CN106267359B - Anti-infective calcium sulfate/load medicine fibroin microsphere/mineralising fibroin nanofiber bone renovating material preparation method - Google Patents
Anti-infective calcium sulfate/load medicine fibroin microsphere/mineralising fibroin nanofiber bone renovating material preparation method Download PDFInfo
- Publication number
- CN106267359B CN106267359B CN201610672750.2A CN201610672750A CN106267359B CN 106267359 B CN106267359 B CN 106267359B CN 201610672750 A CN201610672750 A CN 201610672750A CN 106267359 B CN106267359 B CN 106267359B
- Authority
- CN
- China
- Prior art keywords
- fibroin
- microsphere
- mineralising
- vancomycin
- solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- 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
- A61L27/40—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material
- A61L27/42—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material having an inorganic matrix
-
- 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
- A61L27/54—Biologically active materials, e.g. therapeutic substances
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B11/00—Calcium sulfate cements
- C04B11/02—Methods and apparatus for dehydrating gypsum
-
- 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
- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/20—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing organic materials
- A61L2300/252—Polypeptides, proteins, e.g. glycoproteins, lipoproteins, cytokines
-
- 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
- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/40—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a specific therapeutic activity or mode of action
- A61L2300/404—Biocides, antimicrobial agents, antiseptic agents
- A61L2300/406—Antibiotics
-
- 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
- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/60—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a special physical form
- A61L2300/602—Type of release, e.g. controlled, sustained, slow
-
- 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
- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/60—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a special physical form
- A61L2300/62—Encapsulated active agents, e.g. emulsified droplets
- A61L2300/622—Microcapsules
-
- 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
- A61L2400/12—Nanosized materials, e.g. nanofibres, nanoparticles, nanowires, nanotubes; Nanostructured surfaces
-
- 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
- A61L2430/02—Materials or treatment for tissue regeneration for reconstruction of bones; weight-bearing implants
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Medicinal Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Epidemiology (AREA)
- Ceramic Engineering (AREA)
- Dermatology (AREA)
- Oral & Maxillofacial Surgery (AREA)
- Transplantation (AREA)
- Materials Engineering (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Biomedical Technology (AREA)
- Molecular Biology (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Composite Materials (AREA)
- Materials For Medical Uses (AREA)
- Medicinal Preparation (AREA)
Abstract
Anti-infective calcium sulfate/load medicine fibroin microsphere/mineralising fibroin nanofiber bone renovating material preparation method, belong to biomedical materials field, vancomycin fibroin microsphere, 5wt% vancomycin, 75wt% ~ 85wt% α type half-H 2 O calcium sulphate are carried by 5wt% ~ 10wt% calcium sulphate dihydrate, 5wt% ~ 10wt%, above-mentioned raw materials are added to the mineralising fibroin nanofiber solution that concentration is 3wt% ~ 15wt% after mixing, obtain anti-infective calcium sulfate/load medicine fibroin microsphere/mineralising fibroin nanofiber bone renovating material.The present invention promotes skeletonization while effectively control is infected at bone defect.After bone material surface and inside are absorbed, with the deposition of new bone, the remodeling process of bone tissue is imitated, material can be made to be integrated into the metabolism of living body bone and finally for replaced itself bone tissue.
Description
Technical field
The invention belongs to biomaterial for medical purpose fields, and in particular to a kind of anti-infective calcium sulfate/load medicine fibroin microsphere/mineralising
The preparation method of fibroin nanofiber bone renovating material.
Background technique
Due to there is the dual lesion of infection and bone defect in infectious bone defect, treatment is intractable, and the course for the treatment of is long, and flesh easily occurs
Meat atrophy, local scar and cause limb function to be severely impacted.So far, infectious bone defect is still clinically to compare spine
Hand and treatment problem urgently to be resolved.Bacterium forms biomembrane in implant surfaces and makes simple bone grafting operation because of sense after infection
Dye is not easy to control and fails, therefore patient tends not to carry out one-stage bone grafting, and needs thorough debridement, eliminates to infective agent, wound
The second stage of bone grafting repairing bone defect is carried out again after mouth healing, reconstructing blood vessel.This treatment method had both increased the pain of patient, also prolonged
Treatment time is grown.Antibiotic is released into part by carrier by local drug delivery system (DDS), can be obtained in infection part
Higher blood concentration is obtained, and topically effective Mlc can be maintained for a long time, avoids whole body toxicity, is inhibiting infection
The reparation to bone defect is realized simultaneously.
