionized water, crushing in ultrasonic cell crusher, and centrifuging to obtain supernatant as aloe extract; adding extracts of rhizoma Bletillae and radix Arnebiae into the aloe extract to obtain mixed extract;
2.3) irradiating medical stone, vermiculite and zeolite in sunlight for 12-24 hours, mixing, grinding and crushing the mixture to obtain mixed particles, dispersing the mixed particles into the mixed extract obtained in the step 2.2), ultrasonically stirring uniformly, adding the high-molecular mixed solution obtained in the step 2.1), and stirring uniformly to form a gel microsphere precursor solution;
(3) preparation of medical collagen wound repair film
Injecting the gel microsphere precursor solution obtained in the step (2) into an injector of a high-voltage electrostatic spraying device, fixing the wet graphene oxide/collagen film obtained in the step (1) on a receiver flat-plate aluminum foil, uniformly loading the gel microspheres on the surface of the graphene oxide/collagen film by adopting an electrostatic spraying method, then flatly paving the graphene oxide/collagen film prepared in the step (1) on the surface of the gel microspheres, and drying in a freeze dryer to obtain the medical collagen wound repair film.
Preferably, the mass volume ratio of the fish scale powder and the acetic acid solution in the step 1.1) is 1 g: 30-38 mL;
preferably, the mass percentage concentration of the acetic acid solution in the step 1.2) is 3-5 wt%; the adding amount of the pepsin is 1-3% of the weight of the fish scale filter material; the concentration of the pepsin solution is 800-1000mg/L, and the adding volume of the pepsin solution is 3 times of the volume of the acetic acid solution; the content of collagen in the collagen enzymolysis liquid is 0.6-0.8g/100 mL;
preferably, the mass-to-volume ratio of the added amount of the graphene oxide to the collagen enzymolysis liquid in the step 1.3) is 0.1-0.2g/100mL, and the mass-to-volume ratio of the added amount of the xanthan gum to the collagen enzymolysis liquid is 0.1-0.3g/100 mL; the volume ratio of the polylysine solution to the collagen enzymolysis liquid is 1:1, and the mass percentage concentration of the polylysine solution is 5-10 wt%; the volume ratio of the added garlic extract to the collagen enzymolysis liquid is 1: 10;
preferably, the garlic extract is prepared by peeling garlic, mashing, adding a mixture of water and glycerol (volume ratio of 1:1) 20 times, soaking at room temperature for 1-2h, centrifuging, filtering, and separating to obtain a supernatant (garlic extract), wherein the content of allicin in the garlic extract is 0.2-0.4 wt%;
preferably, the particle size of the mixed particles in step 2.3) is 40-100 nm;
preferably, the loading capacity of the gel microspheres on the surface of the graphene oxide/collagen membrane is 1-2g/cm2；
Preferably, the spraying speed of the injection pump in the electrostatic spraying process is 2-4mL/min, the distance between the receiver and the spray head is 5-10cm, the voltage is 16-20kv, and the inner diameter of the spray head is 0.5 mm;
the medical collagen wound repair membrane is composed of a three-layer structure, wherein the upper layer and the lower layer are both graphene oxide/collagen membranes, the middle layer is a composite gel microsphere, and electrostatic action and chemical bonding action exist between the graphene oxide/collagen membranes and the composite gel microsphere, so that the combination is tight; the preparation of the graphene oxide/collagen film adopts polylysine as a cross-linking agent, so that the adverse effect on wounds caused by the residue of chemical reagents (glutaraldehyde and ethylene oxide) as the cross-linking agent is avoided; the mechanical strength of the membrane is improved, and the polylysine has good hydrophilicity, so that the repairing membrane can be quickly wetted when being in contact with the wound surface and has strong adhesion with the wound surface; the composite gel ball has elasticity, gives a good force buffering effect to the membrane, and reduces the damage of external force to the wound;
in the medical collagen wound repair film, the graphene oxide/collagen film is obtained by adopting graphene oxide and collagen under the condition that polylysine is used as a cross-linking agent, and under the acidic condition, the graphene oxide and the collagen belong to anionic type and react with cationic polylysine to form a net structure, so that the mechanical strength of the collagen film is improved; the graphene oxide is introduced into the membrane structure, so that the mechanical strength of the collagen membrane is improved, and the membrane has the function of radiating infrared rays, promotes blood circulation and is beneficial to wound healing; meanwhile, the polylysine is used as a cross-linking agent for replacing a conventional chemical reagent, has the antibacterial and antiseptic effects, has the synergistic antibacterial effect with the garlic extract, and improves the antibacterial performance and the storage stability of the repairing film; in addition, polylysine has strong hygroscopicity, which is beneficial to the adhesion of a repair film and a wound surface, and the polylysine has degradability, and amino acid generated by degradation provides nutrient substances for the healing of wound surface tissues;
in the medical collagen wound repair film, the gel microspheres are loaded on the graphene oxide/collagen film by adopting an electrostatic spraying method, and the graphene oxide/collagen film and the collagen film have strong electrostatic binding force; the gel microspheres have certain elasticity, improve the buffering effect of the wound repair film on external force, have a porous structure and have strong water absorption.
