CN107899069A - A kind of preparation method of medical collagen complex stephanoporate bracket - Google Patents
A kind of preparation method of medical collagen complex stephanoporate bracket Download PDFInfo
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- CN107899069A CN107899069A CN201711113528.XA CN201711113528A CN107899069A CN 107899069 A CN107899069 A CN 107899069A CN 201711113528 A CN201711113528 A CN 201711113528A CN 107899069 A CN107899069 A CN 107899069A
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- magnesium silk
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- mixed liquor
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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
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
- A61L27/58—Materials at least partially 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
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/02—Inorganic materials
- A61L27/04—Metals or alloys
- A61L27/047—Other specific metals or alloys not covered by A61L27/042 - A61L27/045 or A61L27/06
-
- 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
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/02—Inorganic materials
- A61L27/12—Phosphorus-containing materials, e.g. apatite
-
- 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
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/14—Macromolecular materials
- A61L27/22—Polypeptides or derivatives thereof, e.g. degradation products
- A61L27/24—Collagen
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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
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
-
- 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
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
- A61L27/56—Porous materials, e.g. foams or sponges
-
- 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
- A61L2430/00—Materials or treatment for tissue regeneration
- A61L2430/06—Materials or treatment for tissue regeneration for cartilage reconstruction, e.g. meniscus
Abstract
The invention discloses a kind of preparation method of medical collagen complex stephanoporate bracket, belong to Medical rack preparing technical field.The present invention is first by after phosphatide and stirring solvent dissolving, it is concentrated under reduced pressure, concentrate is made, ultrasonic disperse after concentrate is mixed with buffer solution again, again through Frozen-thawed cycled, obtain mixed liquor, then magnesium silk is polished and is cut, and with acetone, second alcohol and water cleans, reacted again with oxidation mixed liquor heating, the pretreatment short fibre of magnesium silk is made, then short fine be mixed with dipping with mixed liquor of pretreatment magnesium silk is modified, finally and collagen, water and pretreatment calcium hydroxy phosphate are stirred, through refrigeration, freezing, after drying, soaked successively with absolute ethyl alcohol and sodium hydroxide solution, it is washed again, up to medical collagen complex stephanoporate bracket.Gained collagen scaffold of the invention has higher porosity and elasticity modulus.
Description
Technical field
The invention discloses a kind of preparation method of medical collagen complex stephanoporate bracket, belongs to Medical rack and prepares skill
Art field.
Background technology
Collagen is a kind of very important protein, for human skin, blood vessel, bone, tendon, tooth and cartilage
Formation play an important roll, be these connective tissues main matter basis.Cognition of the ordinary people for collagen is most
Health care of food aspect is rested on, as the health treatment for improving immunity, slowing down aging.And come for medical researchers
Say, collagen is huger in the application potential of medical field, especially collagen scaffold technology, even more possesses very wide
Wealthy prospect.
As a kind of ideal material of Bionics application, collagen has very strong stretch capability, can be used as laboratory or
The important materials of regeneration in clinic.The collagen of loose structure can be used as " stent ", make to depend on cell thereon and group
Knit by it is a kind of it is predetermined in the form of grow, ultimately become the tissue extremely similar to required tissue.This is so-called collagen
Protein scaffold technology.
Clinical treatment articular cartilage damage is mainly transplanted using autologous or allogeneic cartilage at present, but is existed and damaged for area
Wound, newly form the defects of tissue comprehensive performance is not good enough.The fast development of organizational engineering provides new think of for cartilage damage reparation
Road.At present, a large number of researchers be directed to seeking it is a kind of there is excellent hole, mechanical property is good, good biocompatibility three-dimensional is more
Hole timbering material.In numerous materials, fibroin albumen and collagen are research hotspots as natural biologic material.Fibroin albumen
With good biocompatibility；Collagen is the natural component of osteochondral tissue, in the tendon of the animals such as ox, its
Contain amino acid and protein structure sequence in structure sequence itself, cell adhesion and protein expression can be promoted.Collagen degradation
Speed is fast, but mechanical strength is insufficient, easily fragmentation.Current collagen scaffold also there are mechanical property it is bad the problem of,
Therefore also need to study it.
