CN107569714A - A kind of preparation method of functionalization fracture adhesive - Google Patents
A kind of preparation method of functionalization fracture adhesive Download PDFInfo
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- CN107569714A CN107569714A CN201710711867.1A CN201710711867A CN107569714A CN 107569714 A CN107569714 A CN 107569714A CN 201710711867 A CN201710711867 A CN 201710711867A CN 107569714 A CN107569714 A CN 107569714A
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Abstract
The invention discloses a kind of preparation method of functionalization fracture adhesive, this method is using the PLGA microballoon of mussel mucin and hydroxyl apatite as raw material, mussel meat mincing are dissolved with basic solvent, add neutral proteinase, acid flux material precipitation extraction mussel mucin；The PLGA microballoon containing hydroxyapatite is made in the acetum of hydroxyapatite and PLGA solution using multi-emulsion method；The mussel mucin prepared and the PLGA microballoon containing hydroxyapatite are weighed, functionalization fracture adhesive is obtained after mixing cooling.The adhesive of the present invention has extremely strong adhesive property, can physiological environment it is moist under the conditions of give full play to bone adhesive effect, there is good adhesion property and higher biological safety while with Cranial defect filling capacity.
Description
Technical field
The invention belongs to medical biomaterial technical field, is related to a kind of preparation method for adhesive of fracturing, and in particular to
A kind of preparation method of functionalization fracture adhesive.
Background technology
Clinical treatment fracture generally has two methods of outer fixation and operative treatment, and its China and foreign countries' fixed race is fixed in indirect,
The problems such as easily causing limb muscle atrophy, osteoporosis after the fixed long period；And interior fixation easily cause osteoporosis or
Interior fixed loosening is caused, and is once infected, metallic foreign body will seriously hinder wound and union, particularly with powder
It is more difficult to fix for fragility fracture, effect is bad to cause a series of sequelae.With the progress of medical science, clinically to skill of performing the operation
The requirement more and more higher of art and auxiliary material effect, medical bone-cementum are a kind of new fracture fixation materials, have operation letter
Just, usage amount is few, steady performance, can overcome outer fixation and internal fixation operation is complicated, easy infection and difficult degradation etc.
Problem, gradually receive the favor of numerous doctors and patient.
Current bone-cementum mainly includes a-cyanoacrylate class adhesive, polymethyl methacrylate class bonds
Agent, series of calcium phosphate bone cement, magnesium phosphate pastern bone cement etc., in the operation technique of reality, the various surface of a wound are at one and gone out
Blood, the wet environment of tissue fluid infiltration, for above bone-cementum, are all difficult to realize under water or under wet environment
Strongly adherent, its use environment is mostly better in dry environments, and its bonding effect can be influenceed under wet environment, therefore
Need to develop under a kind of nontoxic, wet environment using the new bone-cementum still with high intensity tissue adhesion.
The content of the invention
For in the prior art the defects of and deficiency, the invention provides a kind of functionalization fracture adhesive preparation side
Method, the defects of overcoming bone-cementum of the prior art sticky poor in wet condition.
To reach above-mentioned purpose, the present invention takes following technical scheme：
A kind of preparation method of functionalization fracture adhesive, this method is with mussel mucin and the poly- breast of hydroxyl apatite
Acid-co-glycolic acid microballoon is that raw material prepares functionalization fracture adhesive.
The present invention also has following distinguishing feature：
The preparing raw material of described mussel mucin is：Mussel meat mincing and neutral proteinase.
The preparing raw material of the Poly(D,L-lactide-co-glycolide microballoon of described hydroxyl apatite is：Hydroxyapatite
And Poly(D,L-lactide-co-glycolide.
The specific preparation of functionalization fracture adhesive comprises the following steps：
Step 1：Prepare mussel mucin：Under alkalescence condition, mussel meat mincing are dissolved, add described neutral proteinase,
Supernatant is collected, under acid condition, precipitation extraction mussel mucin；
Step 2：Hydroxyapatite and acetum are weighed, obtains the acetum of hydroxyapatite；
Step 3：Poly(D,L-lactide-co-glycolide is dissolved in organic solvent, using multi-emulsion method by described hydroxyl phosphorus
The poly lactic-co-glycolic acid containing hydroxyapatite is made with Poly(D,L-lactide-co-glycolide solution in the acetum of lime stone
Copolymer microsphere；
Step 4：Weigh the mussel mucin prepared and the Poly(D,L-lactide-co-glycolide containing hydroxyapatite
Microballoon, certain time is mixed, functionalization fracture adhesive is obtained after cooling.
