CN101301487A - Gelatine/biological activity glass composite sponge dressing and preparation thereof - Google Patents
Gelatine/biological activity glass composite sponge dressing and preparation thereof Download PDFInfo
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- CN101301487A CN101301487A CN 200810039461 CN200810039461A CN101301487A CN 101301487 A CN101301487 A CN 101301487A CN 200810039461 CN200810039461 CN 200810039461 CN 200810039461 A CN200810039461 A CN 200810039461A CN 101301487 A CN101301487 A CN 101301487A
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Abstract
The present invention relates to a gelatin/biological activity glass compounded sponge dressing and a preparation method thereof, belonging to the biomaterial field. The dressing is characterized in that a solution of a content of between 1 and 30 percent is prepared with gelatin as the raw material; the biological activity glass powder with a weight percentage of between 2 and 20 percent, prepared by the fusion method or the sol-gel method, is put into the solution; and then a mixed solution is obtained by magnetic stirring. The mixed solution is poured into a mould, the liquid layer is up to between 1 and 8 mm, the mixed solution is kept stand for 0.5 to 3 h, and then the prefreezing temperature is controlled between 20 DEG C below zero and 80 DEG C below zero; the lyophilization is controlled to be carried out at a temperature of 40 DEG C below zero and a pressure of between 5 and 10 KPa. The section of the present invention is of a double layer composite structure with a thickness of between 0.5 and 5 mm, wherein, the upper layer is a loose porous layer, and the lower layer is a dense powder layer, the thickness of the powder layer being up to between 0.1 and 2.0 mm. The double layer sponge dressing is flexible, which can be used as a parenchyma wound restoring material. Particularly, the double sponge dressing is suitable for any one of parenchyma ulcers of cervix erosions, oral ulcers, bedsores, sinuses, fat liquescency wounds, venereal disease ulcers, hemorrhoids, diabetes ulcers, etc. and the long-term erosions thereof.
Description
Technical field
The present invention relates to a kind of gelatin/bioactivity glass composite sponge dressing that is used for soft tissue repair and preparation method thereof, belong to technical field of biological material.
Background technology
Skin is the organ of human body maximum, if skin is subjected to large tracts of land damage, then can cause many parts even general problem, as metabolism aggravation, moisture and protein excessively scatter and disappear, immune system disorder etc., the serious entail dangers to life of going back.If wound surface covers suitable dressing, can effectively reduce the metabolic order of severity of patient's body superelevation, ease the pain, prevent bacterial infection, quicken wound healing.Wherein, treating long-term erosive wound is one of puzzlement medical circle difficult problem, does not have very ineffective and simple drug treatment.Critically ill patient can only clean a wound, sterilize, change dressings and treat by carrying out in hospital every day.At present, there is the somatomedin of taking from allosome allos, to extract to promote the Therapeutic Method of wound healing both at home and abroad.This exogenous growth factor may cause scabbing.In addition, because somatomedin extracts preparation mostly from allosome allos, there is the possibility of introducing viral infection.
Bioactivity glass has 30 years of researches history, and existing more than 15 year of successful clinical practice is the synthetic material of the growth healing of at present unique growth, bone damaged healing can the promotion again soft tissue that can promote osseous tissue.This artificial synthetic material is compared with the biomaterial that other extracts from allosome, and biggest advantage is its safety, does not worry the infection of other allosome pathogenic bacteria.The good characteristic of bioactivity glass derives from its surface activity.Up-to-date studies show that, the surface activity of bioactivity glass can promote the generation of somatomedin, procreation, the activating cell gene expression of promotion cell.Like this, bioactivity glass begins direct control with the gene of process by directly cell cycle being brought out in those adjustings, thereby strengthens and reached the facilitation that tissue is formed growth.The characteristic that these are unique makes bioactivity glass use clinically as medical apparatus and instruments and has huge potential value, causes the bigger concern of academia and industrial circle.Although its excellent biological compatibility and biological activity, bioactivity glass has only a kind of granular pattern and present porous block timbering material as the bone defect repair at present as the clinical practice product.
