CN109045346A - A kind of preparation method of medical collagen sponge - Google Patents
A kind of preparation method of medical collagen sponge Download PDFInfo
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- A61L24/00—Surgical adhesives or cements; Adhesives for colostomy devices
- A61L24/04—Surgical adhesives or cements; Adhesives for colostomy devices containing macromolecular materials
- A61L24/10—Polypeptides; Proteins
- A61L24/102—Collagen
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- A61L24/00—Surgical adhesives or cements; Adhesives for colostomy devices
- A61L24/001—Use of materials characterised by their function or physical properties
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L24/00—Surgical adhesives or cements; Adhesives for colostomy devices
- A61L24/001—Use of materials characterised by their function or physical properties
- A61L24/0036—Porous materials, e.g. foams or sponges
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L24/00—Surgical adhesives or cements; Adhesives for colostomy devices
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- A61L24/0042—Materials resorbable by the body
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L24/00—Surgical adhesives or cements; Adhesives for colostomy devices
- A61L24/04—Surgical adhesives or cements; Adhesives for colostomy devices containing macromolecular materials
- A61L24/08—Polysaccharides
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2400/00—Materials characterised by their function or physical properties
- A61L2400/04—Materials for stopping bleeding
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Abstract
The invention discloses a kind of preparation methods of medical collagen sponge, belong to biomaterial for medical purpose preparation technical field.Cobweb main chemical compositions are glycine in the present invention, the serine of alanine and fraction, in addition other amino acid monomer Harmonic Protein Molecular Chains are constituted, since Na-alginate is soluble easily in water, belong to hydrophilic macromolecule, it can water swelling in neutral aqueous solution, with stronger moisture holding capacity, using sodium metaperiodate by sodium alginate partial oxidation, obtain the oxidized sodium alginate containing aldehyde radical, this method reduce chain rigidities, the sodium alginate of partial oxidation is due to introducing active group aldehyde radical, hydrogel is formed by chemical crosslinking with the high-molecular compound with amino groups, degumming bamboo fibre is doped in collagem membrane, after degumming process, the pectin of bamboo fibre is separated with lignin hydrolysis, form the bamboo fibre of ultrafine micropore structure, improve the flexibility and sorptivety performance of collagen protein sponge, before wide application Scape.
Description
Technical field
The invention discloses a kind of preparation methods of medical collagen sponge, belong to biomaterial for medical purpose technology of preparing neck
Domain.
Background technique
Medical collagen sponge is common medical treatment consumptive materials in operation, has and serves as filler, quick-acting haemostatic powder prevents from gluing
Even, accelerating wound healing and other effects reduces prevention of postoperative complication.In neurosurgery, orthopaedics, gynaecology, department of general surgery, operating room etc.
Suffer from universal application.
Collagen is a kind of extracellular protein, it is to twist into spiral fibrous proteins, collagen by 3 peptide chains
Albumen is the most abundant protein of people's in-vivo content, accounts for 30% or more of whole body gross protein.It is present in nearly all tissue,
Be a kind of extracellular matrix protein, exist in the form of insoluble fiber, have height tensile energy, to animal and human skin, blood vessel,
Bone, the formation of cartilage are particularly significant, are the important substances of connective tissue, are the principal element for determining connective tissue toughness, collagen
Albumen is also most important component part in extracellular matrix.
Collagen is also to be made of amino acid, but glycine almost accounts in its composition as other albumen
1/3, and proline and hydroxyproline be it is highest in different kinds of proteins, just because of the compositing characteristic of amino acid, collagen
Exist in space with stable triple-helix structure.Collagen has many excellent biological properties, such as hypoimmunity: glue
Repeatability unit in original molecule structure is big, and immunogenicity is very low, and to body without rejection, compatibility is good, general biology
Body will not generate chronic rejection to it.