The pH of described alkalescence condition is 7.5；The pH of described acid condition is 6.
Described neutral proteinase is serrapeptass；Count in parts by weight, described mussel meat mincing：Neutral proteinase=
100:3。
Described hydroxyapatite：Acetum=5：100~15：200；
Described acetum is the acetum that mass fraction is 5%；
Described organic solvent is dichloromethane；
Count in parts by weight, described Poly(D,L-lactide-co-glycolide：Dichloromethane=10：250~15：400.
Count in parts by weight, the acetum of described hydroxyapatite and the dichloro of Poly(D,L-lactide-co-glycolide
The weight ratio of dichloromethane is 10：50~10：30.
Count in parts by weight, described mussel mucin and the Poly(D,L-lactide-co-glycolide containing hydroxyapatite
The weight ratio of microballoon is 40：30~50：40.
Described step four mixed the time as 10~15 minutes.
Compared with prior art, beneficial has the technical effect that the present invention：
Functionalization fracture adhesive prepared by the present invention has extremely strong adhesive property, can be in the moist condition of physiological environment
Under give full play to bone adhesive effect, there is good adhesion property and higher biological safety, and can be in knitting process
In slowly degrade, there is good gumminess and excellent water resistance, be adapted to large-scale promotion use, the preparation of the adhesive
Technique is simple, reaction condition is gentle, in process of production with good operability.
Functionalization fracture adhesive tool Cranial defect filling capacity prepared by the present invention, can promote osteanagenesis, and preparation method
Simplicity, the present invention are dissolved using basic solvent and extract mussel mucin with acid flux material precipitation, then with hydroxyapatite and
Poly(D,L-lactide-co-glycolide synthesizes microballoon, and the bone that the mussel mucin of extraction and microballoon are mixed to get to functionalization bonds
Agent, be allowed to the function of possessing osteoacusis and self-bone grafting, the functionalization bone-cementum physiological environment it is moist under the conditions of can be abundant
Tissue adhesion effect is played, there is preferable tissue adhension performance and higher biological safety, and can be in organization healing
Slowly degraded in journey.
Embodiment
The preparation method of the functionalization fracture adhesive of the present invention, with mussel mucin and the poly- breast of hydroxyl apatite
Acid-co-glycolic acid microballoon is raw material, and the raw material for preparing mussel mucin is：Mussel meat mincing and neutral proteinase.Prepare
The raw material of the Poly(D,L-lactide-co-glycolide microballoon of hydroxyl apatite is：Hydroxyapatite and poly lactic-co-glycolic acid are total to
Polymers.Wherein, the adhesion protein that mussel is secreted by byssus, there is high intensity, high tenacity, water proofing property and extremely strong adhesion etc.
Feature；Neutral proteinase is more preferable relative to pepsin and pawpaw Amylase digestion effect, and neutral starch enzyme is by microorganism
Fermentation forms, competitively priced；Hydroxyapatite is a kind of surface active material, it have to organism sclerous tissues similar chemistry into
Point and structure, there is good bioactivity and compatibility, is implanted into after human body to the non-stimulated and repulsive interaction of tissue, can be with bone shape
Into very strong chemical bond, the filler as Cranial defect, support is provided for the formation of new bone, bone conduction effect is played, is
Preferable hard tissue substituting material；Poly(D,L-lactide-co-glycolide is that a kind of biology with good biocompatibility can drop
Solve material, the carrier material for hydroxyapatite.