α type half-H 2 O calcium sulphate as bone renovating material, because its defect self solidified in situ performance, it is degradable, connect
The mechanical property of person of modern times's cancellous bone；A large amount of micropores are formed after solidification；The unobvious big calorimetric of release is living without influencing loaded drug
Property and promote the excellent performances such as knitting, be used as product clinically to be used.Filler of the calcium sulfate as bone defect, resistance
Only soft tissue is grown into；The calcium ion for the local microenvironment and high local concentrations that are formed of degrading is conducive to the length of blood vessel and osteoblast
Enter, promotes proliferation, the differentiation of osteoblast, adjust the formation of osteoid.In the raising to half-H 2 O calcium sulphate material bioactivity
The middle multistage that the organic principle of mineralising need to be added from composition and increase material from structure is realized further bionical.Together
When high-molecular organic material fibroin microsphere addition can reduce the brittleness of calcium sulfate material and improve the toughness of material.And in material
High molecular drug bearing microsphere is added in material, the sustained release of drug may be implemented.Calcium sulfate has good biocompatibility, especially
With one's own department or unit self-curing and plasticity, in conjunction with mineralising nanometer fibroin fiber material self-bone grafting repair ability the characteristics of, this hair
Bright one kind of developing has one's own department or unit self-curing performance, and the bone implant repair materials with good self-bone grafting repair ability.
Summary of the invention
The object of the present invention is to provide a kind of anti-infective calcium sulfate/load medicine fibroin microsphere/mineralising fibroin nanofiber bones to repair
The preparation method of multiple material, makes it have regulatable drug releasing rate, and what initial stage release and subsequent sustained release combined releases
Put feature.It specifically proposes that calcium sulfate and vancomycin are bound directly and discharges carrier, calcium sulfate and load vancomycin as initial stage
Fibroin microsphere is combined as later period release carrier, realizes the lasting controlled release of drug.
A kind of anti-infective calcium sulfate/load medicine fibroin microsphere/mineralising fibroin nanofiber bone renovating material, it is characterized in that by
5wt% ~ 10wt% calcium sulphate dihydrate, 5wt% ~ 10wt% carry vancomycin fibroin microsphere, 5wt% vancomycin, 75wt% ~ 85wt% α type
For half-H 2 O calcium sulphate as Solid raw materials, concentration is the mineralising fibroin nanofiber solution of 3wt% ~ 15wt% as liquid phase feed.System
Standby anti-infective calcium sulfate/load medicine fibroin microsphere/mineralising fibroin nanofiber bone renovating material.
Above-mentioned solid phase raw material and liquid phase feed are mixed into slurry, and the carrying drug ratio for carrying vancomycin fibroin microsphere is
4.03wt%~4.72wt%；Liquid-solid ratio is 0.5mL/g ~ 0.7mL/g；It is porous structure after solidification, porosity is 30% ~ 40%.
A kind of preparation method of anti-infective calcium sulfate/load medicine fibroin microsphere/mineralising fibroin nanofiber bone renovating material, packet
Include following steps:
(1) hydro-thermal method prepares α type half-H 2 O calcium sulphate: 300 g calcium sulphate dihydrates and 1.5 g enuatrols sufficiently being mixed, are added
Enter 1200mL distilled water and stir evenly to be placed in closed autoclave, is heated to 120 DEG C, pressure is about at this time
0.138MPa keeps 7 h of pressure heated at constant temperature.Then take out the electrothermal ventilation drying box that material prepared is placed on 120 DEG C
Middle 4 h of drying, then cooled to room temperature, with mortar grinder, the half water sulphur of α type of uniform particle diameter is made in the sieving of 180 mesh plugs
Sour calcium powder.