Wherein, collagen protein sponge is white sponge solid, is one kind of collagen.As common medical treatment consumption
Material has and serves as filler, and quick-acting haemostatic powder prevents adhesion, accelerating wound healing and other effects, postoperative complications is reduced, in medical treatment
It is upper widely used.The special quaternary structure of collagen is mainly utilized in it, thus make platelet activation, release particulate component, it is fast
Rapid hardening blood, in normal blood circulation, blood platelet is not had an effect with endothelial cell surface or other cells, but along hair
Thin blood vessel arrangement, maintains its integrality, and when blood vessel Local Damaged, the hemostasis of blood platelet has mechanicalness blocking wound and change concurrently
The property learned adhesion and aggregation effect.
But the collagen due to isolating and purifying from different tissues is in purity, physicochemical property and collagen
There is significant difference in terms of configuration, antibacterial anti-infection performance is poor, and bleeding and diffusate effect are absorbed when for being applied with processing wound
Fruit is limited, and water-swelling property is to be improved.
Therefore, it invents a kind of good antimicrobial effect and the good medical collagen sponge of water swellability prepares medical material
Technical field has positive effect.
Summary of the invention
Present invention mainly solves the technical issues of, use poor for the current existing antibacterial anti-infection performance of collagen protein sponge
Bleeding is absorbed when being applied with and handling wound and diffusate effect is limited, and water-swelling property defect to be improved provides one
The preparation method of kind medical collagen sponge.
In order to solve the above-mentioned technical problem, the technical scheme adopted by the invention is that:
A kind of preparation method of medical collagen sponge, it is characterised in that specific preparation step are as follows:
(1) 6~10g sodium alginate is taken to be added in the beaker equipped with 200~250mL deionized water, with magnetic stirrer, directly
It is dissolved to sodium alginate, obtains sodium alginate soln, 3~4g sodium metaperiodate is dissolved in 10~12g deionized water, is aoxidized
Liquid；
(2) above-mentioned oxidation solution is fitted into the three-necked flask with dropping funel and blender, starts blender, with 300~
The revolving speed of 500r/min starts to stir, then above-mentioned sodium alginate soln is fitted into dropping funel, and sea is added dropwise into three-necked flask
Solution of sodium alginate after being added dropwise, is placed on three-necked flask under the conditions of being protected from light, reacts under room temperature, obtain oxidized sodium alginate；
(3) 4~5mL ethylene glycol is added to above-mentioned oxidized sodium alginate, terminates reaction, adds 0.8~1.0g sodium chloride, obtain
Mixed liquor is fitted into bag filter by mixed liquor, is protected from light dialysis 3~5 days with distilled water, is changed water 3~4 times daily, is obtained dialysing pure
Change liquid, dialysis purification liquid is put into freeze drier, is freeze-dried, obtains White Flocculus；
(4) 70~80g bamboo fibre is placed in a beaker, it is sub- that 100~130mL sodium hydroxide solution, 8~10g is added into beaker
Sodium sulphate, 10~12g sodium pyrophosphate, place the beaker in water-bath, heat temperature raising, keep the temperature 1~2h, and cooling continues heat preservation 30
~35min obtains degumming bamboo fibre, White Flocculus, carboxymethyl chitosan sugar aqueous solution, degumming bamboo fibre is mixed, mixing is stirred
It mixes 20~30min and obtains oxidation hydrogel；
(5) by 10~15mL gelatin solution, 2~3mL sorbitan mono-oleic acid ester, 4~6g chloramphenicol, 4~5g hydroxylmethyl cellulose
Element is mixed to get antibacterial gelatin solution, and 10~15g cobweb, 20~25g ox heel string, 0.6~0.8g are added into antibacterial gelatin solution
Trypsase is mixed 20~25min of enzymatic hydrolysis, obtains sticky glue, heat temperature raising is stirred with the revolving speed of 800~1000r/min
10~15min of emulsification is mixed, collagen liquid is obtained；
(6) above-mentioned collagen liquid is mixed with oxidation hydrogel and is put into beaker, obtained mixed glue solution, place the beaker ice water
In bath, it is added 1~3mL glutaraldehyde solution after cooling 7~10min into beaker, 40~50min of crosslinking curing, then into beaker
30~50mL acetone is added, obtains mixing suspension, above-mentioned mixing suspension is put into supercentrifuge, centrifuge separation 5~
8min removes upper liquid, obtains fiber gel liquid, then fiber gel liquid is put into freeze drier, and freeze-drying is cured
Use collagen protein sponge.