The content of the invention
The present invention solves the technical problem of：For traditional collagen scaffold porosity is low, mechanical property is bad
The problem of, there is provided a kind of preparation method of medical collagen complex stephanoporate bracket.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is：
（1）It is 1 in mass ratio by phosphatide and solvent：40~1：50 stirring and dissolvings, then through being concentrated under reduced pressure, obtain concentrate；
（2）It is 1 by volume by concentrate and buffer solution：20~1：Ultrasonic disperse after 25 mixing, then through Frozen-thawed cycled 3~5 times,
Obtain mixed liquor；
（3）The short fibre of magnesium silk is cut into after magnesium silk is polished, then magnesium silk is short fine clear with acetone, absolute ethyl alcohol and water ultrasound successively
Wash, and be 1 in mass ratio by the short fibre of the magnesium silk after washing and oxidation mixed liquor：5~1：10 heating reactions, are filtered, washing, obtains pre-
Handle the short fibre of magnesium silk；
（4）It is 1 in mass ratio by the short fine and mixed liquor of pretreatment magnesium silk：10~1：After 15 mixing, insulation dipping, is filtered, washing,
The short fibre of magnesium silk must be modified；
（5）Count in parts by weight, take 20~30 parts of collagens successively, 150~200 parts of water, 10~15 parts of short fibres of modified magnesium silk,
20~30 parts of pretreatment calcium hydroxy phosphates, after being stirred, move into orifice plate, after refrigerating 2~4h, freeze 8~12h, then through true
Vacuum freecing-dry, obtains drying bracket blank；
（6）Drying bracket blank is soaked with absolute ethyl alcohol and sodium hydroxide solution successively, then is washed with deionized, up to curing
With collagen complex stephanoporate bracket.
Step（1）The phosphatide is any one in egg yolk lecithin or soybean lecithin.
Step（1）The solvent is that chloroform, methanol and triethylamine are 10 in mass ratio：7：1 configuration forms.
Step（2）The buffer solution is the phosphate buffer that pH is 7.2~7.4.
Step（3）The magnesium silk is a diameter of 0.02~0.04mm, and length is 8~10cm.
Step（3）It is 1 in mass ratio by citric acid, hydrogen peroxide and water that the oxidation mixed liquor, which is,：1：8 configurations form.
Step（5）It is described pretreatment calcium hydroxy phosphate preprocessing process be：It is with mass concentration by nano-hydroxy phosphoric acid calcium
After the mixing of 2.0~2.2g/L dopamine solutions, pH to 8.0~8.2,45~60min of sonic oscillation are adjusted with sodium hydroxide solution,
Filtering, washing, obtains pretreatment calcium hydroxy phosphate.
Step（5）The orifice plate is any one in 12 orifice plates, 24 orifice plates or 96 orifice plates.