The gel microspheres are prepared by coating medical stone and vermiculite zeolite with surfaces adsorbing bletilla striata, alkannin roots and aloe extracts by adopting a biopolymer material, and the coating of the plant extracts improves the dispersibility of mineral substances in the gel and ensures that the gel microspheres have a homogeneous structure and certain elasticity and mechanical strength; simultaneously has the function of synergistically promoting the healing of the wound surface;
the medical stone has a porous spongy structure, has strong adsorption effect, can adsorb metabolic wastes of the wound, and enhances the cell activity of the skin of the wound to promote the healing of the wound; the medical stone contains various trace elements necessary for human bodies, and the trace elements in the medical stone are gradually released along with the occurrence of adsorption, so that nutrient substances required for wound healing are provided; the medical stone also has the function of radiating far infrared rays, and has the health-care functions of promoting blood circulation and activating tissue cells by cooperating with the graphene oxide, so that the healing of wounds can be promoted; vermiculite is a natural, inorganic and nontoxic mineral substance, has a layered structure, is used in combination with medical stone, and is beneficial to storage and slow release of far infrared radiation.
Compared with the prior art, the invention has the following beneficial effects:
the medical collagen wound repair film has excellent mechanical strength and good elasticity, has the effects of quickly stopping bleeding and promoting wound healing, generates certain buffer effect when a wound is acted by external force, reduces the damage of the external force to the wound, has the effect of radiating far infrared, stimulates the activity of wound tissue cells, promotes the blood circulation of wound tissue, promotes the healing of the wound and shortens the healing period of the wound;
the wound repair film has higher bonding speed and stronger bonding force with the wound skin, so that the bleeding can be quickly stopped;
the medical collagen wound repair film has the antibacterial and antiseptic effects, and the storage stability of the medical collagen wound repair film is improved, and the wound healing effect is promoted;
the collagen of the invention is derived from waste fish scales, the price is low, and the preparation process is simple, and the cost is low; and the fish scale collagen overcomes the risk of disease infection existing in the mammal collagen; and the collagen molecules are easy to absorb and utilize, and are more beneficial to wound healing.
Detailed Description
The technical solution of the present invention is further described below with reference to specific examples.
Example 1
A medical collagen wound repair film has a three-layer structure consisting of a graphene oxide/collagen film and composite gel microspheres, wherein the upper layer and the lower layer of the wound repair film are both the graphene oxide/collagen film, and the middle layer is the composite gel microspheres; the graphene oxide/collagen film is prepared by taking graphene oxide, fish scale collagen and garlic extract as raw materials and polylysine as a cross-linking agent; the composite gel microsphere is prepared from the following raw materials in parts by weight: 4 parts of sodium alginate, 4 parts of polyethylene glycol, 2 parts of polyethyleneimine, 0.2 part of liquid silicone rubber, 0.4 part of zeolite, 0.1 part of medical stone, 0.05 part of vermiculite, 0.5 part of aloe extract, 0.4 part of alkanna tinctoria root extract and 0.2 part of bletilla striata extract;
the preparation method of the medical collagen wound repair membrane specifically comprises the following steps:
(1) preparation of graphene oxide/collagen film
1.1) cleaning 1000g of fish scales, removing impurities, drying, crushing into powder, adding 30L of 5wt% acetic acid solution, stirring for reacting for 24h, filtering to obtain a fish scale filter material and a filtrate, washing the fish scale filter material for 1-3 times by using the acetic acid solution, and transferring the washing solution into the filtrate for later use;
1.2) taking the fish scale filter material washed in the step 1.1), heating to 90 ℃, sterilizing for 5-10min, adding a mixture of 3 wt% acetic acid solution and 800mg/L pepsin solution after cooling, reacting for 36h at 36-37 ℃, and performing centrifugal separation to obtain supernatant collagen enzymatic hydrolysate; standby; wherein, the adding amount of the pepsin is 1 percent of the weight of the fish scale filter material; the volume of the acetic acid solution is 1/3 times the volume of the pepsin solution.