Magnetic agitation rotating speed described in step (1) is 500~550r/min, the mass fraction of sodium alginate soln is 2~
4%。
Dropping funel drop rate described in step (2) is 4~6mL/min, and the normal-temperature reaction time is 20 under the conditions of being protected from light
~for 24 hours.
The termination reaction time described in step (3) is 2~3h, and it is 12000~14000D that bag filter, which controls molecular cut off,
Being freeze-dried temperature is -40~-20 DEG C, and sublimation drying is 40~45min.
The mass fraction of sodium hydroxide solution described in step (4) is 45%, and oil bath pan heating rate is 2 DEG C/min, heating
Temperature is 80~90 DEG C after heating, and temperature is 40~45 DEG C after cooling, and the mass fraction of carboxymethyl chitosan sugar aqueous solution is 6%, white
Color floccule, carboxymethyl chitosan sugar aqueous solution, degumming bamboo fibre mixing mass ratio are 1 ︰, 4 ︰ 5.
The mass fraction of gelatin solution described in step (5) is 20%, and temperature is 60~65 DEG C after heat temperature raising.
Collagen liquid described in step (6) and oxidation hydrogel mixed volume ratio are 4 ︰ 1, the quality point of glutaraldehyde solution
Number is 50%, and high speed centrifugation revolving speed is 2500~3000r/min, and freeze-drying temperature is -35~-30 DEG C, sublimation drying
For 30~35min.
The beneficial effects of the present invention are:
(1) present invention prepares oxidation solution with sodium metaperiodate, and sodium alginate soln is instilled in oxidation solution, oxidation is protected from light and is aoxidized
Oxidized sodium alginate is added ethylene glycol and terminates reaction, then added sodium chloride and obtain mixed liquor by sodium alginate, and mixed liquor is packed into
Bag filter is dialysed to obtain dialysis purification liquid with distilled water, and freeze-drying obtains White Flocculus, and it is water-soluble to prepare carboxymethyl chitosan
White Flocculus and carboxymethyl chitosan sugar aqueous solution are mixed to get oxidation hydrogel by liquid, with gelatin solution, sorbitol anhydride list oil
Acid esters, chloramphenicol, hydroxymethyl cellulose etc. are raw material, are mixed to get antibacterial gelatin solution, then spider is added into antibacterial gelatin solution
Net, trypsase, enzymatic hydrolysis obtain sticky glue, and sticky glue is added in palm oil, heat and stirring and emulsifying obtains collagen egg
White liquor is added glutaraldehyde solution crosslinking curing after mixing collagen liquid with oxidation hydrogel, adds acetone and mixed
Mixing suspension is centrifugally separating to obtain fiber gel liquid, then is freeze-dried to obtain medical collagen sponge, this hair by suspension
Bright middle cobweb main chemical compositions are the serines of glycine, alanine and fraction, in addition other amino acid monomer albumen
Matter strand is constituted, and this differential protein can play the same coagulation of blood platelet, can quickly be condensed in wound, thus
Play the role of hemostasis, reduce the generation of sepage, and is loaded into the antibiotic properties drugs such as chloramphenicol using microballoon in gelatin solution to reach
Antibacterial purpose reduces bacterium infection；
(2) belong to hydrophilic macromolecule since Na-alginate is soluble easily in water in the present invention, can absorb water in neutral aqueous solution swollen
It is swollen, have stronger moisture holding capacity, be the ideal material that hydrogel is formed in situ, due on sodium alginate strand due to lack
Corresponding message structure is difficult to generate cell positive biological response, and alginate degradation rate is slow, works as jel product
It is difficult to exclude in vitro when accumulating excessive, thus is prepared in vivo using the crosslinking of the oxidation hydrogel and collagen liquid of sodium alginate
Degradable, the medical collagen sponge of high sorptivety expansion, the present invention, by sodium alginate partial oxidation, is obtained using sodium metaperiodate
Oxidized sodium alginate containing aldehyde radical, this method reduce chain rigidities, improve dissolution of the sodium alginate in wound exudate
Degree and degradation capability, in addition, the sodium alginate of partial oxidation is due to introducing active group aldehyde radical, can with amino groups
High-molecular compound hydrogel is formed by chemical crosslinking, oxidized sodium alginate still can promote cell growth, to improve
Medical performance and physiological activity of the medical collagen membrane when handling wound, and the efficiency for absorbing sepage is also accelerated, in addition, this hair
Degumming bamboo fibre is doped in bright collagem membrane, after degumming process, the pectin of bamboo fibre is separated with lignin hydrolysis, is formed
The bamboo fibre of ultrafine micropore structure improves the flexibility and sorptivety performance of collagen protein sponge, has broad application prospects.