The beneficial effects of the invention are as follows：
（1）Technical solution of the present invention with the modification magnesium silk of homemade loose structure it is short fibre for substrate, using aoxidize mixed liquor into
In row processing procedure, first, weakly acidic environment can carry out micro- corruption to magnesium silk, make magnesium silk that loose structure be presented, in addition, aoxidizing
Under environment, oxide-film can be formed in magnesium silk table face and pore structure, so as to be conducive to the deposition of phospholipid molecule, phospholipid bilayer
Formation in system, on the one hand, can make pretreatment calcium hydroxy phosphate by the bridge joint function well scattered adsorption of dopamine in
System phospholipid molecule layer surface, on the other hand, phospholipid molecule and collagen have an excellent compatibility, phospholipid molecule band in itself
There is negative electrical charge, Electrostatic Absorption can be produced with collagen, collagen is fixed in system, so that magnesium silk, phosphorus in system
Fat molecule, collagen molecules and nanometer hydroxyapatite form organic whole, system mechanical property is effectively lifted, then
Person, phosphatide has two kinds of groups of hydrophilic and oleophilic, therefore can play the role of reducing viscosity by emulsifying in system, and makes collagen can be in base
The good wetting and spreading in body surface face, and in whipping process, air can be made to be scattered in the form of micro-bubble in system, in system
Lotion is internally formed, in freezing dry process, gas is internally formed porous knot with moisture evaporation, and in system in lotion bubble
Structure, further lifts system interior porosity；
（2）In technical solution of the present invention, the use of magnesium silk on the one hand can be as the mechanical property of matrix raising system, the opposing party
The inducible factor that face, magnesium and calcium hydroxy phosphate can be grown as body bone tissue, is conducive to the regeneration of bone tissue, and present invention production
Use raw material most of for degradable raw material in product, harmful effect will not be caused to human body.
Embodiment
It is 1 in mass ratio：10~1：Nano-hydroxy phosphoric acid calcium and mass concentration are 2.0~2.2g/L dopamine solutions by 15
Pour into beaker, after being stirred 10~15min with glass bar, with mass fraction for 6~8% sodium hydroxide solutions adjust pH to
8.0~8.2, then beaker is moved into sonic oscillation instrument, under the conditions of supersonic frequency is 45~55kHz, sonic oscillation 45~
60min, filtering, obtain filter cake, and be washed with deionized filter cake until cleaning solution be in neutrality, obtain pretreatment calcium hydroxy phosphate；Will
Phosphatide is 1 in mass ratio with solvent：40~1：50 stirring and dissolvings, obtain phosphatide liquid, and gained phosphatide liquid is transferred to Rotary Evaporators,
It it is 75~80 DEG C in temperature, under the conditions of pressure is 500~600kPa, be concentrated under reduced pressure 4~6h, obtains concentrate；By gained concentrate
It is 1 by volume with buffer solution：20~1：After 25 mixing, under the conditions of supersonic frequency is 55~60kHz, 2~3h of ultrasonic disperse,
Dispersion liquid is obtained, and gained dispersion liquid is moved into refrigerator, after freezing 4~6h under the conditions of being -20~-18 DEG C in temperature, is solved naturally
Freeze 6~8h, such freeze-thaw circulation 3~5 times, obtains mixed liquor；After magnesium silk is polished with abrasive paper for metallograph, length is cut into as 3
The short fibre of~5mm magnesium silks, then gained magnesium silk is short fine successively with acetone, absolute ethyl alcohol and water ultrasonic cleaning, setting ultrasonic cleaning frequency
Rate is 45~55kHz, 30~45min of single wash, must wash the short fibre of magnesium silk, then will the short fibre of washing magnesium silk and oxidation mix acid liquor
It is 1 in mass ratio：5~1：10 mixing are poured into beaker, and beaker immigration digital display is tested the speed constant temperature blender with magnetic force, are in temperature
45~50 DEG C, rotating speed be 300~500r/min under the conditions of, constant temperature stirring reaction 10~15min, filtering, obtain filter residue, and spend from