1.3) adding 2L of garlic extract into 20L of collagen hydrolysate in 1.2), carrying out ultrasonic stirring reaction, adding 10g of graphene oxide into the mixture, adding 10g of xanthan gum, fully and uniformly stirring to obtain a mixed solution, injecting the mixed solution into a film forming mold, injecting an isovolumetric 5wt% polylysine solution into the mold, and soaking at 2 ℃ for 24 hours to obtain a wet graphene oxide/collagen film for later use;
preparing a garlic extract: peeling 500g of garlic, mashing, adding a mixture of 20 times of ethanol and glycerol, soaking at normal temperature for 1-2h, and centrifuging, filtering and separating to obtain a supernatant, namely a garlic extract, wherein the content of allicin in the garlic extract is 0.2-0.4 wt%;
(2) preparing a gel microsphere precursor solution:
2.1) dispersing a mixture of 4g of sodium alginate, 4g of polyethylene glycol, 2g of polyethyleneimine and 0.2g of liquid silicone rubber in deionized water to obtain a high-molecular mixed solution;
2.2) grinding 10g of bletilla striata and 10g of alkanna tinctoria root into powder, adding 75% ethanol solution into the powder for soaking, and then carrying out vacuum filtration to obtain an extract; cleaning fresh 20g of aloe, cutting, mashing, adding equivalent deionized water, crushing in an ultrasonic cell crusher, and centrifuging to obtain supernatant as aloe extract; adding extracts of rhizoma Bletillae and radix Arnebiae into the aloe extract to obtain mixed extract;
2.3) irradiating 0.1g of medical stone, 0.05g of vermiculite and 0.4g of zeolite under sunlight for 12 hours, mixing, grinding and crushing the mixture to obtain 40-100nm mixed particles, dispersing the mixed particles in the mixed extract obtained in the step 2.2), ultrasonically stirring uniformly, adding the polymer mixed solution obtained in the step 2.1), and stirring uniformly to form a gel microsphere precursor solution;
3) preparation of medical collagen wound repair film
Injecting the gel microsphere precursor solution obtained in the step (2) into an injector of a high-voltage electrostatic spraying device, fixing the graphene oxide/collagen film obtained in the step (1) on a receiver flat-plate aluminum foil, and adopting an electrostatic spraying method to fix the gelUniformly loading microspheres on the surface of a graphene oxide/collagen membrane, then loading the graphene oxide/collagen membrane prepared in the step (1) on the surface of gel microspheres, and drying in a freeze dryer to obtain a medical collagen wound repair membrane; wherein the loading capacity of the gel microspheres on the surface of the graphene oxide/collagen film is 1g/cm2(ii) a In the electrostatic spraying process, the spraying speed of the injection pump is 2 mL/min, the distance between the receiver and the spray head is 5cm, the voltage is 16kv, and the inner diameter of the spray head is 0.5 mm;
example 2
A medical collagen wound repair film has a three-layer structure consisting of a graphene oxide/collagen film and composite gel microspheres, wherein the upper layer and the lower layer of the wound repair film are both the graphene oxide/collagen film, and the middle layer is the composite gel microspheres; the graphene oxide/collagen film is prepared by taking graphene oxide, fish scale collagen and garlic extract as raw materials and polylysine as a cross-linking agent; the composite gel microsphere is prepared from the following raw materials in parts by weight: 5 parts of sodium alginate, 5 parts of polyethylene glycol, 2.5 parts of polyethyleneimine, 0.25 part of liquid silicone rubber, 0.5 part of zeolite, 0.15 part of medical stone, 0.075 part of vermiculite, 0.75 part of aloe extract, 0.6 part of alkanna tinctoria root extract and 0.25 part of bletilla striata extract;
the preparation method of the medical collagen wound repair membrane specifically comprises the following steps:
(1) preparation of graphene oxide/collagen film
1.1) cleaning 1000g of fish scales, removing impurities, drying, crushing into powder, adding 34L of 4wt% acetic acid solution, stirring and reacting for 18h, filtering to obtain a fish scale filter material and a filtrate, washing the fish scale filter material for 1-3 times by using the acetic acid solution, and transferring the washing solution into the filtrate for later use;
1.2) taking the fish scale filter material washed in the step 1.1), heating to 90 ℃, sterilizing for 5-10min, adding a mixture of 4wt% acetic acid solution and 900mg/L pepsin solution after cooling, reacting for 30h at 36-37 ℃, and performing centrifugal separation to obtain supernatant collagen enzymatic hydrolysate; wherein, the adding amount of the pepsin is 2 percent of the weight of the fish scale filter material; the volume of acetic acid solution was 1/3 times the volume of pepsin solution;