People extensively explore the Wound dressing that can be used as skin barrier in recent years.Chinese patent (CN1554448A) discloses the biological bleeding-stopping dressing of a kind of chitosan gelatin polyvinyl alcohol, is formulated by chitosan, gelatin, polyvinyl alcohol, glycerol.This dressing has hydrophilic, film property, tractive and haemostatic effect preferably, but wound surface is not had the obvious treatment effect.Chinese patent ZL02111437.4 discloses a kind of chitosan, collagen and calcium alginate compounded spongy biological dressing and preparation technology thereof.This dressing good biocompatibility, adhesiveness is strong, has the active function and the anastalsis that promote wound healing.But its used type i collagen price is comparatively expensive, and has certain antigenicity, is unfavorable for widespread adoption.And gelatin is the soluble mixtures of polypeptides of a kind of hot water, get by the collagen hydrolysate in the skin that extensively is present in higher mammal, the bone connective tissue, antigenicity and excellent biological compatibility that it is weak, of many uses at pharmaceutical sanitary fields such as burn, wound, cornea disease, beauty treatment, orthopedic, wound surface hemostasis.Chinese invention patent (ZL200410018370.4) has proposed the application of bioactive glass powder in preparation treatment ulcer and erosive wound dressing.In order further to enlarge the range of application of bioactivity glass in soft tissue injury is repaired, the present invention intends selecting for use gelatin as carrier material, with the compound with it dressing form of making of bioactive glass powder, be used for the treatment of soft-tissue trauma and long-term erosive wound better.
Summary of the invention
The object of the present invention is to provide a kind of gelatin/bioactivity glass composite sponge dressing and preparation method.The sponge dressing that provides is carrier with the gelatin, makes bioactive glass powder is compound with it, and this dressing is not only soft, good biocompatibility, and is two-layer composite, and the bioactivity glass of fine and close bisque can effectively be treated long-term erosive wound.This dressing is as the soft tissue defects repair materials, be specially adapted to long-term erosion, can satisfy the needs of biomaterial development of new generation and clinical practice as any or they in the soft tissue ulcers such as cervical erosion, oral ulcer, decubital ulcer, sinus tract, fat liquor voltinism wound, sexually transmitted disease (STD) ulcer, hemorrhoid, diabetic ulcer.
The present invention is to be that feedstock production becomes solution with the gelatin, and (prepare with fusion method, the mass percent of its chemical composition is 24-45%CaO, 34-50%SiO to add bioactive glass powder
2, 0-25%Na
2O, 5-17%P
2O
5, 0-5%MgO and 0-1%CaF
2Perhaps obtain with Prepared by Sol Gel Method, the mass percent of its chemical composition is 50-91%SiO
2, 5-50%CaO, surplus is P
2O
5), get mixed solution through magnetic agitation.Then mixed solution is poured in the mould, left standstill at normal temperatures, pre-freeze, vacuum lyophilization get the two-layer compound film dressing.Its detailed process is: under 40 ℃～60 ℃ temperature, a certain amount of gelatin is dissolved in the deionized water, the preparation mass percentage concentration is 1～30% solution A, adding the quality percentage composition in A is 2～20% bioactive glass powders, magnetic agitation 1-5h, make glass powder be uniformly dispersed mixed solution B.Mixed solution B is poured in the mould, liquid layer reaches 1-8mm, leave standstill 0.5-3h under the room temperature, the pre-freeze temperature was controlled under the low temperature between-20 ℃～-80 ℃ pre-freeze 1 hour then, then with the lyophilization in the vacuum freeze drier again of the gel of pre-freeze, lyophilization is controlled at-40 ℃ to be carried out under 5～10KPa, finally obtains having double-deck sponge dressing, and thickness reaches 0.5～5mm.It is loose porous layer at the middle and upper levels, and lower floor is fine and close bisque, and fine and close powder layer thickness reaches 0.1～2.0mm.Employed mould is glass mold or politef mould.The gelatin and the compound sponge dressing of bioactivity glass that adopt method provided by the invention to prepare to have difformity, different thickness.By technology controlling and process the bioactivity glass powder layer thickness is controlled to some extent, the bioactive glass powder of capacity is contacted with the wound sepage, the accelerated surface reaction takes place, promote wound healing.