Sub- water washing filter residue is in neutrality up to cleaning solution, must pre-process the short fibre of magnesium silk；It is 1 in mass ratio：10~1：15 will pre-process magnesium
Short fibre of silk mix with mixed liquor, under the conditions of temperature is 55~60 DEG C, is kept the temperature and is impregnated 8~12h, filters, obtain filter cake, and spend from
Sub- water washing filter cake 3~5 times, obtains the modified short fibre of magnesium silk；Count in parts by weight, take 20~30 parts of collagens successively, 150~
200 parts of water, 10~15 parts of short fibres of modified magnesium silk, 20~30 parts of pretreatment calcium hydroxy phosphates, pour into batch mixer, are in rotating speed
Under the conditions of 800~1200r/min, after being stirred 3~5h, material in batch mixer is moved into orifice plate, and by orifice plate in temperature
To refrigerate 2~4h under the conditions of 2~4 DEG C, then by the orifice plate after refrigeration be -20~-18 DEG C in temperature under the conditions of freeze 3~5h, then
Through vacuum freeze drying, discharging, obtains drying bracket blank；Drying bracket blank is continued with after 3~5h of soaked in absolute ethyl alcohol again
6~8h is soaked for 20% sodium hydroxide solution with mass fraction, obtains alkali leaching stent blank, then alkali leaching stent is washed with deionized
Blank is until cleaning solution is in neutrality, up to medical collagen complex stephanoporate bracket.The phosphatide is egg yolk lecithin or soybean
Any one in lecithin.The solvent is that chloroform, methanol and triethylamine are 10 in mass ratio：7：1 configuration forms.The buffering
Liquid is the phosphate buffer that pH is 7.2~7.4.The magnesium silk is a diameter of 0.02~0.04mm, and length is 8~10cm.It is described
It is 1 in mass ratio by citric acid, hydrogen peroxide and water that oxidation mixed liquor, which is,：1：8 configurations form.The orifice plate is 12 orifice plates, 24 holes
Any one in plate or 96 orifice plates.
Example 1
It is 1 in mass ratio：15 pour into nano-hydroxy phosphoric acid calcium and mass concentration in beaker for 2.2g/L dopamine solutions, use glass
After glass rod is stirred 15min, pH is adjusted to 8.2 for 8% sodium hydroxide solution with mass fraction, then beaker immigration ultrasound is shaken
Instrument is swung, under the conditions of supersonic frequency is 55kHz, sonic oscillation 60min, filtering, obtains filter cake, and it is straight that filter cake is washed with deionized
It is in neutrality to cleaning solution, obtains pretreatment calcium hydroxy phosphate；It is 1 in mass ratio by phosphatide and solvent：50 stirring and dissolvings, obtain phosphatide
Liquid, and gained phosphatide liquid is transferred to Rotary Evaporators, it is 80 DEG C in temperature, under the conditions of pressure is 600kPa, be concentrated under reduced pressure 6h, obtains
Concentrate；It is 1 by volume by gained concentrate and buffer solution：After 25 mixing, under the conditions of supersonic frequency is 60kHz, ultrasound
Scattered 3h, obtains dispersion liquid, and gained dispersion liquid is moved into refrigerator, after freezing 6h under the conditions of being -18 DEG C in temperature, naturally to thaw
8h, such freeze-thaw circulation 5 times, obtains mixed liquor；After magnesium silk is polished with abrasive paper for metallograph, it is short for 5mm magnesium silks to cut into length
Fibre, then gained magnesium silk is short fine successively with acetone, absolute ethyl alcohol and water ultrasonic cleaning, ultrasonic cleaning frequency is set as 55kHz, list
Secondary washing 45min, must wash the short fibre of magnesium silk, then it is 1 in mass ratio that will wash the short fibre of magnesium silk with oxidation mix acid liquor：10 mixing are fallen
Enter in beaker, and beaker immigration digital display is tested the speed constant temperature blender with magnetic force, be 50 DEG C in temperature, rotating speed is 500r/min conditions
Under, constant temperature stirring reaction 15min, filtering, obtain filter residue, and be washed with deionized filter residue until cleaning solution be in neutrality, obtain pre- place
Manage the short fibre of magnesium silk；It is 1 in mass ratio：15 mix the pretreatment short fibre of magnesium silk with mixed liquor, under the conditions of temperature is 60 DEG C, insulation