Specific embodiment
6~10g sodium alginate is taken to be added in the beaker equipped with 200~250mL deionized water, with magnetic stirring apparatus with 500
The revolving speed of~550r/min stirs, until sodium alginate dissolves, obtaining mass fraction is 2~4% sodium alginate solns, by 3~4g
Sodium metaperiodate is dissolved in 10~12g deionized water, obtains oxidation solution；Above-mentioned oxidation solution is packed into and has dropping funel and blender
Three-necked flask in, start blender, start to stir with the revolving speed of 300~500r/min, then above-mentioned sodium alginate soln is filled
Enter in dropping funel, sodium alginate soln is added dropwise into three-necked flask with the drop rate of 4~6mL/min, it, will after being added dropwise
Three-necked flask is placed on be protected from light under the conditions of, under room temperature react 20~for 24 hours, obtain oxidized sodium alginate；To above-mentioned oxidized sodium alginate
4~5mL ethylene glycol is added, terminates 2~3h of reaction, adds 0.8~1.0g sodium chloride, obtain mixed liquor, mixed liquor is packed into
In bag filter, control molecular cut off is 12000~14000D, is protected from light dialysis 3~5 days with distilled water, changes daily water 3~4 times,
Obtain dialysis purification liquid, dialysis purification liquid be put into freeze drier, at a temperature of -40~-20 DEG C be freeze-dried 40~
45min obtains White Flocculus；70~80g bamboo fibre is placed in a beaker, 100~130mL mass fraction is added into beaker
For 45% sodium hydroxide solution, 8~10g sodium sulfite, 10~12g sodium pyrophosphate, place the beaker in water-bath, with 2 DEG C/
The heating rate of min is heated to 80~90 DEG C, keeps the temperature 1~2h, is cooled to 40~45 DEG C, continues 30~35min of heat preservation, obtain
To degumming bamboo fibre, the carboxymethyl chitosan sugar aqueous solution that mass fraction is 6% is prepared, by White Flocculus, carboxymethyl chitosan syrup
Solution, degumming bamboo fibre are 1 ︰ 4 mixing in mass ratio, and 20~30min is mixed and obtains oxidation hydrogel；By 10~15mL
Gelatin solution, 2~3mL sorbitan mono-oleic acid ester, 4~6g chloramphenicol, 4~5g hydroxymethyl cellulose of the mass fraction for 20%
It is mixed to get antibacterial gelatin solution, 10~15g cobweb, 20~25g ox heel string, 0.6~0.8g pancreas are added into antibacterial gelatin solution
Protease is mixed 20~25min of enzymatic hydrolysis, obtains sticky glue, 60~65 DEG C are heated to, with 800~1000r/min
Revolving speed 10~15min of stirring and emulsifying, obtain collagen liquid；It is by volume by above-mentioned collagen liquid and oxidation hydrogel
4 ︰ 1 mixing is put into beaker, is obtained mixed glue solution, is placed the beaker in ice-water bath, and 1 is added into beaker after cooling 7~10min
The glutaraldehyde solution that~3mL mass fraction is 50%, 40~50min of crosslinking curing, then 30~50mL acetone is added into beaker,
Mixing suspension is obtained, above-mentioned mixing suspension is put into the revolving speed in supercentrifuge with 2500~3000r/min, centrifugation point
From 5~8min, upper liquid is removed, fiber gel liquid is obtained, then fiber gel liquid is put into freeze drier, -35~-30
It is freeze-dried 30~35min under the conditions of DEG C temperature, obtains medical collagen sponge.