1.3) adding 2L of garlic extract into 20L of collagen hydrolysate in 1.2), carrying out ultrasonic stirring reaction, adding 30g of graphene oxide into the mixture, adding 40g of xanthan gum, fully and uniformly stirring to obtain a mixed solution, injecting the mixed solution into a film forming mold, injecting an isovolumetric 7.5 wt% polylysine solution into the mold, and soaking at 3 ℃ for 18h to obtain a wet graphene oxide/collagen film;
preparing a garlic extract: peeling 500g of garlic, mashing, adding a mixture of 20 times of ethanol and glycerol, soaking at normal temperature for 1-2h, and centrifuging, filtering and separating to obtain a supernatant, namely a garlic extract, wherein the content of allicin in the garlic extract is 0.2-0.4 wt%;
(2) preparing a gel microsphere precursor solution:
2.1) dispersing a mixture of 5g of sodium alginate, 5g of polyethylene glycol, 2.5g of polyethyleneimine and 0.25g of liquid silicone rubber in deionized water to obtain a polymer mixed solution;
2.2) grinding 12.5g of bletilla striata and 15g of alkanna tinctoria root into powder, adding 75% ethanol solution into the powder for soaking, and then carrying out vacuum filtration to obtain an extract; cleaning fresh aloe 30g, cutting, mashing, adding equivalent deionized water, crushing in an ultrasonic cell crusher, and centrifuging to obtain supernatant as aloe extract; adding extracts of rhizoma Bletillae and radix Arnebiae into the aloe extract to obtain mixed extract;
2.3) irradiating 0.15g of medical stone, 0.075g of vermiculite and 0.5g of zeolite under sunlight for 18 hours, mixing, grinding and crushing the mixture to obtain 40-100nm mixed particles, dispersing the mixed particles in the mixed extract obtained in the step 2.2), ultrasonically stirring uniformly, adding the polymer mixed solution obtained in the step 2.1), and stirring uniformly to form a gel microsphere precursor solution;
3) preparation of medical collagen wound repair film
Injecting the gel microsphere precursor solution obtained in the step (2) into an injector of a high-voltage electrostatic spraying device, and fixing the graphene oxide/collagen film obtained in the step (1)Uniformly loading gel microspheres on the surface of a graphene oxide/collagen membrane by adopting an electrostatic spraying method, then loading the graphene oxide/collagen membrane prepared in the step (1) on the surface of the gel microspheres, and drying in a freeze dryer to obtain the medical collagen wound repair membrane; wherein the loading capacity of the gel microspheres on the surface of the graphene oxide/collagen film is 1.5g/cm2(ii) a In the electrostatic spraying process, the spraying speed of the injection pump is 3 mL/min, the distance between the receiver and the spray head is 7.5cm, the voltage is 18kv, and the inner diameter of the spray head is 0.5 mm;
example 3
A medical collagen wound repair film has a three-layer structure consisting of a graphene oxide/collagen film and composite gel microspheres, wherein the upper layer and the lower layer of the wound repair film are both the graphene oxide/collagen film, and the middle layer is the composite gel microspheres; the graphene oxide/collagen film is prepared by taking graphene oxide, fish scale collagen and garlic extract as raw materials and polylysine as a cross-linking agent; the composite gel microsphere is prepared from the following raw materials in parts by weight: 6 parts of sodium alginate, 6 parts of polyethylene glycol, 3 parts of polyethyleneimine, 0.3 part of liquid silicone rubber, 0.6 part of zeolite, 0.2 part of medical stone, 0.1 part of vermiculite, 1 part of aloe extract, 0.8 part of alkanna tinctoria root extract and 0.3 part of bletilla striata extract;
the preparation method of the medical collagen wound repair membrane specifically comprises the following steps:
(1) preparation of graphene oxide/collagen film
1.1) cleaning 1000g of fish scales, removing impurities, drying, crushing into powder, adding 38L of 3 wt% acetic acid solution, stirring and reacting for 12h, filtering to obtain a fish scale filter material and a filtrate, washing the fish scale filter material for 1-3 times by using the acetic acid solution, and transferring the washing solution into the filtrate for later use;
1.2) taking the fish scale filter material washed in the step 1.1), heating to 90 ℃, sterilizing for 5-10min, adding a mixture of 3 wt% acetic acid solution and 1000mg/L pepsin solution after cooling, reacting for 24h at 36-37 ℃, and performing centrifugal separation to obtain supernatant collagen enzymatic hydrolysate; wherein, the adding amount of the pepsin is 3 percent of the weight of the fish scale filter material; the volume of acetic acid solution was 1/3 times the volume of pepsin solution.
