CN109793920A - A kind of collagen dressing of the microballoon containing PCL and preparation method thereof and 3D printing application - Google Patents
A kind of collagen dressing of the microballoon containing PCL and preparation method thereof and 3D printing application Download PDFInfo
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Abstract
The invention belongs to biomedical materials fields, more particularly to a kind of collagen dressing containing polycaprolactone microballoon sphere, including the following raw material contained in water and every 100mL water: collagen 0.5-4g, hydroxyapatite 1-15g, PCL drug bearing microsphere 0.5-3g, glucolactone 2-5g and sodium alginate 3-8g.Collagen in conjunction with alginate solution, is prepared collagen/alginate hydrogel material by simple plural gel approach by the present invention, can obtain good biological activity, compatibility and can drug load and sustained release medical material；And it is added to the PCL microballoon for having loaded drug, stress dispersion can be played the role of, improve the mechanical property of collagen dressing；In addition drug load, it can be achieved that drug slow release, the collagen dressing of 3D printing can be prevented to be contaminated by bacterial, play the role of antibiotic and sterilizing, be conducive to wound reparation and healing.
Description
Technical field
The invention belongs to biomedical materials fields, and in particular to a kind of 3D printing is used containing polycaprolactone (PCL) microballoon
Collagen dressing and preparation method thereof.
Background technique
Collagen is structural proteins important in the main component and animal connective tissue of extracellular matrix.Naturally
Collagen has many advantages, such as good biocompatibility, biodegradability, hydrophily, nontoxic, in tissue engineering bracket, wound
The medical function materials such as face dressing, pharmaceutical carrier field has a wide range of applications.Skin is the maximum organ of human body and main
Natural defence line, since large area is externally exposed environment, the moment may be damaged.Some slight damages for pertaining only to epidermis
Wound can be related to the surface of a wound that epidermis and skin corium seriously damage and be difficult to self-heal with self-heal, and easily be caused thin
Bacterium infects and causes various concurrent inflammation, causes great pain to patient.Deep wounds how are effectively thus repaired, especially
The depth wound surface of a wound has become one of the hot spot of medical domain research.Wound dressing can temporarily substitute skin sparing wound not by thin
Bacterium infection, provides good environment for wound healing.Especially collagen hydrogels have good as novel Wound dressing
Biocompatibility, be able to maintain wound moist environment, can continuous absorption surface of a wound exudate, adhesion wound when replacement has temperature
The cooling effect of sum can substantially reduce postoperative pain and inflammation etc., can temporarily substitute skin sparing wound, and wound is promoted to be cured
It closes.Collagen hydrogels have the advantages that collagen and hydrogel simultaneously, in addition it can load some active medicines, play anti-
Bacterium, inoxidizability or it is anti-inflammatory the effects of, have broad application prospects as a kind of new medical aerogel dressing.
Chinese patent CN105079864A discloses a kind of dressing of 3D printing preparation, by inorganic silicon compound and/or nothing
Machine calcium compound is printed using 3D printer to gauze surface, and dressing is obtained.Inorganic compound is directly printed upon by this kind of dressing
Gauze surface, the combination between the two is insecure, easily causes inorganic compound to fall off in use process with gauze and separates, makes
At wound infection；Although wound cannot be accelerated in addition, traditional gauze dressing can completely cut off external environment to a certain extent
Healing can also easily cause secondary damage, therefore develop novel dressing with important because with wound exudate adhesion in dressing
Meaning.It is porous compound that a kind of fibroin/titanium for loading Anti-radiation Microbes is disclosed in Chinese patent CN108714238A
Medical dressing and preparation method thereof, the preparation of this kind of dressing need to handle by -20 to -80 DEG C of low temperature environment, preparation condition
Harshness, complex process are at high cost；In addition, this kind of dressing does not have anti-microbial property, during dressing progress wound repair
Wound is easy to be unfavorable for wound reparation by bacterium infection.
Summary of the invention
In view of the above-mentioned problems, available the object of the present invention is to provide a kind of better mechanical property, with long-acting bacteriostatic
In the collagen dressing of the microballoon containing PCL of 3D printing building, and devise preparation method.
In order to solve the above technical problems, the invention is realized by the following technical scheme:
Design the following raw material contained in a kind of collagen dressing of microballoon containing PCL, including water and every 100mL water: collagen
Albumen 0.5-4g, hydroxyapatite 1-15g, PCL drug bearing microsphere 0.5-3g, glucolactone 2-5g and sodium alginate 3-8g.