6g sodium alginate is taken to be added in the beaker equipped with 200mL deionized water, with magnetic stirring apparatus turning with 500r/min
Speed stirring, until sodium alginate dissolve, obtain mass fraction be 2% sodium alginate soln, by 3g sodium metaperiodate be dissolved in 10g go from
In sub- water, oxidation solution is obtained；Above-mentioned oxidation solution is fitted into the three-necked flask with dropping funel and blender, starting stirring
Device starts to stir with the revolving speed of 300r/min, then above-mentioned sodium alginate soln is fitted into dropping funel, with the drop of 4mL/min
Sodium alginate soln is added dropwise into three-necked flask for rate of acceleration, after being added dropwise, three-necked flask is placed under the conditions of being protected from light, under room temperature
20h is reacted, oxidized sodium alginate is obtained；4mL ethylene glycol is added to above-mentioned oxidized sodium alginate, terminates reaction 2h, adds
0.8g sodium chloride, obtains mixed liquor, and mixed liquor is fitted into bag filter, and control molecular cut off is 12000D, is kept away with distilled water
Light is dialysed 3 days, is changed water 3 times daily, is obtained dialysis purification liquid, dialysis purification liquid is put into freeze drier, in -40 DEG C of temperature
Lower freeze-drying 40min, obtains White Flocculus；70g bamboo fibre is placed in a beaker, 100mL mass point is added into beaker
Sodium hydroxide solution, 8g sodium sulfite, 10g sodium pyrophosphate of the number for 45%, place the beaker in water-bath, with the liter of 2 DEG C/min
Warm rate is heated to 80 DEG C, keeps the temperature 1h, is cooled to 40 DEG C, continues to keep the temperature 30min, obtains degumming bamboo fibre, prepares quality
White Flocculus, carboxymethyl chitosan sugar aqueous solution, degumming bamboo fibre are pressed quality by the carboxymethyl chitosan sugar aqueous solution that score is 6%
Than being mixed for 1 ︰ 4,20min is mixed and obtains oxidation hydrogel；Gelatin solution, 2mL sorb by 10mL mass fraction for 20%
Alcohol acid anhydride monoleate, 4g chloramphenicol, 4g hydroxymethyl cellulose are mixed to get antibacterial gelatin solution, and 10g is added into antibacterial gelatin solution
Cobweb, 20g ox heel string, 0.6g trypsase are mixed enzymatic hydrolysis 20min, obtain sticky glue, be heated to 60 DEG C,
With the revolving speed stirring and emulsifying 10min of 800r/min, collagen liquid is obtained；Above-mentioned collagen liquid and oxidation hydrogel are pressed into body
It is long-pending to be put into beaker than being mixed for 4 ︰ 1, mixed glue solution is obtained, is placed the beaker in ice-water bath, is added after cooling 7min into beaker
Enter the glutaraldehyde solution that 1mL mass fraction is 50%, crosslinking curing 40min, then 30mL acetone is added into beaker, is mixed
Above-mentioned mixing suspension is put into the revolving speed in supercentrifuge with 2500r/min by suspension, is centrifugated 5min, in removal
Layer liquid, obtains fiber gel liquid, then fiber gel liquid is put into freeze drier, is freeze-dried under the conditions of -35 DEG C of temperature
30min obtains medical collagen sponge.