12h is impregnated, filtering, obtains filter cake, and filter cake is washed with deionized 5 times, obtains the modified short fibre of magnesium silk；Count in parts by weight, successively
30 parts of collagens are taken, 200 parts of water, 15 parts of short fibres of modified magnesium silk, 30 parts of pretreatment calcium hydroxy phosphates, are poured into batch mixer, in
Rotating speed be 1200r/min under the conditions of, after being stirred 5h, by batch mixer material move into orifice plate in, and by orifice plate in temperature be 4
4h is refrigerated under the conditions of DEG C, then the orifice plate after refrigeration is freezed into 5h under the conditions of temperature is -18 DEG C, then through vacuum freeze drying, is gone out
Material, obtains drying bracket blank；It is again 20% hydrogen-oxygen with after soaked in absolute ethyl alcohol 5h, continuing with mass fraction by drying bracket blank
Change sodium solution immersion 8h, obtain alkali leaching stent blank, then alkali leaching stent blank is washed with deionized until cleaning solution is in neutrality, i.e.,
Obtain medical collagen complex stephanoporate bracket.The phosphatide is egg yolk lecithin.The solvent is pressed for chloroform, methanol and triethylamine
Mass ratio is 10：7：1 configuration forms.The buffer solution is the phosphate buffer that pH is 7.4.The magnesium silk is a diameter of
0.04mm, length 10cm.It is 1 in mass ratio by citric acid, hydrogen peroxide and water that the oxidation mixed liquor, which is,：1：8 configurations form.
The orifice plate is 12 orifice plates.
Example 2
It is 1 in mass ratio：15 pour into nano-hydroxy phosphoric acid calcium and mass concentration in beaker for 2.2g/L dopamine solutions, use glass
After glass rod is stirred 15min, pH is adjusted to 8.2 for 8% sodium hydroxide solution with mass fraction, then beaker immigration ultrasound is shaken
Instrument is swung, under the conditions of supersonic frequency is 55kHz, sonic oscillation 60min, filtering, obtains filter cake, and it is straight that filter cake is washed with deionized
It is in neutrality to cleaning solution, obtains pretreatment calcium hydroxy phosphate；After magnesium silk is polished with abrasive paper for metallograph, it is 5mm magnesium silks to cut into length
Short fibre, then the short fibre of gained magnesium silk is cleaned by ultrasonic with acetone, absolute ethyl alcohol and water successively, set and be cleaned by ultrasonic frequency as 55kHz,
Single wash 45min, must wash the short fibre of magnesium silk, then it is 1 in mass ratio that will wash the short fibre of magnesium silk with oxidation mix acid liquor：10 mixing
Pour into beaker, and beaker immigration digital display is tested the speed constant temperature blender with magnetic force, be 50 DEG C in temperature, rotating speed is 500r/min conditions
Under, constant temperature stirring reaction 15min, filtering, obtain filter residue, and be washed with deionized filter residue until cleaning solution be in neutrality, obtain pre- place
Manage the short fibre of magnesium silk；Count in parts by weight, take 30 parts of collagens successively, 200 parts of water, 15 parts of pretreatment short fibres of magnesium silk, 30 parts pre-
Calcium hydroxy phosphate is handled, is poured into batch mixer, under the conditions of rotating speed is 1200r/min, after being stirred 5h, by thing in batch mixer
Material is moved into orifice plate, and by orifice plate be 4 DEG C in temperature under the conditions of refrigerate 4h, then by the orifice plate after refrigeration in temperature be -18 DEG C of bars
5h is freezed under part, then through vacuum freeze drying, discharging, obtains drying bracket blank；Drying bracket blank is soaked with absolute ethyl alcohol again
After steeping 5h, continue to soak 8h with mass fraction for 20% sodium hydroxide solution, obtain alkali leaching stent blank, then be washed with deionized
Alkali leaching stent blank is until cleaning solution is in neutrality, up to medical collagen complex stephanoporate bracket.The solvent is chloroform, methanol
It is 10 in mass ratio with triethylamine：7：1 configuration forms.The buffer solution is the phosphate buffer that pH is 7.4.The magnesium silk is straight
Footpath is 0.04mm, length 10cm.It is 1 in mass ratio by citric acid, hydrogen peroxide and water that the oxidation mixed liquor, which is,：1：8 configurations
Form.The orifice plate is 12 orifice plates.