The effect of bioactivity glass is to utilize its surface activity reaction to cause wound healing.When bioactive glass powder touches soft tissue ulcers and long-term rotten to the corn wound, when contacting with the wound sepage, the accelerated surface reaction takes place.High specific surface area absorption fibroblast, upper epidermis cell and some protein growth factors of bioactive glass particle, these cells are subjected to the effect of the stable and somatomedin of hydroxyapatite shelf layer, help cell metabolism and make up new tissue, make the bioactive glass particle surface become the base of connective tissue and epidermal tissue's growth.In addition, the bioactive glass particle surface reaction can improve wound or soft tissue injury place pH value, can suppress wound infection.All these effects have reached the effect that promotes wound and soft tissue injury healing.
In sum, the double-deck sponge dressing of gelatin of the present invention/bioactivity glass has unique advantage as soft tissue wound repair materials, is specially adapted to burn, the long-term erosion of any or they in the soft tissue ulcers such as surgical wound surface, cervical erosion, oral ulcer, decubital ulcer, sinus tract, fat liquor voltinism wound, sexually transmitted disease (STD) ulcer, hemorrhoid, diabetic ulcer.
Specific implementation method of the present invention is as follows:
1, material preparation
Bioactive glass powder of the present invention prepares by melting method or sol-gel method.Used inorganic raw material is analytical pure.Fusion method is that chemical reagent is needed behind weighing and the mixing 1380-1480 ℃ of following fusion by different component, obtains the glass powder that granularity is 40-300 μ m through cooling off, pulverize, sieving again.Sol-gal process is to adopt inorganic salt or the metal alkoxide presoma as oxide in the bio-vitric, under the catalytic action of nitric acid, in aqueous solution, be hydrolyzed, add mix homogeneously such as nitrate then, form colloidal sol, the colloidal sol for preparing was 60 ℃ of ageings 72 hours, form gel, 120 ℃ of dryings 72 hours, the dry gel powder that ball milling, screening make obtained the glass powder that granularity is 1-40 μ m 600～800 ℃ of calcinings then.It is little that the bioactivity glass of Prepared by Sol Gel Method has density, specific surface area height, the characteristic that biological activity is high.
Gelatin is dissolved in deionized water with it under 40 ℃～60 ℃ temperature, is mixed with mass concentration and is 1%～30% aqueous gelatin solution; Adding quality percentage composition is 2～20% bioactive glass powder in gelatin solution, and magnetic agitation 1-5h is uniformly dispersed glass powder; This mixed solution is poured in the mould, and liquid layer reaches 1-8mm, leaves standstill 0.5-3h under the room temperature, puts under-20 ℃--80 ℃ the low temperature more than the pre-freeze 1h gel lyophilization in vacuum freeze drier that pre-freeze is good then.Lyophilization is controlled at-40 ℃ to be carried out under 5～10KPa, obtains softish gelatin/bioactivity glass composite sponge dressing behind about 48h.Employed gelatin is buied from Chemical Reagent Co., Ltd., Sinopharm Group.
2, performance evaluation
2.1 evaluated biological activity
The bioactive glass powder of gelatin/bioactivity glass composite sponge dressing bottom that the present invention is obtained scrapes, earlier after deionized water and washing with acetone, carry out external solution biological activity test after drying.Solutions employed is human body simulation body fluid (SBF; Simulated Body Fluid).SBF contains ion identical with human plasma and ion cluster concentration.
SBF consists of:
NaCl 7.996g/L
NaHCO
3 0.350g/L
KCl 0.224g/L
K
2HPO
4.3H
2O 0.228g/L
MgCl
2.6H
2O 0.305g/L
HCl 1mol/L
CaCl
2 0.278g/L
Na
2SO
4 0.071g/L
NH
2C(CH
2OH)
3 6.057g/L
Bioactive glass powder is in SBF, and reaction condition is in 0.15g bioactive glass powder, 30.0mL/day SBF, the 37 ℃ of calorstats.The bioactive glass powder immersion after 3 days, is taken out sample also through doing the test of XRD and fourier infrared conversion spectrum (FTIR) behind the deionized water wash, and the result sees Fig. 3, Fig. 4 respectively.Biological activity test shows that the bioactive glass powder of gelatin/bioactivity glass composite sponge dressing bottom that the present invention obtains can generate the bone hydroxyapatite at spatial induction, thereby shows that these materials have good biological activity.