Organic solvent in present embodiment is dichloromethane, and the specific preparation of functionalization fracture adhesive includes following step
Suddenly：
Step 1：Prepare mussel mucin：Deionized water is added into described mussel meat mincing and is stirred, alkaline bar
Under part, described neutral proteinase is added, is then heated to 50 DEG C, removes filter residue after cooking 4~5h, collects supernatant, acid
Property under the conditions of, be put into after 4 DEG C of refrigerators cool down 8~10h and filter, it is mussel mucin to collect filter residue；
Step 2：Prepare the acetum of hydroxyapatite：Hydroxyapatite is weighed, adds acetum, is placed in
60~70 DEG C are warming up in water-bath, stirring obtains the acetum of hydroxyapatite after hydroxyapatite all dissolving；
Step 3：Prepare the Poly(D,L-lactide-co-glycolide microballoon of hydroxyl apatite：By poly lactic-co-glycolic acid
Copolymer is dissolved in organic solvent, using multi-emulsion method by the acetum and Poly(D,L-lactide-co-glycolide of hydroxyapatite
The Poly(D,L-lactide-co-glycolide microballoon containing hydroxyapatite is made in solution；
Step 4：Weigh the mussel mucin prepared and the Poly(D,L-lactide-co-glycolide containing hydroxyapatite
Microballoon, certain time is mixed, functionalization fracture adhesive is obtained after cooling.
Above-mentioned technical proposal is deferred to, specific embodiment of the invention given below is, it is necessary to which explanation is the present invention not office
It is limited to specific examples below, all equivalents done on the basis of technical scheme each fall within the protection model of the present invention
Enclose.The present invention is described in further details with reference to embodiment.
Embodiment 1：
Weigh 0.5kg mussel meat mincing to pour into beaker, deionized water 1L is added into beaker, and is stirred, then to burning
Sodium hydroxide or watery hydrochloric acid regulation pH are added in cup, makes up to 7.5, it is husky thunder peptide that neutral proteinase is added in beaker
Enzyme, enzyme concentration 4000U/g, 50 DEG C are then heated to beaker, cook 4h, filter residue is removed in cooking after terminating, collect supernatant；
Watery hydrochloric acid regulation pH will be added in supernatant obtained above, makes up to 6, is then placed in 4 DEG C of refrigerator coolings, cooling 8h is laggard
Row filtering, collection filter residue is standby, and filter residue is mussel mucin.Weigh 5g hydroxyapatites to be added in flask, add
100mL mass fractions are 5% acetum, are placed in water-bath, are warming up to 60 DEG C, stir 15min, treat that hydroxyapatite is complete
After portion's dissolving, the acetum of hydroxyapatite is obtained；Poly(D,L-lactide-co-glycolide is dissolved in dichloromethane, utilized
The acetum of above-mentioned hydroxyapatite and Poly(D,L-lactide-co-glycolide solution are made containing hydroxyapatite multi-emulsion method
Microballoon.Count in parts by weight, weigh the poly lactic-co-glycolic acid copolymerization of 40 parts of mussel mucins and 30 parts of hydroxyl apatite
Thing microballoon is added in beaker, and after being stirred 10min, imitative mussel functionalization bone-cementum can be obtained after cooling.
Embodiment 2：
Weigh 0.75kg mussel meat mincing to pour into beaker, deionized water 1.5L is added into beaker, and stir, then to
Sodium hydroxide or watery hydrochloric acid regulation pH are added in beaker, makes up to 7.5, it is husky thunder that neutral proteinase is added in beaker
Peptase, enzyme concentration 4000U/g, 50 DEG C are then heated to beaker, cook 4.5h, cooked and remove filter residue after terminating, in collection
Clear liquid；Watery hydrochloric acid regulation pH will be added in supernatant obtained above, makes up to 6, is then placed in 4 DEG C of refrigerator coolings, cooling
Filtered after 9h, collection filter residue is standby, and filter residue is mussel mucin.10g hydroxyapatites are weighed to be added in flask, then
It is 5% acetum to add 150mL mass fractions, is placed in water-bath, is warming up to 65 DEG C, stirs 20min, treats hydroxy-apatite
Stone all after dissolving, obtains the acetum of hydroxyapatite；Poly(D,L-lactide-co-glycolide is dissolved in dichloromethane,
The acetum of above-mentioned hydroxyapatite and Poly(D,L-lactide-co-glycolide solution are made containing hydroxyl phosphorus using multi-emulsion method
The microballoon of lime stone.Count in parts by weight, weigh the poly lactic-co-glycolic acid of 45 parts of mussel mucins and 35 parts of hydroxyl apatite
Copolymer microsphere is added in beaker, and after being stirred 12min, imitative mussel functionalization bone-cementum can be obtained after cooling.