Example 3
It is 1 in mass ratio by phosphatide and solvent：50 stirring and dissolvings, obtain phosphatide liquid, and gained phosphatide liquid is transferred to Rotary Evaporators,
It it is 80 DEG C in temperature, under the conditions of pressure is 600kPa, be concentrated under reduced pressure 6h, obtains concentrate；Gained concentrate and buffer solution are pressed into body
Product is than being 1：After 25 mixing, under the conditions of supersonic frequency is 60kHz, ultrasonic disperse 3h, obtains dispersion liquid, and gained dispersion liquid is moved
Enter in refrigerator, after freezing 6h under the conditions of being -18 DEG C in temperature, naturally to thaw 8h, such freeze-thaw circulation 5 times, obtains mixed liquor；
After magnesium silk is polished with abrasive paper for metallograph, it is the short fibre of 5mm magnesium silks to cut into length, then gained magnesium silk is short fine successively with acetone, nothing
Water-ethanol and water are cleaned by ultrasonic, and set and are cleaned by ultrasonic frequency as 55kHz, single wash 45min, must wash the short fibre of magnesium silk, then will
It is 1 in mass ratio that the short fibre of magnesium silk, which is washed, with oxidation mix acid liquor：10 mixing are poured into beaker, and beaker immigration digital display is tested the speed perseverance
Warm magnetic stirring apparatus, is 50 DEG C in temperature, and under the conditions of rotating speed is 500r/min, constant temperature stirring reaction 15min, filtering, obtains filter residue,
And be washed with deionized filter residue until cleaning solution be in neutrality, the short fibre of magnesium silk must be pre-processed；It is 1 in mass ratio：15 will pretreatment
The short fibre of magnesium silk is mixed with mixed liquor, and under the conditions of temperature is 60 DEG C, insulation dipping 12h, filtering, obtains filter cake, and use deionized water
Wash filter cake 5 times, obtain the modified short fibre of magnesium silk；Count in parts by weight, take 30 parts of collagens, 200 parts of water, 15 parts of modified magnesium successively
The short fibre of silk, is poured into batch mixer, and under the conditions of rotating speed is 1200r/min, after being stirred 5h, material in batch mixer is moved into hole
In plate, and orifice plate is refrigerated into 4h under the conditions of temperature is 4 DEG C, then the orifice plate after refrigeration is freezed under the conditions of temperature is -18 DEG C
5h, then through vacuum freeze drying, discharging, obtains drying bracket blank；Again by drying bracket blank with after soaked in absolute ethyl alcohol 5h, after
It is continuous to soak 8h with mass fraction for 20% sodium hydroxide solution, alkali leaching stent blank is obtained, then alkali leaching stent base is washed with deionized
Material is until cleaning solution is in neutrality, up to medical collagen complex stephanoporate bracket.The phosphatide is egg yolk lecithin.The solvent
It is 10 in mass ratio for chloroform, methanol and triethylamine：7：1 configuration forms.The buffer solution is the phosphate buffer that pH is 7.4.
The magnesium silk is a diameter of 0.04mm, length 10cm.It is described oxidation mixed liquor be by citric acid, hydrogen peroxide and water in mass ratio
For 1：1：8 configurations form.The orifice plate is 12 orifice plates.