Preferably, the following raw material contained in every 100mL water: collagen 1-3g, hydroxyapatite 2-8g, PCL are carried
Medicine microballoon 1-2.5g, glucolactone 2-3.5g and sodium alginate 4-6g.
Preferably, the PCL drug bearing microsphere is made of following steps:
(1) carrying medicament, polycaprolactone (PCL) are distributed in methylene chloride (successively mass volume ratio 1-5g:3-8g:
100ml), (ultrasonic disperse is uniformly rear under room temperature) forms oily phase；Hydroxyapatite (HAP) is distributed in water (2-7:100g/
Ml), water phase is formed (after being dispersed with stirring under room temperature uniformly)；(with liquid-transfering gun amount) takes a certain amount of above-mentioned oil to be mutually distributed in water phase
(ratio between water phase used and oily phase is (2-4): 1), (shaking certain time with vortex vortex mixer) forms oil-in-water cream
Liquid；
(2) methylene chloride in oil-in-water emulsion obtained by step (1) is volatilized naturally, obtains white powder PCL drug bearing microsphere.
Preferably, the carrying medicament is at least one of Enrofloxacin, brufen and gentamicin.
The preparation method of the collagen dressing of the above-mentioned microballoon containing PCL, comprising the following steps:
One, the collagen, hydroxyapatite (HAP), sodium alginate are distributed in water, PCL drug bearing microsphere and Portugal is added
Grape saccharic acid lactone obtains the hydrogel solution of precrosslink after mixing evenly；
Two, by hydrogel solution obtained by step 1, it is imported into 3D printer (in syringe), is beaten according to the model of setting
Print, obtains the collagen dressing of the microballoon containing PCL；Then the collagen dressing of gained microballoon containing PCL is freeze-dried
It handles to get the collagen dressing of the porous microballoon containing PCL is arrived.
The concrete operation step of 3D printing are as follows: squeezed out the hydrogel solution of the precrosslink in syringe by gas pressure
Onto print platform, it is layering molding according to the printer model of setting.
Beneficial effects of the present invention:
The present invention is first prepared for loading the PCL microballoon of antibacterials, then microballoon is mixed into sodium alginate/collagen suspension liquid
In, collagen dressing is prepared using 3D printing technique, when in use according to simulated skin layered structure, according to actual demand
The shape, size, ingredient etc. of collagen hydrogels dressing are accurately controlled.Constructed collagen hydrogels apply
Expect mechanical performance and toughness with higher, good antibiotic property, biocompatibility, gas permeability, water imbibition, water-retaining property, drug
The multiple functions characteristic such as slow release.
(1) present invention develops the bio-medical composite hydrogel that can be used for 3D printing using collagen as main component,
And it is applied to Wound dressing, collagen has good biocompatibility, life as structural proteins important in connective tissue
Biodegradable, hydrophily, it is nontoxic the advantages that, and have hemoglutination, may advantageously facilitate Wound healing.
(2) present invention manufactures medical dressing by 3D printing forming technique.The gel dressing of building being capable of simulated skin
Structure improves dressing porosity and gas permeability, promotes Wound healing.3D printing technique can be according to the reality of wound simultaneously
Situation, personalized rapid build gel dressing targetedly promote wound reparation and healing.
(3) the PCL microballoon of carrying medicament is added in the present invention in the gel solution of 3D printing, stress point can be passed through
It dissipates to play the role of improving mechanical property；In addition drug load, it can be achieved that drug slow release, wound quilt can be prevented
Antibiotic and sterilizing is played the role of in germ contamination.
Detailed description of the invention
Fig. 1 is the SEM figure of the collagen dressing section of the microballoon containing PCL prepared by embodiment 1.
Fig. 2 is the SEM figure of collagen dressing section prepared by comparative example 1.
Fig. 3 is the high power SEM figure of PCL microballoon in the collagen dressing of the microballoon containing PCL prepared by embodiment 1.
Specific embodiment
Below with reference to embodiment to further detailed description of the present invention, embodiments of the present invention are not limited thereto.