(2) it carries the preparation of medicine fibroin microsphere: vancomycin being added for 1:20 with fibroin albumen quality ratio by vancomycin
Concentration is in the silk fibroin solution of 20mg/mL ~ 60mg/mL, and at normal temperature, 30 min of magnetic agitation is obtained and carried medicine silk fibroin solution.It is real
In testing, taking the concentration of silk fibroin solution is respectively 20 mg/mL, 40 mg/mL and 60 mg/mL.100 are added into 500 mL beakers
ML ethyl acetate, and 2 mL Span80 are added with pipette, under room temperature, after the two is stirred 15 min, using syringe
The silk fibroin solution that 2 ml concentration are 20mg/mL ~ 60mg/mL is instilled dropwise in the mixed solution of stirring.Persistently stir 2 h, silk
Plain microballoon will be suspended in ethyl acetate.Three times to microballoon washing, 12 h are lyophilized under the conditions of -50 DEG C by freeze drier,
Microballoon is collected with spare.
(3) preparation of mineralising fibroin nanofiber solution: silk fibroin protein solution is slowly concentrated for 24 hours at 60 DEG C, is obtained
The more uniform fibroin nanoparticle solution for being 20 wt% to concentration.It is diluted to 0.5wt%, culture is sealed in 60 DEG C of baking ovens
For 24 hours, preparing diameter is 15 ~ 50nm, 1 ~ 2 μm of length of fibroin nanofiber.10mL fibroin is added in 50mL10 times of PBS to receive
In rice fiber solution, 12h is reacted.Precipitating is taken, distilled water cleaning is added.It stands, takes precipitating.Repeatedly, mineralising fibroin is obtained to receive
Rice fiber solution.
By 5wt% ~ 10wt% calcium sulphate dihydrate, 5wt% ~ 10wt% carry medicine fibroin microsphere, 5wt% vancomycin, 75wt% ~
For 85wt% α type half-H 2 O calcium sulphate as solid phase, concentration is the mineralising fibroin nanofiber solution of 3wt% ~ 15wt% as liquid phase.System
Standby anti-infective calcium sulfate/load medicine fibroin microsphere/mineralising fibroin nanofiber bone renovating material.
The invention has the benefit that material has good self-curing when liquid/solid ratio is 0.5mL/g ~ 0.7mL/g
Performance.Material has good biocompatibility, mechanical property, medicament slow release performance, and facilitates the adherency of osteocyte.
Specific embodiment
Embodiment 1
The preparation of α type half-H 2 O calcium sulphate: 300 g calcium sulphate dihydrates and 1.5 g enuatrols are sufficiently mixed, and are added
1200mL distilled water, which stirs evenly, to be placed in closed autoclave, is heated to 120 DEG C, pressure 0.138MPa, is protected
Hold 7 h of pressure heated at constant temperature.It then takes out material prepared and is placed on dry 4 h in 120 DEG C of electrothermal ventilation drying box, from
It is so cooled to room temperature, with mortar grinder, the α type sulfate hemihydrate calcium powder of uniform particle diameter is made in the sieving of 180 mesh plugs.
It carries the preparation of medicine fibroin microsphere: fibroin is added in vancomycin for 1:20 by vancomycin and fibroin albumen quality ratio
In protein solution, at normal temperature, 30 min of magnetic agitation obtains the load medicine silk fibroin solution that concentration is 20mg/mL ~ 60mg/mL.It is real
In testing, taking and carrying the concentration of medicine silk fibroin solution is respectively 20 mg/mL, 40 mg/mL and 60 mg/mL.It is added into 500 mL beakers
100 mL ethyl acetate, and 2 mL Span80 are added with pipette, under room temperature, after the two is stirred 15 min, using note
The load medicine silk fibroin solution that 2 mL concentration are 20 mg/mL or 40 mg/mL or 60 mg/mL is instilled the mixing of stirring by emitter dropwise
In solution.2 h are persistently stirred, carrying medicine fibroin microsphere will be suspended in ethyl acetate.It takes out and carries the washing of medicine fibroin microsphere three times, lead to
It crosses freeze drier and 12 h is lyophilized under the conditions of -50 DEG C, it is spare.
The preparation of mineralising fibroin nanofiber solution: silk fibroin protein solution is slowly concentrated for 24 hours at 60 DEG C, is obtained
Concentration is the fibroin nanoparticle solution of 20 wt%.Fibroin nanoparticle solution is diluted to 0.5wt%, training is sealed in 60 DEG C of baking ovens
It supports for 24 hours, preparing diameter is 15nm ~ 50nm, 1 μm ~ 2 μm of length of fibroin nanofiber solution.10 times of PBS of 50mL are added
Enter in 10mL fibroin nanofiber solution, reacts 12h.Distilled water cleaning is added in taking precipitate.It stands, takes precipitating.It repeats more
It is secondary, obtain mineralising fibroin nanofiber solution.