1.3) adding 2L of garlic extract into 20L of collagen hydrolysate in 1.2), carrying out ultrasonic stirring reaction, adding 40g of graphene oxide aqueous dispersion, adding 60g of xanthan gum, fully and uniformly stirring to obtain a mixed solution, injecting the mixed solution into a film forming mold, injecting an isovolumetric 10wt% polylysine solution into the mold, and soaking at 4 ℃ for 12 hours to obtain a wet graphene oxide/collagen film;
preparing a garlic extract: peeling 500g of garlic, mashing, adding a mixture of 20 times of ethanol and glycerol, soaking at normal temperature for 1-2h, and centrifuging, filtering and separating to obtain a supernatant, namely a garlic extract, wherein the content of allicin in the garlic extract is 0.2-0.4 wt%;
(2) preparing a gel microsphere precursor solution:
2.1) dispersing a mixture of 6g of sodium alginate, 6g of polyethylene glycol, 3g of polyethyleneimine and 0.3g of liquid silicone rubber in deionized water to obtain a high-molecular mixed solution;
2.2) grinding 15g of bletilla striata and 20g of alkanna tinctoria root into powder, adding 75% ethanol solution into the powder for soaking, and then carrying out vacuum filtration to obtain an extract; cleaning fresh aloe 40g, cutting, mashing, adding equivalent deionized water, crushing in an ultrasonic cell crusher, and centrifuging to obtain supernatant as aloe extract; adding extracts of rhizoma Bletillae and radix Arnebiae into the aloe extract to obtain mixed extract;
2.3) irradiating 0.2g of medical stone, 0.1g of vermiculite and 0.6g of zeolite under sunlight for 24 hours, mixing, grinding and crushing the mixture to obtain mixed particles of 40-100nm, dispersing the mixed particles in the mixed extract obtained in the step 2.2), ultrasonically stirring uniformly, adding the polymer mixed solution obtained in the step 2.1), and stirring uniformly to form a gel microsphere precursor solution;
3) preparation of medical collagen wound repair film
Injecting the gel microsphere precursor solution in the step (2) into a high-voltage electrostatic spraying devicePlacing the wet graphene oxide/collagen membrane obtained in the step (1) in an injector, fixing the wet graphene oxide/collagen membrane on a receiver flat-plate aluminum foil, uniformly loading gel microspheres on the surface of the graphene oxide/collagen membrane by adopting an electrostatic spraying method, then loading the graphene oxide/collagen membrane prepared in the step (1) on the surface of the gel microspheres, and drying in a freeze dryer to obtain the medical collagen wound repair membrane; the loading capacity of the gel microspheres on the surface of the graphene oxide/collagen film is 2g/cm2(ii) a In the electrostatic spraying process, the spraying speed of the injection pump is 4mL/min, the distance between the receiver and the spray head is 10cm, the voltage is 20kv, and the inner diameter of the spray head is 0.5 mm;
comparative example 1
The preparation method of the medical collagen wound repair membrane obtained in the comparative example 1 is basically the same as that of the example 3, except that the middle layer does not have the gel microspheres;
comparative example 2
The preparation method of the medical collagen wound repair film obtained in the comparative example 2 is basically the same as that of the example 3, except that graphene oxide is not added;
comparative example 3
The preparation method of the medical collagen wound repair film obtained in the comparative example 3 is basically the same as that of the example 3, except that the graphene oxide/collagen film obtained in the step (1) is not soaked in a polylysine solution;
comparative example 4
The preparation method of the medical collagen wound repair film obtained in the comparative example 4 is basically the same as that of the example 3, except that the garlic extract is not added;
comparative example 5
The preparation method of the medical collagen wound repair membrane obtained in the comparative example 5 is basically the same as that of the example 3, except that the medical stone in the gel microspheres is replaced by the same amount of zeolite;
comparative example 6
The preparation method of the medical collagen wound repair membrane obtained in the comparative example 6 is basically the same as that of the example 3, except that vermiculite in the gel microspheres is replaced by the same amount of zeolite;
comparative example 7
The preparation method of the medical collagen wound repair membrane obtained in the comparative example 7 is basically the same as that of the example 3, except that liquid silicon rubber is not added in the preparation of the gel microspheres;
comparative example 8
The preparation method of the medical collagen wound repair membrane obtained in the comparative example 8 is basically the same as that of the example 3, except that the bletilla striata and the alkanna tinctoria root extracts are not added in the preparation of the gel microspheres;
comparative example 9
The preparation method of the medical collagen wound repair membrane obtained in the comparative example 9 is basically the same as that of the example 3, except that the aloe extract is not added in the preparation of the gel microspheres;
performance testing
The medical collagen wound repair films prepared in the examples 1 to 3 were tested for various properties, and the test items, reference methods and test results are shown in table 1.
Table 1 performance test results of medical collagen wound repair membrane
| Detecting items | Detection method | Example 1 | Example 2 | Example 3 |
| Liquid uptake/%) | YY/T0471.1-2004 | 1034 | 1078 | 1100 |
| Breaking Strength/N | GB/T24218.3-2010 | 92 | 93 | 95 |
| Elongation at break/% | GB/T24218.3-2010 | 70.9 | 71.4 | 73.3 |
| Peel strength/N/cm | YY/T0148-2006 | 3.2 | 3.0 | 2.9 |
| Degree of blocking | GB/T14233.2-2005 | Non-adhesion | Non-adhesion | Non-adhesion |
| Cytotoxicity | GB/T14233.2-2005 | Is free of | Is free of | Is free of |
| Sensitization | GB/T16886.10-2005 | Is free of | Is free of | Is free of |
| Intradermal reaction | GB/T16886.10-2005 | Is free of | Is free of | Is free of |
| Acute systemic toxicity | GB/T16886.11-2011 | Is free of | Is free of | Is free of |
As can be seen from Table 1, the medical collagen wound repair film prepared by the invention has excellent performances such as good water absorption performance, good adhesion capability and good anti-fracture capability, is nontoxic and harmless to human bodies, and meets the standards of medical and sanitary products.