Embodiment 1
A kind of preparation method of the collagen dressing of 3D printing microballoon containing PCL, comprising the following steps:
(1) 0.06 g Enrofloxacin is weighed, 0.225 g polycaprolactone (PCL) is added in 3 ml methylene chloride, ultrasound under room temperature
After dispersing 20min, oily phase is formed；It is added in 9 mL deionized waters in addition, weighing 0.3 g hydroxyapatite (HAP), under room temperature
After being dispersed with stirring 30 min, water phase is formed；Above-mentioned oil, which is measured, with liquid-transfering gun is added in water phase (the ratio between water phase and oily phase
Example is 3:1), 10 min are shaken with vortex vortex mixer, form oil-in-water emulsion；
(2) oil-in-water emulsion that above-mentioned steps (1) obtain is poured into culture dish, allows methylene chloride to volatilize naturally 24 h, finally
Obtain white powder PCL drug bearing microsphere；
(3) 0.3 g collagen, 0.6 g hydroxyapatite (HAP), 1.2 g sodium alginates are weighed and are added to 30 ml deionizations
In water, after 30 min are dispersed with stirring under room temperature, 0.3 g of PCL drug bearing microsphere obtained in step (2) is added, adds 0.6 Portugal g
Grape saccharic acid lactone obtains the hydrogel solution of precrosslink after mixing evenly；
(4) it by the hydrogel solution of precrosslink in step (3), imported into the syringe of 3D printer, according to the model of setting
Start to print, after printing, obtains the collagen dressing of the microballoon containing PCL；Then by the collagen dressing of the microballoon containing PCL
It is put into freeze drier, carries out freeze-drying process, obtain finished product afterwards for 24 hours.
Embodiment 2
A kind of preparation method of the collagen dressing of 3D printing microballoon containing PCL, comprising the following steps:
(1) 0.06 g Enrofloxacin is weighed, 0.225 g polycaprolactone (PCL) is added in 3 ml methylene chloride, ultrasound under room temperature
After dispersing 20min, oily phase is formed；It is added in 9 mL deionized waters in addition, weighing 0.3 g hydroxyapatite (HAP), under room temperature
After being dispersed with stirring 30 min, water phase is formed；Above-mentioned oil, which is measured, with liquid-transfering gun is added in water phase (the ratio between water phase and oily phase
Example is 3:1), 10 min are shaken with vortex vortex mixer, form oil-in-water emulsion；
(2) oil-in-water emulsion that above-mentioned steps (1) obtain is poured into culture dish, allows methylene chloride to volatilize naturally 24 h, finally
Obtain white powder PCL drug bearing microsphere；
(3) 0.3 g collagen, 0.6 g hydroxyapatite (HAP), 1.5 g sodium alginates are weighed and are added to 30 ml deionizations
In water, after 30 min are dispersed with stirring under room temperature, 0.3 g of PCL drug bearing microsphere obtained in step (2) is added, adds 0.9 Portugal g
Grape saccharic acid lactone obtains the hydrogel solution of precrosslink after mixing evenly；
(4) it by the hydrogel solution of precrosslink in step (3), imported into the syringe of 3D printer, according to the model of setting
Start to print, after printing, obtains the collagen dressing of the microballoon containing PCL；Then by the collagen dressing of the microballoon containing PCL
It is put into freeze drier, carries out freeze-drying process, obtain finished product afterwards for 24 hours.
Embodiment 3
A kind of preparation method of the collagen dressing of 3D printing microballoon containing PCL, comprising the following steps:
(1) 0.06 g Enrofloxacin is weighed, 0.225 g polycaprolactone (PCL) is added in 3 ml methylene chloride, ultrasound under room temperature
After dispersing 20min, oily phase is formed；It is added in 9 mL deionized waters in addition, weighing 0.3 g hydroxyapatite (HAP), under room temperature
After being dispersed with stirring 30 min, water phase is formed；Above-mentioned oil, which is measured, with liquid-transfering gun is added in water phase (the ratio between water phase and oily phase
Example is 3:1), 10 min are shaken with vortex vortex mixer, form oil-in-water emulsion；
(2) oil-in-water emulsion that above-mentioned steps (1) obtain is poured into culture dish, allows methylene chloride to volatilize naturally 24 h, finally
Obtain white powder PCL drug bearing microsphere；
(3) 0.3 g collagen, 0.6 g hydroxyapatite (HAP), 1.8 g sodium alginates are weighed and are added to 30 ml deionizations
In water, after 30 min are dispersed with stirring under room temperature, 0.3 g of PCL drug bearing microsphere obtained in step (2) is added, adds 1.05 g
Glucolactone obtains the hydrogel solution of precrosslink after mixing evenly；
(4) it by the hydrogel solution of precrosslink in step (3), imported into the syringe of 3D printer, according to the model of setting
Start to print, after printing, obtains the collagen dressing of the microballoon containing PCL；Then by the collagen dressing of the microballoon containing PCL
It is put into freeze drier, carries out freeze-drying process, obtain finished product afterwards for 24 hours.