8g sodium alginate is taken to be added in the beaker equipped with 220mL deionized water, with magnetic stirring apparatus turning with 520r/min
Speed stirring, until sodium alginate dissolve, obtain mass fraction be 3% sodium alginate soln, by 3g sodium metaperiodate be dissolved in 11g go from
In sub- water, oxidation solution is obtained；Above-mentioned oxidation solution is fitted into the three-necked flask with dropping funel and blender, starting stirring
Device starts to stir with the revolving speed of 400r/min, then above-mentioned sodium alginate soln is fitted into dropping funel, with the drop of 5mL/min
Sodium alginate soln is added dropwise into three-necked flask for rate of acceleration, after being added dropwise, three-necked flask is placed under the conditions of being protected from light, under room temperature
22h is reacted, oxidized sodium alginate is obtained；4mL ethylene glycol is added to above-mentioned oxidized sodium alginate, terminates reaction 2.5h, adds
0.9g sodium chloride, obtains mixed liquor, and mixed liquor is fitted into bag filter, and control molecular cut off is 13000D, is kept away with distilled water
Light is dialysed 4 days, is changed water 3 times daily, is obtained dialysis purification liquid, dialysis purification liquid is put into freeze drier, in -30 DEG C of temperature
Lower freeze-drying 42min, obtains White Flocculus；75g bamboo fibre is placed in a beaker, 120mL mass point is added into beaker
Sodium hydroxide solution, 9g sodium sulfite, 11g sodium pyrophosphate of the number for 45%, place the beaker in water-bath, with the liter of 2 DEG C/min
Warm rate is heated to 85 DEG C, keeps the temperature 1.5h, is cooled to 42 DEG C, continues to keep the temperature 32min, obtains degumming bamboo fibre, prepares matter
The carboxymethyl chitosan sugar aqueous solution that score is 6% is measured, White Flocculus, carboxymethyl chitosan sugar aqueous solution, degumming bamboo fibre are pressed into matter
Amount is mixed 25min and obtains oxidation hydrogel than being that 1 ︰ 4 is mixed；Gelatin solution, the mountain 2mL by 12mL mass fraction for 20%
Pears alcohol acid anhydride monoleate, 5g chloramphenicol, 4g hydroxymethyl cellulose are mixed to get antibacterial gelatin solution, are added into antibacterial gelatin solution
12g cobweb, 22g ox heel string, 0.7g trypsase are mixed enzymatic hydrolysis 22min, obtain sticky glue, be heated to 62
DEG C, with the revolving speed stirring and emulsifying 12min of 900r/min, obtain collagen liquid；By above-mentioned collagen liquid and oxidation hydrogel
It is put into beaker for 4 ︰ 1 mixing by volume, obtains mixed glue solution, place the beaker in ice-water bath, to beaker after cooling 8min
The middle glutaraldehyde solution that 2mL mass fraction is added and is 50%, crosslinking curing 45min, then 40mL acetone is added into beaker, it obtains
Above-mentioned mixing suspension is put into the revolving speed in supercentrifuge with 2700r/min, is centrifugated 7min, goes by mixing suspension
Except upper liquid, fiber gel liquid is obtained, then fiber gel liquid is put into freeze drier, is freezed under the conditions of -32 DEG C of temperature
Dry 32min, obtains medical collagen sponge.
10g sodium alginate is taken to be added in the beaker equipped with 250mL deionized water, with magnetic stirring apparatus turning with 550r/min
Speed stirring, until sodium alginate dissolve, obtain mass fraction be 4% sodium alginate soln, by 4g sodium metaperiodate be dissolved in 10g go from
In sub- water, oxidation solution is obtained；Above-mentioned oxidation solution is fitted into the three-necked flask with dropping funel and blender, starting stirring
Device starts to stir with the revolving speed of 500r/min, then above-mentioned sodium alginate soln is fitted into dropping funel, with the drop of 6mL/min
Sodium alginate soln is added dropwise into three-necked flask for rate of acceleration, after being added dropwise, three-necked flask is placed under the conditions of being protected from light, under room temperature