The water absorbing capacity and mechanical properties of the repair films obtained in example 3, comparative example 1, comparative example 2, and comparative example 3 were further tested, and the test results are shown in table 2.
Table 2 test results of wound repair films
| Liquid uptake/%) | Breaking Strength/N | Elongation at break/% | |
| Example 3 | 1100 | 95 | 73.3 |
| Comparative example 1 | 780 | 85 | 63.4 |
| Comparative example 2 | 1000 | 68 | 60.5 |
| Comparative example 3 | 730 | 70 | 48 |
As can be seen from table 2, the liquid absorption capacity, the breaking strength and the breaking elongation of the medical wound repair film prepared in example 3 are all higher than those of comparative examples 1, 2 and 3, compared with example 3, comparative examples 1, 2 and 3 are respectively gel-free microspheres, graphene oxide is not added, and polylysine is not added, the liquid absorption capacity of comparative example 1 is lower than that of example 3, which indicates that the gel spheres and the graphene oxide/collagen layer have a synergistic water absorption effect, and the graphene oxide/collagen layer is a main water absorption layer; the breaking strength and the breaking elongation of the comparative example 1 are slightly lower than those of the example 3, which shows that the gel microspheres are beneficial to enhancing the mechanical strength of the collagen repair film, but have little influence on the mechanical strength; compared with example 3, the liquid absorption amount, the breaking strength and the breaking elongation of comparative example 2 are reduced, but the reduction of the liquid absorption amount is small, and the change of the mechanical strength is large, which indicates that the graphene oxide plays an important role in improving the mechanical strength of the repair film; compared with comparative example 3, the liquid absorption capacity, the breaking strength and the breaking elongation of comparative example 3 are greatly reduced, which shows that the polylysine as the cross-linking agent has a remarkable effect on the water absorption capacity and the mechanical property of the repairing film.
Antibacterial property test
The medical collagen wound repair films prepared in the examples 1 to 3 and the wound repair films prepared in the comparative examples 1 to 9 are subjected to antibacterial tests on staphylococcus aureus, escherichia coli and candida albicans; the antimicrobial results are shown in table 3.
Table 3 bacteriostatic rate of wound repair film to several hospital bacteria
As can be seen from table 3, the wound repair films prepared in examples 1, 2, and 3 of the present invention have higher bacteriostatic rates of over 90% for staphylococcus aureus, escherichia coli, and candida albicans, which indicates that the medical wound repair film of the present invention has good antibacterial ability;
the bacteriostatic rate of the wound repair film in the comparative example 1 to three bacteria is far lower than that in the example 3, which shows that the gel microspheres and the graphene oxide/collagen film have synergistic effect in bacteriostatic performance;
the bacteriostasis rates of the repairing films prepared in the comparative examples 3 and 4 to the three bacteria are far lower than those of the repairing films prepared in the example 3, which shows that the polylysine and the garlic extract have a synergistic bacteriostasis effect and play an important role in the aspect of bacteriostasis performance of the repairing films;
the bacteriostasis rates of comparative examples 2, 5, 6, 8 and 9 to three bacteria are lower than that of example 3, which shows that the raw materials of the wound repair film have bacteriostasis function in the aspect of bacteriostasis performance of the wound repair film;
compared with example 3, the wound repair film of comparative example 7 has no great change in the bacteriostatic rate of three bacteria, which shows that the liquid silicone rubber mainly affects the elasticity of the gel microspheres and the bonding strength with the graphene oxide/collagen film, and has little influence on the bacteriostatic performance of the repair film;
animal wound healing experiment
The wound repair films prepared in the examples 1-3 and the comparative examples 1-9 are used for repairing the wounds of the rabbits, and the wound healing conditions of the rabbits are explored; the experimental method is as follows:
dividing 120 rabbits (with good health condition and weight of 2-3kg) into 12 groups of 10 rabbits, wherein A and A1B and B1C and C1Groups of rabbits treated with the medical repair film prepared in example 1, example 2 and example 3, respectively, and D, E, F, G, H, I, J, K, L groups of rabbits treated with the medical repair film prepared in comparative examples 1 to 9, in that order; reserving a 5cm multiplied by 5cm part of the rabbit back for removing the back hair, disinfecting the rabbit back, making a 1cm multiplied by 1cm wound on the back of the rabbit by using an operation knife, cutting the medical wound repair film prepared in the invention examples 1-3 and the comparative examples 1-9 into a size of 5cm multiplied by 5cm, pasting the medical wound repair film on the surface of the wound, observing the hemostasis condition of the wound, replacing the repair film 1 time every day, and removing A after the next day1、B1、C1Applying a force of 10N to the wound every 48h for each group of rabbits (observing and recording the reaction of the rabbits at the same time) until the wound of the rabbit is completely healed, and counting and recording the infection and healing conditions of the wound surface of the rabbit, wherein the result is shown in table 4, wherein the wound surface healing rate (%) is (original wound surface area-unhealed wound surface area)/original wound surface area.