Comparative example 1
A kind of preparation method of 3D printing collagen dressing, comprising the following steps:
(1) 0.3 g collagen, 0.6 g hydroxyapatite (HAP), 1.2 g sodium alginates are weighed and are added to 30 ml deionizations
In water, after 30 min are dispersed with stirring under room temperature, 0.6 g glucolactone is added, after mixing evenly, obtains the water of precrosslink
Gel solution；
(2) it by the hydrogel solution of precrosslink in step (1), imported into the syringe of 3D printer, according to the model of setting
Start to print, after printing, obtains collagen dressing；Then collagen dressing is put into freeze drier, into
Row freeze-drying process obtains finished product afterwards for 24 hours.
The section SEM of the collagen gel dressing prepared according to embodiment 1 and comparative example 1 schemes respectively such as Fig. 1 and Fig. 2 institute
Show.It can be seen from the figure that containing in the dressing porous structure that the embodiment of the present invention 1 obtains in identical technical parameter
There are a large amount of micro-sphere structures, be conducive to drug and load and be sustained, release antibacterials, protection wound are conducive in the practical application of dressing
Mouthful, from bacterium infection, promote Wound healing.
Embodiment 4
A kind of preparation method of the collagen dressing of 3D printing microballoon containing PCL, comprising the following steps:
(1) 1 g Enrofloxacin is weighed, 3 g polycaprolactones (PCL) are added in 100 ml methylene chloride, ultrasonic disperse under room temperature
After 20min, oily phase is formed；It is added in 100 mL deionized waters in addition, weighing 2 g hydroxyapatites (HAP), is stirred under room temperature
After dispersing 30 min, water phase is formed；Above-mentioned oil, which is measured, with liquid-transfering gun is added in water phase that (ratio between water phase and oily phase is
3:1), 10 min are shaken with vortex vortex mixer, form oil-in-water emulsion；
(2) oil-in-water emulsion that above-mentioned steps (1) obtain is poured into culture dish, allows methylene chloride to volatilize naturally 24 h, finally
Obtain white powder PCL drug bearing microsphere；
(3) 0.5 g collagen, 1 g hydroxyapatite (HAP), 3 g sodium alginates are weighed to be added in 100ml deionized water,
After being dispersed with stirring 30 min under room temperature, 0.5 g of PCL drug bearing microsphere obtained in step (2) is added, adds 2 g gluconic acids
Lactone obtains the hydrogel solution of precrosslink after mixing evenly；
(4) it by the hydrogel solution of precrosslink in step (3), imported into the syringe of 3D printer, according to the model of setting
Start to print, after printing, obtains the collagen dressing of the microballoon containing PCL；Then by the collagen dressing of the microballoon containing PCL
It is put into freeze drier, carries out freeze-drying process, obtain finished product afterwards for 24 hours.
Embodiment 5
A kind of preparation method of the collagen dressing of 3D printing microballoon containing PCL, comprising the following steps:
(1) 5 g Enrofloxacins are weighed, 8 g polycaprolactones (PCL) are added in 100 ml methylene chloride, ultrasonic disperse under room temperature
After 20min, oily phase is formed；It is added in 100 mL deionized waters in addition, weighing 7 g hydroxyapatites (HAP), is stirred under room temperature
After dispersing 30 min, water phase is formed；Above-mentioned oil, which is measured, with liquid-transfering gun is added in water phase that (ratio between water phase and oily phase is
4:1), 10 min are shaken with vortex vortex mixer, form oil-in-water emulsion；
(2) oil-in-water emulsion that above-mentioned steps (1) obtain is poured into culture dish, allows methylene chloride to volatilize naturally 24 h, finally
Obtain white powder PCL drug bearing microsphere；
(3) 4 g collagens, 15 g hydroxyapatites (HAP), 8 g sodium alginates are weighed to be added in 100 ml deionized waters,
After being dispersed with stirring 30 min under room temperature, 3 g of PCL drug bearing microsphere obtained in step (2) is added, adds 5 glucolactones,
After mixing evenly, the hydrogel solution of precrosslink is obtained；
(4) it by the hydrogel solution of precrosslink in step (3), imported into the syringe of 3D printer, according to the model of setting
Start to print, after printing, obtains the collagen dressing of the microballoon containing PCL；Then by the collagen dressing of the microballoon containing PCL
It is put into freeze drier, carries out freeze-drying process, obtain finished product afterwards for 24 hours.