Description of drawings
The present invention is described in further detail in conjunction with the accompanying drawings by following, can understand content mentioned above better.Wherein,
Fig. 1 is the manufacture method sketch map of gelatin/bioactivity glass composite sponge dressing.
Fig. 2 is the gelatin/bioactivity glass composite sponge dressing outward appearance photo of preparation.
Fig. 3 is the gelatin/bioactivity glass composite sponge dressing section optical microscope photograph of preparation.
Fig. 4 is that the bioactive glass powder (B) of the gelatin/bioactivity glass composite sponge dressing bottom of pure bioactive glass powder (A) and the embodiment of the invention 1 preparation soaks the XRD figure after 3 days in SBF (human body simulation body fluid); Picture display material soaks 3 days surfaces through SBF has the great amount of hydroxy group phosphorite crystal to occur.
Fig. 5 is that the bioactive glass powder of the gelatin/bioactivity glass composite sponge dressing bottom of the embodiment of the invention 1 preparation soaks Fourier transform infrared spectroscopy (FTIR) figure after 3 days in SBF.
The specific embodiment
Below by embodiments of the invention, further illustrate substantive distinguishing features of the present invention and obvious improvement, but the present invention is limited to embodiment by no means.
Adopt fusion method to prepare bioactive glass powder, with analytical pure SiO
2, Na
2CO
3, CaCO
3, P
2O
5Deng raw material uniform mixing in proportion, be melt into homogeneous melt at 1420 ℃, cooling is then pulverized, and sieving obtains the bioactive glass powder of particle diameter at 40-300 μ m.The quality percentage composition of this glass powder is CaO 24.5%, SiO
245%, Na
2O 24.5%, P
2O
56%.
Gelatin is dissolved in deionized water with it under 40 ℃～60 ℃ temperature, is mixed with mass concentration and is 2% aqueous gelatin solution; Adding quality percentage composition is that 5% granularity is the bioactive glass powder of 100-150 μ m in gelatin solution, and magnetic agitation 3h is uniformly dispersed glass powder; This mixed solution is poured in the mould, and liquid layer reaches 2mm, leaves standstill 1h under the room temperature, puts into pre-freeze 1h under-75 ℃ the low temperature then, gel lyophilization in vacuum freeze drier that pre-freeze is good.Lyophilization is controlled at-40 ℃ to be carried out under 5KPa, obtains softish gelatin/bioactivity glass composite sponge dressing behind the 48h.This two-layer composite thickness reaches 2mm, and powder layer thickness reaches 0.15mm.As shown in Figure 5, after soaking 3 days, SBF promptly have hydroxyapatite (wave number is 571.97) to occur.
Embodiment 2
Adopt the Prepared by Sol Gel Method bioactive glass powder, use ethyl orthosilicate (TEOS) as SiO
2Presoma, triethyl phosphate (TEP) is as P
2O
5Presoma.Under the catalytic action of nitric acid, in aqueous solution, be hydrolyzed, add mix homogeneously such as nitrate then, form colloidal sol, the colloidal sol for preparing was 60 ℃ of ageings 72 hours, form gel, 120 ℃ of dryings 72 hours, the dry gel powder that ball milling, screening make obtained the bioactive glass powder of particle diameter at 1-40 μ m 700 ℃ of calcinings then.This glass powder consist of SiO
258%, CaO 33%, P
2O
59%.