A and A1B and B1C and C1The wound of the rabbit group has high bleeding stopping speed, and the repairing film has high water absorption speed so that the repairing film is easy to attach and apply on the surface of the wound;
TABLE 4 animal wound healing and infection status
When 10N force is applied to the rabbits, the rabbits in the groups D, E and J have large reaction and large pain feeling, and the rabbits in other groups have no special reaction;
as can be seen from Table 4, A and A1B and B1C and C1The rabbit group has high wound repair rate in 7 days, the wound repair time is short, A and A1B and B1C and C1The wound repair conditions of rabbits in the group are basically the same, which shows that the medical wound repair film prepared in the embodiments 1-3 of the present invention has good wound repair effect and has a buffering effect on external force, and even if the wound is acted by the external force, the wound healing is not affected basically due to the buffering protection effect of the wound repair film;
compared with the group C, the wound repair effect of the D, E, F, G, H, I, J, K, L group rabbits is poor, the D, E, F, G, H group repair cycle is greatly different from the group C, and the wound surface has slight scars after the wound surface is healed, because compared with the wound surface repair film prepared in the example 3 adopted in the group C, D, E, F, G, H group is respectively adjusted on the basis of the example 3 without adding gel microspheres, graphene oxide, polylysine, garlic extract and aloe extract, which shows that the gel microspheres and the graphene oxide/collagen film have a synergistic effect in promoting the wound surface healing, and the graphene oxide/collagen film layer in the wound surface repair film has important effects in the antibacterial property of the wound surface repair film and the promotion of wound healing; h, I, K groups respectively adopt the repairing films obtained by adjusting without adding medical stone, vermiculite and bletilla striata and alkanna tinctoria root extracts on the basis of the embodiment 3, and the healing time of the wound surface is longer than that of the group C and much shorter than that of the group D; the healing time of the wound surface of the group J is slightly longer than that of the group C, probably because liquid silicon rubber is not added in the repairing film of the group J, the elasticity of the gel microspheres is reduced, and when external force is applied, secondary damage is caused to the wound surface, so that the healing time of the wound surface is prolonged; the components in the gel microspheres have the synergistic antibacterial and wound healing promoting effects; the raw materials of the medical collagen wound repair film prepared by the invention have synergistic effect and play an important role in wound repair.
In conclusion, the medical wound repair film has reasonable structure and raw material ratio, the graphene oxide/collagen film and the gel microspheres cooperate with each other to enable the wound repair film to be capable of rapidly absorbing water and adhering to the surface of a wound, and the medical wound repair film has good antibacterial property and capability of promoting wound healing, has a protective effect on the wound, and has a buffering effect on external force acting on the surface of the wound to prevent the wound from being damaged.
Finally, the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting, and other modifications or equivalent substitutions made by the technical solutions of the present invention by those of ordinary skill in the art should be covered within the scope of the claims of the present invention as long as they do not depart from the spirit and scope of the technical solutions of the present invention.