Embodiment 3：
Weigh 1kg mussel meat mincing to pour into beaker, deionized water 2L is added into beaker, and is stirred, then to beaker
Middle addition sodium hydroxide or watery hydrochloric acid regulation pH, makes up to 7.5, it is husky thunder peptide that neutral proteinase is added in beaker
Enzyme, enzyme concentration 4000U/g, 50 DEG C are then heated to beaker, cook 5h, filter residue is removed in cooking after terminating, collect supernatant；
Watery hydrochloric acid regulation pH will be added in supernatant obtained above, makes up to 6,4 DEG C of refrigerator coolings are then placed in, after cooling down 10h
Filtered, collection filter residue is standby, and filter residue is mussel mucin.Weigh 15g hydroxyapatites to be added in flask, add
200mL mass fractions are 5% acetum, are placed in water-bath, are warming up to 70 DEG C, stir 30min, treat that hydroxyapatite is complete
After portion's dissolving, the acetum of hydroxyapatite is obtained；Poly(D,L-lactide-co-glycolide is dissolved in dichloromethane, utilized
The acetum of above-mentioned hydroxyapatite and Poly(D,L-lactide-co-glycolide solution are made containing hydroxyapatite multi-emulsion method
Microballoon.Count in parts by weight, weigh the poly lactic-co-glycolic acid copolymerization of 50 parts of mussel mucins and 40 parts of hydroxyl apatite
Thing microballoon is added in beaker, and after being stirred 15min, imitative mussel functionalization bone-cementum can be obtained after cooling.
Comparative example 1：
This comparative example as different from Example 1, weighs 0.5kg mussel meat mincing and poured into beaker, add and go into beaker
Ionized water 1L, and stir, then sodium hydroxide or watery hydrochloric acid regulation pH are added into beaker, 7.5 are made up to, then at burning
It is serrapeptass that neutral proteinase is added in cup, enzyme concentration 4000U/g, 50 DEG C is then heated to beaker, cooks 4h, is cooked
Remove filter residue after end, collect supernatant；Watery hydrochloric acid regulation pH will be added in supernatant obtained above, makes up to 6, then
4 DEG C of refrigerator coolings are put into, are filtered after cooling down 8h, collection filter residue is standby, and filter residue is mussel mucin.Weigh mussel and stick egg
It is added in vain in beaker, is stirred 10min, product is can obtain after cooling.
Comparative example 2：
This comparative example as different from Example 2, weighs 10g hydroxyapatites and is added in flask, add 150mL matter
Amount fraction is 5% acetum, is placed in water-bath, is warming up to 65 DEG C, stirs 20min, treats that hydroxyapatite all dissolves
Afterwards, the acetum of hydroxyapatite is obtained；Poly(D,L-lactide-co-glycolide is dissolved in dichloromethane, utilizes multi-emulsion method
The acetum of above-mentioned hydroxyapatite and Poly(D,L-lactide-co-glycolide solution are made containing the micro- of hydroxyapatite
Ball.The Poly(D,L-lactide-co-glycolide microballoon for weighing hydroxyl apatite is added in beaker, is stirred 12min, cooling
After can obtain product.
Performance measurement is as follows：
Performance measurement to the product obtained by embodiment 1, embodiment 2, embodiment 3, comparative example 1 and comparative example 2 is as follows：
First, cell attachment
The product that embodiment 1,2 and 3 and comparative example 1 and 2 are obtained, using disinfection with high pressure steam 1h, and turn into sheet
Structure, it is placed in 24 orifice plates with DMEM culture mediums, adds L-929 cell suspensions, be placed in constant incubator in 5%
CO2, cultivate 24h under the conditions of 37 DEG C, when L-929 cell growths converge rate for more than 80% when, carry out pancreatin digestion, centrifugation, again
It is outstanding, it is inoculated into culture plate, 24h is cultivated under the conditions of 5%CO2,37 DEG C, removes the cell not attached, use hoechst33.258
Solution dyes, and then proceedes to after being cleaned 2 times using phosphate buffer solution, the sample dyed using fluorescence microscope.
As a result：The product of embodiment 1, embodiment 2 and embodiment 3：L-929 cells are in functionalization fracture adhesive after 24h
Surface attaches well, is easy to cell propagation growth.The product of comparative example 1 and comparative example 2：L-929 cells are in comparative example 1 after 24h
Attached with its surface of comparative example 2 good.This explanation L-929 cell is in embodiment 1, embodiment 2, embodiment 3, comparative example 1
Attached with its surface obtained by comparative example 2 good.