Embodiment 6
A kind of preparation method of the collagen dressing of 3D printing microballoon containing PCL, comprising the following steps:
(1) 3 g Enrofloxacins are weighed, 5 g polycaprolactones (PCL) are added in 100 ml methylene chloride, ultrasonic disperse under room temperature
After 20min, oily phase is formed；It is added in 100 mL deionized waters in addition, weighing 5 g hydroxyapatites (HAP), is stirred under room temperature
After dispersing 30 min, water phase is formed；Above-mentioned oil, which is measured, with liquid-transfering gun is added in water phase that (ratio between water phase and oily phase is
2:1), 10 min are shaken with vortex vortex mixer, form oil-in-water emulsion；
(2) oil-in-water emulsion that above-mentioned steps (1) obtain is poured into culture dish, allows methylene chloride to volatilize naturally 24 h, finally
Obtain white powder PCL drug bearing microsphere；
(3) 2 g collagens, 8 g hydroxyapatites (HAP), 5 g sodium alginates are weighed to be added in 100 ml deionized waters,
After being dispersed with stirring 30 min under room temperature, 1.8 g of PCL drug bearing microsphere obtained in step (2) is added, adds 3.5 g glucose
Acid lactone obtains the hydrogel solution of precrosslink after mixing evenly；
(4) it by the hydrogel solution of precrosslink in step (3), imported into the syringe of 3D printer, according to the model of setting
Start to print, after printing, obtains the collagen dressing of the microballoon containing PCL；Then by the collagen dressing of the microballoon containing PCL
It is put into freeze drier, carries out freeze-drying process, obtain finished product afterwards for 24 hours.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be effective substitute mode, be included within the scope of the present invention.
Claims (9)
1. a kind of collagen dressing of microballoon containing PCL, including water, it is characterised in that: further include contain in every 100mL water with
Lower raw material: collagen 0.5-4g, hydroxyapatite 1-15g, PCL drug bearing microsphere 0.5-3g, glucolactone 2-5g and sea
Mosanom 3-8g.
2. collagen dressing according to claim 1, it is characterised in that: the following raw material contained in every 100mL water: glue
Former albumen 1-3g, hydroxyapatite 2-8g, PCL drug bearing microsphere 1-2.5g, glucolactone 2-3.5g and sodium alginate 4-
6g。
3. collagen dressing according to claim 1 or 2, it is characterised in that: the PCL drug bearing microsphere is by following step
Suddenly it is made:
(1) a certain amount of carrying medicament, polycaprolactone are distributed in methylene chloride, form oily phase；Hydroxyapatite is distributed to
In water, water phase is formed；It takes a certain amount of above-mentioned oil to be mutually distributed in water phase, forms oil-in-water emulsion；
(2) methylene chloride in oil-in-water emulsion obtained by step (1) is volatilized naturally, obtains white powder PCL drug bearing microsphere.
4. collagen dressing according to claim 3, it is characterised in that: step (1) carrying medicament, polycaprolactone
Mass volume ratio between methylene chloride is (1-5) g:(3-8) g:100ml.
5. collagen dressing according to claim 3, it is characterised in that: step (2) hydroxyapatite and water it
Between mass volume ratio be (2-7): 100g/ml.
6. collagen dressing according to claim 3, it is characterised in that: the ratio between water phase used and oily phase is
(2-4): 1.
7. collagen dressing according to claim 3, it is characterised in that: the carrying medicament is Enrofloxacin, Bu Luo
At least one of fragrant and gentamicin.
8. the preparation method of collagen dressing described in claim 1-7, which comprises the following steps:
One, the collagen, hydroxyapatite, sodium alginate are distributed in water, PCL drug bearing microsphere and gluconic acid is added
Lactone obtains the hydrogel solution of precrosslink after mixing evenly；
Two, by hydrogel solution obtained by step 1, it is imported into 3D printer, is printed according to the model of setting, obtained containing PCL
The collagen dressing of microballoon；Then it is more to get arriving the collagen dressing of gained microballoon containing PCL to be subjected to freeze-drying process
The collagen dressing of hole microballoon containing PCL.
9. application of any one of the claim 1-7 collagen dressing in 3D printing.
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Application publication date: 20190524 |