Reaction for 24 hours, obtains oxidized sodium alginate；5mL ethylene glycol is added to above-mentioned oxidized sodium alginate, terminates reaction 3h, adds
1.0g sodium chloride, obtains mixed liquor, and mixed liquor is fitted into bag filter, and control molecular cut off is 14000D, is kept away with distilled water
Light is dialysed 5 days, is changed water 4 times daily, is obtained dialysis purification liquid, dialysis purification liquid is put into freeze drier, in -20 DEG C of temperature
Lower freeze-drying 45min, obtains White Flocculus；80g bamboo fibre is placed in a beaker, 130mL mass point is added into beaker
Sodium hydroxide solution, 10g sodium sulfite, 12g sodium pyrophosphate of the number for 45%, place the beaker in water-bath, with 2 DEG C/min's
Heating rate is heated to 90 DEG C, keeps the temperature 2h, is cooled to 45 DEG C, continues to keep the temperature 35min, obtains degumming bamboo fibre, prepares matter
The carboxymethyl chitosan sugar aqueous solution that score is 6% is measured, White Flocculus, carboxymethyl chitosan sugar aqueous solution, degumming bamboo fibre are pressed into matter
Amount is mixed 30min and obtains oxidation hydrogel than being that 1 ︰ 4 is mixed；Gelatin solution, the mountain 3mL by 15mL mass fraction for 20%
Pears alcohol acid anhydride monoleate, 6g chloramphenicol, 5g hydroxymethyl cellulose are mixed to get antibacterial gelatin solution, are added into antibacterial gelatin solution
15g cobweb, 25g ox heel string, 0.8g trypsase are mixed enzymatic hydrolysis 25min, obtain sticky glue, be heated to 65
DEG C, with the revolving speed stirring and emulsifying 15min of 1000r/min, obtain collagen liquid；By above-mentioned collagen liquid and oxidation hydrogel
It is put into beaker for 4 ︰ 1 mixing by volume, obtains mixed glue solution, place the beaker in ice-water bath, to beaker after cooling 10min
The middle glutaraldehyde solution that 3mL mass fraction is added and is 50%, crosslinking curing 50min, then 50mL acetone is added into beaker, it obtains
Above-mentioned mixing suspension is put into the revolving speed in supercentrifuge with 3000r/min, is centrifugated 8min, goes by mixing suspension
Except upper liquid, fiber gel liquid is obtained, then fiber gel liquid is put into freeze drier, is freezed under the conditions of -30 DEG C of temperature
Dry 35min, obtains medical collagen sponge.
The medical collagen sponge that comparative example is produced with Wuxi company is as a comparison case to produced by the present invention medical
Medical collagen sponge in collagen protein sponge and comparative example carries out performance detection, and testing result is as shown in table 1:
Test method:
Cell toxicity test presses the cytotoxicity grade of GB/T 16886.5-2003 standard detection collagen protein sponge.
Bacterial endotoxin test presses the bacterial endotoxin of EN455-3-2000 standard detection collagen protein sponge.
Using sponge sucks in water, rate tester is detected water absorption rate test.
Bleeding and diffusate measure of merit are absorbed when for being applied with processing wound: by the collagen in example 1~3 and comparative example
Protein sponge measures bleeding stopping period and amount of bleeding for being applied with wound.
Expansion multiplying power test is detected by 10802 standard of GB/T.
1 medical collagen sponge performance measurement result of table
Good, the collagen protein sponge according to the antibacterial anti-infectious effect of above-mentioned detection data medical collagen sponge of the invention
Cytotoxin it is low, intracellular toxin is low, and water absorption rate is high, and minimum of bleeding stopping period need 80 seconds, amount of bleeding is low, handles for external application
Bleeding is absorbed when wound and diffusate effect is good, and water swelling multiplying power is high, has broad application prospects.