Claims (8)
1. The medical collagen wound repair film is characterized by having a three-layer structure consisting of a graphene oxide/collagen film and composite gel microspheres, wherein the upper layer and the lower layer of the wound repair film are both the graphene oxide/collagen film, and the middle layer is the composite gel microspheres; the graphene oxide/collagen film is prepared by taking graphene oxide, fish scale collagen and garlic extract as raw materials and polylysine as a cross-linking agent; the composite gel microsphere is prepared from the following raw materials in parts by weight: 4-6 parts of sodium alginate, 4-6 parts of polyethylene glycol, 2-3 parts of polyethyleneimine, 0.2-0.3 part of liquid silicone rubber, 0.4-0.6 part of zeolite, 0.1-0.2 part of medical stone, 0.05-0.1 part of vermiculite, 0.5-1 part of aloe extract, 0.4-0.8 part of alkanna tinctoria root extract and 0.2-0.3 part of bletilla striata extract; the preparation method specifically comprises the following steps:
(1) preparation of graphene oxide/collagen film
1.1) cleaning, removing impurities and drying fish scales, crushing the fish scales into powder, adding an acetic acid solution into the powder, stirring and reacting for 12-24h, filtering to obtain a fish scale filter material and a filtrate, washing the fish scale filter material for 1-3 times by using the acetic acid solution, and transferring the washing solution into the filtrate for later use;
1.2) taking the fish scale filter material washed in the step 1.1), heating to 90 ℃, sterilizing for 5-10min, cooling, and adding acetic acid
Reacting the mixture of the solution and the pepsin solution at 36-37 ℃ for 24-36h, and performing centrifugal separation to obtain supernatant collagen enzymatic hydrolysate;
1.3) adding the garlic extract into the collagenase hydrolysate, carrying out ultrasonic stirring reaction, adding graphene oxide, carrying out ultrasonic dispersion uniformly, adding xanthan gum, carrying out stirring and mixing uniformly to obtain a mixed solution, injecting the mixed solution into a film forming mold, injecting a polylysine solution into the mold, and soaking at 2-4 ℃ for 12-24 hours to obtain a wet graphene oxide/collagen film;
(2) preparing a gel microsphere precursor solution:
2.1) dispersing a mixture of sodium alginate, polyethylene glycol, polyethyleneimine and liquid silicone rubber in deionized water to obtain a high-molecular mixed solution;
2.2) grinding bletilla striata and alkanna tinctoria root into powder, adding 75% ethanol solution for soaking, and obtaining an extract through reduced pressure suction filtration; cleaning fresh aloe, cutting, mashing, adding equivalent amount of deionized water, crushing in ultrasonic cell crusher, and centrifuging to obtain supernatant as aloe extract; adding extracts of rhizoma Bletillae and radix Arnebiae into the aloe extract to obtain mixed extract;
2.3) irradiating the medical stone, the vermiculite and the zeolite for 12-24 hours in the sun, mixing, grinding and crushing the mixture to obtain the mixture
Mixing particles, dispersing the mixed particles in the mixed extract obtained in the step 2.2), ultrasonically dispersing the mixed particles uniformly, adding the polymer mixed solution obtained in the step 2.1), and stirring the mixture uniformly to form a gel microsphere precursor solution;
(3) preparation of medical collagen wound repair film
Injecting the gel microsphere precursor solution obtained in the step (2) into an injector of a high-voltage electrostatic spraying device, fixing the wet graphene oxide/collagen film obtained in the step (1) on a receiver flat-plate aluminum foil, uniformly loading gel microspheres on the surface of the graphene oxide/collagen film by adopting an electrostatic spraying method, then flatly paving the graphene oxide/collagen film prepared in the step (1) on the surface of the gel microspheres, and drying in a freeze dryer to obtain the medical collagen wound repair film.
2. A medical collagen wound healing membrane as claimed in claim 1, wherein the mass volume ratio of the fish scale powder and the acetic acid solution in step 1.1) is 1 g: 30-38 mL.
3. The medical collagen wound healing film according to claim 1, wherein the mass percentage concentration of the acetic acid solution in step 1.2) is 3-5 wt%; the adding amount of the pepsin is 1-3% of the weight of the fish scale filter material; the concentration of the pepsin solution is 800-1000mg/L, and the adding volume of the pepsin solution is 3 times of the volume of the acetic acid solution; the content of collagen in the collagen enzymolysis liquid is 0.6-0.8g/100 mL.
4. The medical collagen wound healing membrane as claimed in claim 1, wherein the mass-to-volume ratio of the addition amount of the graphene oxide to the collagen enzymolysis liquid in step 1.3) is 0.1-0.2g/100mL, and the addition amount of the xanthan gum is equal to that of the collagen enzymolysis liquid
The mass volume ratio of the collagen enzymolysis liquid is 0.1-0.3g/100 mL; the volume ratio of the polylysine solution to the collagen enzymolysis liquid is 1:1, and the mass percentage concentration of the polylysine solution is 5-10 wt%; the volume ratio of the added garlic extract to the collagen enzymolysis liquid is 1: 10.
5. A medical collagen wound healing membrane according to claim 1, wherein the garlic extract is obtained by peeling garlic, mashing, adding a mixture of water and glycerol in an amount of 20 times, soaking at room temperature for 1-2h, and centrifuging, filtering and separating to obtain a supernatant, which is the garlic extract, wherein the content of allicin in the garlic extract is 0.2-0.4 wt%.
6. A medical collagen wound healing film according to claim 1, wherein the particle size of the mixed particles in step 2.3) is 40-100 nm.
7. The medical collagen wound healing film according to claim 1, wherein the loading capacity of the gel microspheres on the surface of the graphene oxide/collagen film is 1-2g/cm2。
8. A medical collagen wound healing film according to claim 1, wherein during the electrostatic spraying process, the spraying speed of the injection pump is 2-4mL/min, the distance between the receiver and the nozzle is 5-10cm, the voltage is 16-20kv, and the inner diameter of the nozzle is 0.5 mm.
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