2nd, cytotoxicity
The product that embodiment 1,2 and 3 and comparative example 1 and 2 are obtained, using disinfection with high pressure steam 1h, and turn into sheet
Structure.It is placed in 24 orifice plates with DMEM culture mediums, adds L-929 cell suspensions, be placed in constant incubator in 5%CO2,37
24h is cultivated under the conditions of DEG C, when it is more than 80% that L-929 cell growths, which converge rate, carries out pancreatin digestion, centrifugation, resuspension, inoculation
Into 96 orifice plates, nutrient solution is sucked respectively at 24h, 48h, 72h, adding MTT solution makes its final concentration of 0.5mg/mL, is incubated 4
Supernatant is removed after hour, adds the dimethyl sulfoxide (DMSO) (DMSO) in 1.5mL/ holes, incubator is put into and is incubated 20 minutes, suction pipe after taking-up
Piping and druming is uniformly dissolved burgundy crystals thing repeatedly, adds in 96 orifice plates liquid by 100 μ L/ holes, determines each hole OD values.
As a result：The product of embodiment 1, embodiment 2 and embodiment 3：OD values increase with the increase of time, illustrate the function
It is relatively low to L-929 cytotoxicities to change fracture adhesive.The product of comparative example 1 and comparative example 2：OD values increase with the increase of time
Greatly, illustrate that the product of comparative example 1 and comparative example 2 is relatively low to L-929 cytotoxicities.This explanation embodiment 1,2 and 3 and comparative example
1 and 2 obtained products are relatively low to L-929 cytotoxicities.
3rd, alkaline phosphatase (ALP) determination of activity
The product that embodiment 1,2 and 3 and comparative example 1 and 2 are obtained, using disinfection with high pressure steam 1h, and turn into sheet
Structure, it is placed in 96 orifice plates, while control group is set, Gegenbaur's cell is inoculated with 96 orifice plates with 5*104/ml density, per hole 100
μ L, when it is more than 80% that cell growth, which converges rate, nutrient solution is sucked, PBS adds 0.1%Triton-X100 liquid after washing 3 times
100 μ L, vibration cracking 30min, takes 50 μ L cell pyrolysis liquids and 150 μ L ALP substrate reactions liquids, 37 DEG C of perseverances on microoscillator
30min is placed in temperature vibration case, with 0.1mol/L NaOH terminating reactions, absorbance is determined at ELIASA 405nm.
As a result：The product of embodiment 1, embodiment 2 and embodiment 3：ALP levels are significantly raised.Comparative example 1 and comparative example 2
Product：ALP levels are significantly lower than embodiment 1,2,3 in comparative example 1, there is significant difference；ALP levels are lower slightly in comparative example 2
In embodiment 1,2,3.This explanation, embodiment 1,2,3 is by the mussel mucin and hydroxyapatite of extraction and polylactic acid-glycolic base second
The functionalization bone-cementum that the microballoon of acid copolymer synthesis is mixed to get possesses very compared with the product of comparative example 1 and comparative example 2
Strong osteoacusis and the function of self-bone grafting.
4th, incompressible experiment
Using goose saw Sawbone artificial synthesis bones neck of femur is cut so as to make Pauwels type III stocks for 70 ° along horizontal line
Bone fracture of cervical vertebra model, the product obtained using embodiment 1,2 and 3 and comparative example 1 and 2, artificial synthesis bone's fracture end is bonded,
And the artificial synthesized bone specimens of Sawbone are fixed on MTS mechanics of biomaterials measuring instruments, by applying the vertical of 100N to sample
Load, the rigidity value and ultimate load of sample are measured, obtained load signal is recorded by computer data acquisition system, and is used
The test software that instrument carries calculates corresponding rigidity value.
As a result：The product of embodiment 1, embodiment 2 and embodiment 3：Axle rigidity is 21 ± 8N/mm, 23 ± 7N/mm, 25
± 11N/mm ultimate loads are 256N, 283N, 289N.The product of comparative example 1 and comparative example 2：The axis rigidity of comparative example 1 is 18
± 5N/mm, ultimate load 233N, the no adhesion of comparative example 2.This explanation, embodiment 1,2,3 by the mussel mucin of extraction with
The functionalization bone-cementum that the microballoon that hydroxyapatite synthesizes with Poly(D,L-lactide-co-glycolide is mixed to get and comparative example 1
Compared with the product of comparative example 2, possess very strong adhesive property.