0.1g calcium sulphate dihydrate, 0.1g are carried medicine fibroin microsphere, 0.1g vancomycin, 1.7g α type half-H 2 O calcium sulphate to mix
Uniformly.Addition 1mL ~ 1.4mL concentration is 3wt% ~ 15wt% mineralising nanometer fibroin fiber solution, and anti-infective calcium sulfate/load medicine is made
Fibroin microsphere/mineralising fibroin nanofiber bone renovating material.
Measuring anti-infective calcium sulfate/load medicine fibroin microsphere/mineralising fibroin nanofiber bone renovating material final setting time is
47min ~ 61min, compression strength are 5.63MPa ~ 7.11MPa, and compression failure function is 12.99J ~ 16.83J.
Increase to 60mg/mL from 20mg/mL with fibroin concentration simultaneously, carries the drug release rate of medicine fibroin microsphere gradually
Reduce, this material 0d ~ 6d drug release rate is that 22% ~ 24%, 0d ~ 22d drug release rate is 60% ~ 63%, carrying drug ratio, encapsulation rate
It is 4.26% ~ 4.44%, 86.94% ~ 91.04%, inhibition zone diameter is 18.67mm ~ 20.59mm.
Embodiment 2
α type half-H 2 O calcium sulphate carries the preparation of medicine fibroin microsphere, mineralising fibroin nanofiber solution with example 1.
0.1g calcium sulphate dihydrate, 0.2g are carried medicine fibroin microsphere, 0.1g vancomycin, 1.6g α type half-H 2 O calcium sulphate to mix
Uniformly.Addition 1mL ~ 1.4mL concentration is 3wt% ~ 15wt% mineralising nanometer fibroin fiber solution, and anti-infective calcium sulfate/load medicine is made
Fibroin microsphere/mineralising fibroin nanofiber bone renovating material.The final setting time for measuring material is 92min ~ 130min, compression strength
For 4.53MPa ~ 6.35MPa, compression failure function is 14.59J ~ 18.83J.As fibroin concentration increases to 60mg/ from 20mg/mL
ML, the drug release rate for carrying medicine fibroin microsphere are gradually reduced, this material 0d ~ 6d drug release rate is 15% ~ 17%, 0d ~ 22d
Drug release rate is 39% ~ 42%, and carrying drug ratio, encapsulation rate are 4.46% ~ 4.64%, 87.98% ~ 92.08%, and inhibition zone diameter is
18.02mm~21.94mm。
Embodiment 3
α type half-H 2 O calcium sulphate carries the preparation of medicine fibroin microsphere, mineralising fibroin nanofiber solution with example 1.
0.2g calcium sulphate dihydrate, 0.2g are carried medicine fibroin microsphere, 0.1g vancomycin, 1.5g α type half-H 2 O calcium sulphate to mix
Uniformly.Addition 1mL ~ 1.4mL concentration is 3wt% ~ 15wt% mineralising nanometer fibroin fiber solution, and anti-infective calcium sulfate/load medicine is made
Fibroin microsphere/mineralising fibroin nanofiber bone renovating material.The final setting time for measuring material is 36min ~ 50min, compression strength
For 4.25MPa ~ 5.99MPa, compression failure function is 15.38J ~ 19.41J.As fibroin concentration increases to 60mg/ from 20mg/mL
ML, the drug release rate for carrying medicine fibroin microsphere are gradually reduced, this material 0d ~ 6d drug release rate is 16% ~ 19%, 0d ~ 22d
Drug release rate is 36% ~ 39%, and carrying drug ratio, encapsulation rate are 4.54% ~ 4.72%, 87.29% ~ 91.39%, and inhibition zone diameter is
19.73mm~21.27mm。
Embodiment 4
α type half-H 2 O calcium sulphate carries the preparation of medicine fibroin microsphere, mineralising fibroin nanofiber solution with example 1.