Claims (7)
1. a kind of preparation method of medical collagen sponge, it is characterised in that specific preparation step are as follows:
(1) 6~10g sodium alginate is taken to be added in the beaker equipped with 200~250mL deionized water, with magnetic stirrer, directly
It is dissolved to sodium alginate, obtains sodium alginate soln, 3~4g sodium metaperiodate is dissolved in 10~12g deionized water, is aoxidized
Liquid；
(2) above-mentioned oxidation solution is fitted into the three-necked flask with dropping funel and blender, starts blender, with 300~
The revolving speed of 500r/min starts to stir, then above-mentioned sodium alginate soln is fitted into dropping funel, and sea is added dropwise into three-necked flask
Solution of sodium alginate after being added dropwise, is placed on three-necked flask under the conditions of being protected from light, reacts under room temperature, obtain oxidized sodium alginate；
(3) 4~5mL ethylene glycol is added to above-mentioned oxidized sodium alginate, terminates reaction, adds 0.8~1.0g sodium chloride, obtain
Mixed liquor is fitted into bag filter by mixed liquor, is protected from light dialysis 3~5 days with distilled water, is changed water 3~4 times daily, is obtained dialysing pure
Change liquid, dialysis purification liquid is put into freeze drier, is freeze-dried, obtains White Flocculus；
(4) 70~80g bamboo fibre is placed in a beaker, it is sub- that 100~130mL sodium hydroxide solution, 8~10g is added into beaker
Sodium sulphate, 10~12g sodium pyrophosphate, place the beaker in water-bath, heat temperature raising, keep the temperature 1~2h, and cooling continues heat preservation 30
~35min obtains degumming bamboo fibre, White Flocculus, carboxymethyl chitosan sugar aqueous solution, degumming bamboo fibre is mixed, mixing is stirred
It mixes 20~30min and obtains oxidation hydrogel；
(5) by 10~15mL gelatin solution, 2~3mL sorbitan mono-oleic acid ester, 4~6g chloramphenicol, 4~5g hydroxylmethyl cellulose
Element is mixed to get antibacterial gelatin solution, and 10~15g cobweb, 20~25g ox heel string, 0.6~0.8g are added into antibacterial gelatin solution
Trypsase is mixed 20~25min of enzymatic hydrolysis, obtains sticky glue, heat temperature raising is stirred with the revolving speed of 800~1000r/min
10~15min of emulsification is mixed, collagen liquid is obtained；
(6) above-mentioned collagen liquid is mixed with oxidation hydrogel and is put into beaker, obtained mixed glue solution, place the beaker ice
In water-bath, it is added 1~3mL glutaraldehyde solution after cooling 7~10min into beaker, 40~50min of crosslinking curing, then to beaker
Middle addition 30~50mL acetone, obtains mixing suspension, above-mentioned mixing suspension is put into supercentrifuge, centrifuge separation 5
~8min removes upper liquid, obtains fiber gel liquid, then fiber gel liquid is put into freeze drier, freeze-drying obtains
Medical collagen sponge.
2. a kind of preparation method of medical collagen sponge according to claim 1, it is characterised in that: step (1) institute
The magnetic agitation rotating speed stated is 500~550r/min, and the mass fraction of sodium alginate soln is 2~4%.
3. a kind of preparation method of medical collagen sponge according to claim 1, it is characterised in that: step (2) institute
The dropping funel drop rate stated be 4~6mL/min, under the conditions of being protected from light the normal-temperature reaction time be 20~for 24 hours.
4. a kind of preparation method of medical collagen sponge according to claim 1, it is characterised in that: step (3) institute
The termination reaction time stated be 2~3h, bag filter control molecular cut off be 12000~14000D, freeze-drying temperature be-
40~-20 DEG C, sublimation drying is 40~45min.
5. a kind of preparation method of medical collagen sponge according to claim 1, it is characterised in that: step (4) institute
The mass fraction for the sodium hydroxide solution stated is 45%, and oil bath pan heating rate is 2 DEG C/min, after heat temperature raising temperature be 80~
90 DEG C, temperature is 40~45 DEG C after cooling, and the mass fraction of carboxymethyl chitosan sugar aqueous solution is 6%, White Flocculus, carboxymethyl
Chitosan aqueous solution, degumming bamboo fibre mixing mass ratio are 1 ︰, 4 ︰ 5.
6. a kind of preparation method of medical collagen sponge according to claim 1, it is characterised in that: step (5) institute
The mass fraction for the gelatin solution stated is 20%, and temperature is 60~65 DEG C after heat temperature raising.
7. a kind of preparation method of medical collagen sponge according to claim 1, it is characterised in that: step (6) institute
The collagen liquid stated and oxidation hydrogel mixed volume ratio are 4 ︰ 1, and the mass fraction of glutaraldehyde solution is 50%, at a high speed from
Heart revolving speed is 2500~3000r/min, and freeze-drying temperature is -35~-30 DEG C, and sublimation drying is 30~35min.
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