5th, stretch-proof is tested
Fresh new zealand rabbit femur is prepared into a fracture face, the production that embodiment 1,2 and 3 and comparative example 1 and 2 are obtained
Thing is used for the bonding of fracture end, and 24h is fixed in (simulated in vivo environment) under 37 DEG C, 100% humidity, then fixes sample
In mechanics of biomaterials experiment survey meter device.With 18mm/min loading velocity extract in fact along artificial synthesis bone's long axis direction
Test, stop after there is fracture end destruction.Extraction standard is decreased obviously immediately after displacement-extraction force curve to peak, is analyzed
Maximum axial withdrawal force.
As a result：The product of embodiment 1, embodiment 2 and embodiment 3：Maximum axial withdrawal force be 216 ± 34N, 238 ±
39N、257±48N.The product of comparative example 1 and comparative example 2：Maximum axial withdrawal force is 122 ± 25N in comparative example 1, comparative example 2
No adhesion.The mussel mucin and hydroxyapatite and poly lactic-co-glycolic acid of extraction are copolymerized by this explanation embodiment 1,2,3
The functionalization bone-cementum that the microballoon of thing synthesis is mixed to get possesses very strong glue compared with the product of comparative example 1 and comparative example 2
Tie performance.
Conclusion：The functionalization fracture adhesive prepared with mussel mucin has extremely strong adhesive property, can be in physiologic ring
Border it is moist under the conditions of give full play to bone adhesive effect, chemical bond that can be very strong with bon e formation has good adhesion property
Higher biological safety, while promoting osteanagenesis, the filler as Cranial defect, branch is provided for the formation of new bone
Frame, bone conduction effect is played, the function of possessing osteoacusis and self-bone grafting, and good bioactivity and compatibility.
Claims (10)
1. a kind of preparation method of functionalization fracture adhesive, it is characterised in that this method is with mussel mucin and hydroxyl phosphorus
The Poly(D,L-lactide-co-glycolide microballoon of lime stone is that raw material prepares functionalization fracture adhesive.
2. preparation method as claimed in claim 1, it is characterised in that the preparing raw material of described mussel mucin is：Mussel
Meat mincing and neutral proteinase.
3. preparation method as claimed in claim 1, it is characterised in that the polylactic acid-glycolic base second of described hydroxyl apatite
The preparing raw material of acid copolymer microballoon is：Hydroxyapatite and Poly(D,L-lactide-co-glycolide.
4. the preparation method as described in Claims 2 or 3 any claim, it is characterised in that functionalization fracture adhesive
Specific prepare comprises the following steps：
Step 1：Prepare mussel mucin：Under alkalescence condition, mussel meat mincing are dissolved, add described neutral proteinase, are collected
Supernatant, under acid condition, precipitation extraction mussel mucin；
Step 2：Hydroxyapatite and acetum are weighed, obtains the acetum of hydroxyapatite；
Step 3：Poly(D,L-lactide-co-glycolide is dissolved in organic solvent, using multi-emulsion method by described hydroxyapatite
Acetum and Poly(D,L-lactide-co-glycolide solution the poly lactic-co-glycolic acid containing hydroxyapatite be made be copolymerized
Thing microballoon；
Step 4：The mussel mucin prepared and the Poly(D,L-lactide-co-glycolide microballoon containing hydroxyapatite are weighed,
Certain time is mixed, functionalization fracture adhesive is obtained after cooling.
5. preparation method as claimed in claim 4, it is characterised in that the pH of described alkalescence condition is 7.5；Described acidity
The pH of condition is 6.
6. preparation method as claimed in claim 4, it is characterised in that described neutral proteinase is serrapeptass；By weight
Number meter, described mussel meat mincing：Neutral proteinase=100：3.
7. preparation method as claimed in claim 4, it is characterised in that count in parts by weight, described hydroxyapatite：Acetic acid
Solution=5：100~15：200；
Described acetum is the acetum that mass fraction is 5%；
Described organic solvent is dichloromethane；
Count in parts by weight, described Poly(D,L-lactide-co-glycolide：Dichloromethane=10：250~15：400.