Gelatin is dissolved in deionized water with it under 40 ℃～60 ℃ temperature, is mixed with mass percentage concentration and is 2.5% aqueous gelatin solution; Adding quality percentage composition is that 10% granularity is the bioactive glass powder of 1-40 μ m in gelatin solution, and magnetic agitation 4h is uniformly dispersed glass powder; This mixed solution is poured in the mould, and liquid layer reaches 2.5mm, leaves standstill 1h under the room temperature, puts into pre-freeze 1h under-75 ℃ the low temperature then, gel lyophilization in vacuum freeze drier that pre-freeze is good.Lyophilization is controlled at-40 ℃ to be carried out under 5KPa, obtains softish gelatin/bioactivity glass composite sponge dressing behind the 48h.This two-layer composite thickness reaches 2.5mm, and powder layer thickness reaches 0.25mm.
Embodiment 3
Adopt fusion method to be melt into homogeneous melt at 1450 ℃.The quality percentage composition that is prepared into bioactivity glass is CaO 40%, SiO
240%, Na
2O 8%, P
2O
512%., all the other are with embodiment 1, and the result is also similar to embodiment 1.
Embodiment 4
Adopt Prepared by Sol Gel Method to become bioactivity glass, the mass percentage concentration of the gelatin of the aqueous gelatin solution of being prepared is 20%, and the adding mass percentage concentration is that 18% granularity is the bioactivity glass of 1-40 μ m in gelatin, and all the other are with embodiment 2.Prepared two-layer composite thickness reaches 4.5mm, and powder layer thickness reaches about 1.5mm.
Claims (8)
1, a kind of gelatin/bioactivity glass composite sponge dressing is characterized in that:
(1) described composite sponge dressing is that the bioactive glass powder that adds quality percentage composition 2-20% in 1～30% the gelatin deionized water solution is formed by mass percentage concentration;
(2) described sponge dressing is a double-decker, and the upper strata is loose porous layer, and lower floor is fine and close bisque.
2, by the described gelatin of claim 1/bioactivity glass composite sponge dressing, it is characterized in that the percentage composition of described bioactivity glass quality is:
(1) 24-45%CaO, 34-50%SiO
2, 0-25%Na
2O, 5-17%P
2O
5, 0-5%MgO and 0-1%CaF
2
Or (2) 50-91%SiO
2, 5-50%CaO, surplus is P
2O
5
3, by the described gelatin of claim 1/bioactivity glass composite sponge dressing, it is characterized in that described double-decker thickness is 0.5-5mm, fine and close powder layer thickness reaches 0.1-2.0mm.
4, preparation is characterized in that as the method for claim 1 or 3 described gelatin/bioactivity glass composite sponge dressings preparation process is:
(1) gelatin is dissolved in deionized water with it under 40 ℃～60 ℃ temperature, is mixed with mass concentration and is 1～30% aqueous gelatin solution;
(2) adding the quality percentage composition in gelatin solution is 2～20% bioactive glass powders, and magnetic agitation 1-5h is uniformly dispersed glass powder;
(3) mixed solution is poured in the mould, liquid layer reaches 1-8mm, leaves standstill 0.5-3h under the room temperature, puts under-20 ℃-80 ℃ the low temperature more than the pre-freeze 1h gel lyophilization in vacuum freeze drier that pre-freeze is good then.Lyophilization is controlled at-40 ℃ to be carried out under 5～10KPa, finally makes to have double-deck sponge dressing.
5,, it is characterized in that employed mould is glass mold or is the politef mould by the preparation method of the described gelatin of claim 4/bioactivity glass composite sponge dressing.
6,, it is characterized in that described bioactive glass powder adopts fusion method or sol-gel process to prepare by the preparation method of the described gelatin of claim 4/bioactivity glass composite sponge dressing.
7,, it is characterized in that the granularity of the bioactive glass powder of fusion method preparation is 40-300 μ m by the preparation method of claim 4 or 6 described gelatin/bioactivity glass composite sponge dressings; The granule of the bioactive glass powder of sol-gel process preparation is 1-40 μ m.
8, press the application of the described gelatin of claim 1/bioactivity glass composite sponge dressing, it is characterized in that described composite sponge dressing as soft tissue wound repair materials, be specially adapted to burn, the long-term erosion of any or they in the soft tissue ulcers such as surgical wound surface, cervical erosion, oral ulcer, decubital ulcer, sinus tract, fat liquor voltinism wound, sexually transmitted disease (STD) ulcer, hemorrhoid, diabetic ulcer.
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