Example 4
It is 1 in mass ratio by phosphatide and solvent：50 stirring and dissolvings, obtain phosphatide liquid, and gained phosphatide liquid is transferred to Rotary Evaporators,
It it is 80 DEG C in temperature, under the conditions of pressure is 600kPa, be concentrated under reduced pressure 6h, obtains concentrate；Gained concentrate and buffer solution are pressed into body
Product is than being 1：After 25 mixing, under the conditions of supersonic frequency is 60kHz, ultrasonic disperse 3h, obtains dispersion liquid, and gained dispersion liquid is moved
Enter in refrigerator, after freezing 6h under the conditions of being -18 DEG C in temperature, naturally to thaw 8h, such freeze-thaw circulation 5 times, obtains mixed liquor；
After magnesium silk is polished with abrasive paper for metallograph, it is the short fibre of 5mm magnesium silks to cut into length, then gained magnesium silk is short fine successively with acetone, nothing
Water-ethanol and water are cleaned by ultrasonic, and set and are cleaned by ultrasonic frequency as 55kHz, single wash 45min, must wash the short fibre of magnesium silk, then will
It is 1 in mass ratio that the short fibre of magnesium silk, which is washed, with oxidation mix acid liquor：10 mixing are poured into beaker, and beaker immigration digital display is tested the speed perseverance
Warm magnetic stirring apparatus, is 50 DEG C in temperature, and under the conditions of rotating speed is 500r/min, constant temperature stirring reaction 15min, filtering, obtains filter residue,
And be washed with deionized filter residue until cleaning solution be in neutrality, the short fibre of magnesium silk must be pre-processed；It is 1 in mass ratio：15 will pretreatment
The short fibre of magnesium silk is mixed with mixed liquor, and under the conditions of temperature is 60 DEG C, insulation dipping 12h, filtering, obtains filter cake, and use deionized water
Wash filter cake 5 times, obtain the modified short fibre of magnesium silk；Count in parts by weight, take 30 parts of collagens, 200 parts of water, 15 parts of modified magnesium successively
The short fibre of silk, 30 parts of calcium hydroxy phosphates, are poured into batch mixer,, will be mixed after being stirred 5h under the conditions of rotating speed is 1200r/min
Material is moved into orifice plate in material machine, and orifice plate is refrigerated 4h under the conditions of temperature is 4 DEG C, then by the orifice plate after refrigeration in temperature
To freeze 5h under the conditions of -18 DEG C, then through vacuum freeze drying, discharging, obtains drying bracket blank；Again by drying bracket blank nothing
Water-ethanol immersion 5h after, continue with mass fraction for 20% sodium hydroxide solution soak 8h, obtain alkali leaching stent blank, then spend from
Sub- water washing alkali leaching stent blank is until cleaning solution is in neutrality, up to medical collagen complex stephanoporate bracket.The phosphatide is
Egg yolk lecithin.The solvent is that chloroform, methanol and triethylamine are 10 in mass ratio：7：1 configuration forms.The buffer solution is pH
For 7.4 phosphate buffer.The magnesium silk is a diameter of 0.04mm, length 10cm.It is described oxidation mixed liquor be by citric acid,
Hydrogen peroxide and water are 1 in mass ratio：1：8 configurations form.The orifice plate is 12 orifice plates.
The gained of example 1 to 4 collagen scaffold is subjected to performance detection, specific detection method is as follows：
Porosity：Using improvement liquid displacement method measure timbering material porosity.Specific steps：Select with graduated test tube,
Addition volume is V1Absolute ethyl alcohol；Drying bracket sample is cut into suitable size and is immersed 5min, negative pressure degasification to stent
Bubble-free escapes, and records ethanol volume at this time（Submerge stent）For V2；Stent sample is gently taken out, remaining ethanol volume is V3.Press
The following formula calculates brace aperture rate：（V1- V3）/（V2- V3）×100%.
Mechanical property：24h is extremely in the 0.01mol/L PBS liquid that 37 DEG C every group takes 3 drying bracket samples to be dipped in pH7.4
Balance.Stent Compressive Mechanical Properties test is carried out using Instron5865 mechanics machines, using 0.5Hz sinusoidal waveforms, is preloaded
Lotus 0.1N, maximum compression strain 10%, is circulated 3 times, draws the elasticity modulus parameter of stent
Specific testing result is as shown in table 1：
Table 1
| Detection content | Example 1 | Example 2 | Example 3 | Example 4 |
| Porosity/% | 96.2 | 60.6 | 94.6 | 93.0 |
| Elasticity modulus/kPa | 33.5 | 25.4 | 21.6 | 18.7 |
From 1 testing result of table, present invention gained collagen scaffold has higher porosity and elasticity modulus.