8. preparation method as claimed in claim 4, it is characterised in that count in parts by weight, the vinegar of described hydroxyapatite
The weight ratio of the dichloromethane solution of acid solution and Poly(D,L-lactide-co-glycolide is 10：50~10：30.
9. preparation method as claimed in claim 4, it is characterised in that count, described mussel mucin and contain in parts by weight
The weight ratio for having the Poly(D,L-lactide-co-glycolide microballoon of hydroxyapatite is 40：30~50：40.
10. preparation method as claimed in claim 4, it is characterised in that described step four mixes the time as 10~15
Minute.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110522946A (en) * | 2019-09-20 | 2019-12-03 | 浙江瑞谷生物科技有限公司 | A kind of bone renovating material microballoon and preparation method thereof carrying rhBMP-2 |
| CN110665060A (en) * | 2019-10-18 | 2020-01-10 | 浙江瑞谷生物科技有限公司 | Bone repair material and preparation method and application thereof |
| CN112852382A (en) * | 2021-03-09 | 2021-05-28 | 中南大学湘雅医院 | Photo-curing bone adhesive and preparation method thereof |
| CN113368298A (en) * | 2021-06-09 | 2021-09-10 | 广东麦迪泰医疗科技有限公司 | Medical orthopedic adhesive material with antibacterial effect and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101961506A (en) * | 2010-09-30 | 2011-02-02 | 深圳市第二人民医院 | Composite nano biological bone glue with osteogenesis inducing activity and preparation method thereof |
| CN103520766A (en) * | 2013-09-25 | 2014-01-22 | 高敏 | Mussel mucoprotein liquid product as well as preparation method and application thereof |
| CN106310357A (en) * | 2016-10-18 | 2017-01-11 | 曹建中 | Bone filling adhesive and preparation method as well as application of bone filling adhesive |
| CN107029273A (en) * | 2017-04-14 | 2017-08-11 | 苏州医甸园医疗科技发展有限公司 | A kind of compound wound repair dressing based on sea-mussel mucin and polylactic acid microsphere and preparation method and application |
-
2017
- 2017-08-18 CN CN201710711867.1A patent/CN107569714B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101961506A (en) * | 2010-09-30 | 2011-02-02 | 深圳市第二人民医院 | Composite nano biological bone glue with osteogenesis inducing activity and preparation method thereof |
| CN103520766A (en) * | 2013-09-25 | 2014-01-22 | 高敏 | Mussel mucoprotein liquid product as well as preparation method and application thereof |
| CN106310357A (en) * | 2016-10-18 | 2017-01-11 | 曹建中 | Bone filling adhesive and preparation method as well as application of bone filling adhesive |
| CN107029273A (en) * | 2017-04-14 | 2017-08-11 | 苏州医甸园医疗科技发展有限公司 | A kind of compound wound repair dressing based on sea-mussel mucin and polylactic acid microsphere and preparation method and application |
Non-Patent Citations (1)
| Title |
|---|
| 倪淞波等: "羟基磷灰石微球的制备、应用和功能化", 《化学进展》 * |
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| CN110522946A (en) * | 2019-09-20 | 2019-12-03 | 浙江瑞谷生物科技有限公司 | A kind of bone renovating material microballoon and preparation method thereof carrying rhBMP-2 |
| CN110522946B (en) * | 2019-09-20 | 2021-11-30 | 浙江瑞谷生物科技有限公司 | rhBMP-2-loaded bone repair material microsphere and preparation method thereof |
| CN110665060A (en) * | 2019-10-18 | 2020-01-10 | 浙江瑞谷生物科技有限公司 | Bone repair material and preparation method and application thereof |
| CN110665060B (en) * | 2019-10-18 | 2021-09-21 | 浙江瑞谷生物科技有限公司 | Bone repair material and preparation method and application thereof |
| CN112852382A (en) * | 2021-03-09 | 2021-05-28 | 中南大学湘雅医院 | Photo-curing bone adhesive and preparation method thereof |
| CN113368298A (en) * | 2021-06-09 | 2021-09-10 | 广东麦迪泰医疗科技有限公司 | Medical orthopedic adhesive material with antibacterial effect and preparation method thereof |
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