0.2g calcium sulphate dihydrate, 0.1g are carried medicine fibroin microsphere, 0.1g vancomycin, 1.6g α type half-H 2 O calcium sulphate to mix
Uniformly.Addition 1mL ~ 1.4mL concentration is 3wt% ~ 15wt% mineralising nanometer fibroin fiber solution, and anti-infective calcium sulfate/load medicine is made
Fibroin microsphere/mineralising fibroin nanofiber bone renovating material.The final setting time for measuring material is 21min ~ 35min, compression strength
For 5.12MPa ~ 6.66MPa, compression failure function is 13.29J ~ 16.89J.As fibroin concentration increases to 60mg/ from 20mg/mL
ML, the drug release rate for carrying medicine fibroin microsphere are gradually reduced, this material 0d ~ 6d drug release rate is 16% ~ 18%, 0d ~ 22d
Drug release rate is 45% ~ 48%, and carrying drug ratio, encapsulation rate are 4.03% ~ 4.21%, 86.04% ~ 90.14%, and inhibition zone diameter is
19.14mm~20.62mm。
Embodiment 5
Calcium sulphate dihydrate quality is 0.2g, load medicine fibroin microsphere quality is 0.1g, vancomycin quality is 0.1g, α type half
H 2 O calcium sulphate quality is 1.6g.It is that 5wt% mineralising nanometer fibroin fiber solution stirs evenly that 1.2mL concentration, which is added, when measuring final set
Between be 29min ± 3min, compression strength be ± 0.06 MPa of 6.65MPa, compression failure function be 15.82J ± 0.30J.Fibroin is dense
When degree is 40mg/mL, this material 0d ~ 6d drug release rate is that 16% ± 1%, 0d ~ 22d drug release rate is 45% ± 1%, carries medicine
Rate, encapsulation rate are 4.34% ± 0.03%, 96.38% ± 0.05%, and inhibition zone diameter is 19.88mm ± 0.53mm.It is made anti-infective
Calcium sulfate/load medicine fibroin microsphere/mineralising fibroin nanofiber bone renovating material setting time can be controlled in 30min or so, and full
Sufficient cancellous bone mechanical property has good bacteriostasis property and medicine-releasing performance, and the operation of most Complex Clinical requires.
Illustrate: the PBS in this specification is phosphate buffered saline solution.
Claims (3)
1. anti-infective calcium sulfate/load medicine fibroin microsphere/mineralising fibroin nanofiber bone renovating material, former by Solid raw materials and liquid phase
Material composition, the Solid raw materials are 5wt% ~ 10wt% calcium sulphate dihydrate, 5wt% ~ 10wt% load vancomycin fibroin microsphere, 5wt% ten thousand
Ancient mycin, 75wt% ~ 85wt% α type half-H 2 O calcium sulphate, liquid phase feed use concentration for the mineralising fibroin Nanowire of 3wt% ~ 15wt%
Tie up solution；It is characterized in that its preparation method includes the following steps:
It (1) be 1:20 by vancomycin and fibroin albumen quality ratio by vancomycin addition concentration is 20mg/mL ~ 60mg/mL's
In silk fibroin solution, 30 min of magnetic agitation under room temperature is obtained and is carried vancomycin silk fibroin solution；
(2) 2 mL Span80 are added in 100 mL ethyl acetate, are stirred 15 min, 2 mL concentration of instillation are 20mg/mL
The load vancomycin silk fibroin solution of ~ 60mg/mL persistently stirs 2 h, and ethyl acetate will be suspended in by carrying vancomycin fibroin microsphere
In；
(3) it takes out and carries the washing of vancomycin fibroin microsphere three times, 12 h are lyophilized under the conditions of -50 DEG C by freeze drier, receive
It is spare that collection carries vancomycin fibroin microsphere；
(4) calcium sulphate dihydrate, load vancomycin fibroin microsphere, vancomycin, α type half-H 2 O calcium sulphate are uniformly mixed, mine is added
Change nanometer fibroin fiber solution, obtains anti-infective calcium sulfate/load medicine fibroin microsphere/mineralising fibroin nanofiber Bone Defect Repari material
Material；The anti-infective calcium sulfate/load medicine fibroin microsphere/mineralising fibroin nanofiber bone renovating material is 0.5mL/ in liquid/solid ratio
When g ~ 0.7mL/g, there is good self-curing performance；It is described carry vancomycin fibroin microsphere carrying drug ratio be 4.03wt% ~
4.72wt%；It is porous structure after solidification, porosity is 30% ~ 40%.