Claims (8)
1. a kind of preparation method of medical collagen complex stephanoporate bracket, it is characterised in that specifically preparation process is：
（1）It is 1 in mass ratio by phosphatide and solvent：40~1：50 stirring and dissolvings, then through being concentrated under reduced pressure, obtain concentrate；
（2）It is 1 by volume by concentrate and buffer solution：20~1：Ultrasonic disperse after 25 mixing, then through Frozen-thawed cycled 3~5 times,
Obtain mixed liquor；
（3）The short fibre of magnesium silk is cut into after magnesium silk is polished, then magnesium silk is short fine clear with acetone, absolute ethyl alcohol and water ultrasound successively
Wash, and be 1 in mass ratio by the short fibre of the magnesium silk after washing and oxidation mixed liquor：5~1：10 heating reactions, are filtered, washing, obtains pre-
Handle the short fibre of magnesium silk；
（4）It is 1 in mass ratio by the short fine and mixed liquor of pretreatment magnesium silk：10~1：After 15 mixing, insulation dipping, is filtered, washing,
The short fibre of magnesium silk must be modified；
（5）Count in parts by weight, take 20~30 parts of collagens successively, 150~200 parts of water, 10~15 parts of short fibres of modified magnesium silk,
20~30 parts of pretreatment calcium hydroxy phosphates, after being stirred, move into orifice plate, after refrigerating 2~4h, freeze 8~12h, then through true
Vacuum freecing-dry, obtains drying bracket blank；
（6）Drying bracket blank is soaked with absolute ethyl alcohol and sodium hydroxide solution successively, then is washed with deionized, up to curing
With collagen complex stephanoporate bracket.
A kind of 2. preparation method of medical collagen complex stephanoporate bracket according to claim 1, it is characterised in that：Step
Suddenly（1）The phosphatide is any one in egg yolk lecithin or soybean lecithin.
A kind of 3. preparation method of medical collagen complex stephanoporate bracket according to claim 1, it is characterised in that：Step
Suddenly（1）The solvent is that chloroform, methanol and triethylamine are 10 in mass ratio：7：1 configuration forms.
A kind of 4. preparation method of medical collagen complex stephanoporate bracket according to claim 1, it is characterised in that：Step
Suddenly（2）The buffer solution is the phosphate buffer that pH is 7.2~7.4.
A kind of 5. preparation method of medical collagen complex stephanoporate bracket according to claim 1, it is characterised in that：Step
Suddenly（3）The magnesium silk is a diameter of 0.02~0.04mm, and length is 8~10cm.
A kind of 6. preparation method of medical collagen complex stephanoporate bracket according to claim 1, it is characterised in that：Step
Suddenly（3）It is 1 in mass ratio by citric acid, hydrogen peroxide and water that the oxidation mixed liquor, which is,：1：8 configurations form.
A kind of 7. preparation method of medical collagen complex stephanoporate bracket according to claim 1, it is characterised in that：Step
Suddenly（5）It is described pretreatment calcium hydroxy phosphate preprocessing process be：It is 2.0~2.2g/L by nano-hydroxy phosphoric acid calcium and mass concentration
After dopamine solution mixing, pH to 8.0~8.2,45~60min of sonic oscillation are adjusted with sodium hydroxide solution, is filtered, washing,
Calcium hydroxy phosphate must be pre-processed.
A kind of 8. preparation method of medical collagen complex stephanoporate bracket according to claim 1, it is characterised in that：Step
Suddenly（5）The orifice plate is any one in 12 orifice plates, 24 orifice plates or 96 orifice plates.
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