2. anti-infective calcium sulfate/load medicine fibroin microsphere/mineralising fibroin nanofiber bone renovating material according to claim 1,
It is characterized in that the preparation step of the mineralising fibroin nanofiber solution is:
(1) silk fibroin protein solution is slowly concentrated to the fibroin nanoparticle solution for obtaining that concentration is 20 wt% for 24 hours at 60 DEG C；
(2) fibroin nanoparticle solution is diluted to 0.5wt%, in 60 DEG C of baking ovens sealing culture for 24 hours, prepare diameter be 15 ~
50nm, length are 1 ~ 2 μm of fibroin nanofibers；
(3) 10 times of PBS of 50mL are added in 10mL fibroin nanofiber solution, react 12h；
(4) sediment is taken out, distilled water cleaning is added；It stands, taking precipitate obtains mineralising fibroin nanofiber solution.
3. anti-infective calcium sulfate/load medicine fibroin microsphere/mineralising fibroin nanofiber bone renovating material according to claim 1,
It is characterized in that the α type half-H 2 O calcium sulphate preparation step is:
(1) calcium sulphate dihydrate is sufficiently mixed with enuatrol, addition 1200mL distilled water, which stirs evenly, is placed on closed high pressure
In reaction kettle；
(2) 120 DEG C are heated to, keeps heating 7 h under the pressure of 0.138MPa and 120 DEG C of constant temperature；
(3) prepared product is taken out from autoclave, is placed in 120 DEG C of electrothermal ventilation drying box dry 4 h；
(4) cooled to room temperature；
(5) 180 mesh sieve are ground and crossed, α type half-H 2 O calcium sulphate is obtained.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610672750.2A CN106267359B (en) | 2016-08-16 | 2016-08-16 | Anti-infective calcium sulfate/load medicine fibroin microsphere/mineralising fibroin nanofiber bone renovating material preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610672750.2A CN106267359B (en) | 2016-08-16 | 2016-08-16 | Anti-infective calcium sulfate/load medicine fibroin microsphere/mineralising fibroin nanofiber bone renovating material preparation method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106267359A CN106267359A (en) | 2017-01-04 |
| CN106267359B true CN106267359B (en) | 2019-06-25 |
Family
ID=57670496
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610672750.2A Active CN106267359B (en) | 2016-08-16 | 2016-08-16 | Anti-infective calcium sulfate/load medicine fibroin microsphere/mineralising fibroin nanofiber bone renovating material preparation method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106267359B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108379654A (en) * | 2018-05-06 | 2018-08-10 | 西北工业大学 | A kind of more gradients carry the preparation method of concentration artificial bone scaffold |
| CN113559315B (en) * | 2021-07-28 | 2022-05-17 | 太原理工大学 | Micro-nano silk fibroin induced bone mineralization calcium phosphate-based bone cement and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102552985A (en) * | 2012-01-20 | 2012-07-11 | 苏州大学 | Silk fibroin/calcium phosphate bone cement-based porous composite material and preparation method thereof |
| CN102764455A (en) * | 2012-07-20 | 2012-11-07 | 清华大学 | Anti-infection mineralized collagen and calcium sulfate bone repair material and preparation method thereof |
| CN103100109A (en) * | 2013-01-28 | 2013-05-15 | 暨南大学 | Silk fibroin composite scaffold loaded with vancomycin/gelatin microspheres and preparation method of silk fibroin composite scaffold |
-
2016
- 2016-08-16 CN CN201610672750.2A patent/CN106267359B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102552985A (en) * | 2012-01-20 | 2012-07-11 | 苏州大学 | Silk fibroin/calcium phosphate bone cement-based porous composite material and preparation method thereof |
| CN102764455A (en) * | 2012-07-20 | 2012-11-07 | 清华大学 | Anti-infection mineralized collagen and calcium sulfate bone repair material and preparation method thereof |
| CN103100109A (en) * | 2013-01-28 | 2013-05-15 | 暨南大学 | Silk fibroin composite scaffold loaded with vancomycin/gelatin microspheres and preparation method of silk fibroin composite scaffold |
Non-Patent Citations (2)
| Title |
|---|
| 丝素蛋白生物材料在骨修复中的应用研究进展;施李杨等;《蚕业科学》;20131231;第39卷(第4期);第0812-0819页 |
| 抗感染硫酸钙/丝素人工骨的构建及相关性能研究;刘力明;《中国优秀硕士学位论文全文数据库 医药卫生科技辑》;20160815(第08期);第E080-38页 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106267359A (en) | 2017-01-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Szcześ et al. | Synthesis of hydroxyapatite for biomedical applications | |
| Saravanan et al. | Chitosan based biocomposite scaffolds for bone tissue engineering | |
| WO2018072679A1 (en) | Biomimetic biomineralized artificial bone repair material and preparation method therefor and use thereof | |
| Fardjahromi et al. | Metal-organic framework-based nanomaterials for bone tissue engineering and wound healing | |
| Fricain et al. | A nano-hydroxyapatite–pullulan/dextran polysaccharide composite macroporous material for bone tissue engineering | |
| Charbonnier et al. | Custom-made macroporous bioceramic implants based on triply-periodic minimal surfaces for bone defects in load-bearing sites | |
| Hou et al. | The hydroxyapatite microtubes enhanced GelMA hydrogel scaffold with inner “pipeline framework” structure for bone tissue regeneration | |
| Zhao et al. | Gadolinium phosphate/chitosan scaffolds promote new bone regeneration via Smad/Runx2 pathway | |
| Zhou et al. | Incorporation of dexamethasone-loaded mesoporous silica nanoparticles into mineralized porous biocomposite scaffolds for improving osteogenic activity | |
| Li et al. | Controllable synthesis of biomimetic hydroxyapatite nanorods with high osteogenic bioactivity | |
| CN108144115B (en) | Injectable bone cement with continuous antibacterial and anti-inflammatory effects and preparation method thereof | |
| CN110051881A (en) | A kind of 3D printing nanometer silver antimicrobial bone renovating material and preparation method thereof | |
| Leng et al. | Material-based therapy for bone nonunion | |
| CN108553691B (en) | Injectable self-curing artificial bone repair material and preparation method thereof | |
| Guo et al. | Biomimetic and immunomodulatory baicalin-loaded graphene oxide-demineralized bone matrix scaffold for in vivo bone regeneration | |
| CN109771693A (en) | A kind of preparation method for the new injectable spontaneous coagulation cmposite artificial bone carrying rhBMP_2 microballoon | |
| Moris et al. | Preparation and characterization of Pullulan-based nanocomposite scaffold incorporating Ag-Silica Janus particles for bone tissue engineering | |
| CN106267359B (en) | Anti-infective calcium sulfate/load medicine fibroin microsphere/mineralising fibroin nanofiber bone renovating material preparation method | |
| Xu et al. | Bone tissue engineering scaffold materials: Fundamentals, advances, and challenges | |
| Rattanachan et al. | Development of injectable chitosan/biphasic calcium phosphate bone cement and in vitro and in vivo evaluation | |
| Jiang et al. | BMSCs-laden mechanically reinforced bioactive sodium alginate composite hydrogel microspheres for minimally invasive bone repair | |
| Miao et al. | Multi-stage controllable degradation of strontium-doped calcium sulfate hemihydrate-tricalcium phosphate microsphere composite as a substitute for osteoporotic bone defect repairing: degradation behavior and bone response | |
| Hussain et al. | GelMA-catechol coated FeHAp nanorods functionalized nanofibrous reinforced bio-instructive and mechanically robust composite hydrogel scaffold for bone tissue engineering | |
| Nabipour et al. | Evaluation of Ibuprofen Release from Gelatin/Hydroxyapatite/Polylactic Acid Nanocomposites: Ibuprofen Release from Gelatin/Hydroxyapatite/Polylactic Acid Nanocomposites | |
| Mudhafar et al. | The natural and commercial sources of hydroxyapatite/collagen composites For biomedical applications: A review study |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20210809 Address after: 030032 No.18, Jinbo street, Taiyuan Tanghuai Park, Shanxi comprehensive reform demonstration zone, Taiyuan City, Shanxi Province Patentee after: SHANXI JINBO BIOMEDICAL Co.,Ltd. Address before: 030024 No. 79 West Main Street, Wan Berlin District, Shanxi, Taiyuan, Yingze Patentee before: Taiyuan University of Technology |