CN108744062A - A kind of injection-type high-strength degradable porous calcium phosphate magnesium bone renovating material - Google Patents
A kind of injection-type high-strength degradable porous calcium phosphate magnesium bone renovating material Download PDFInfo
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- CN108744062A CN108744062A CN201810850018.9A CN201810850018A CN108744062A CN 108744062 A CN108744062 A CN 108744062A CN 201810850018 A CN201810850018 A CN 201810850018A CN 108744062 A CN108744062 A CN 108744062A
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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
- A61L27/56—Porous materials, e.g. foams or sponges
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- 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
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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
- A61L27/14—Macromolecular materials
- A61L27/20—Polysaccharides
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- 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
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2400/00—Materials characterised by their function or physical properties
- A61L2400/06—Flowable or injectable implant compositions
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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
- A61L2430/00—Materials or treatment for tissue regeneration
- A61L2430/02—Materials or treatment for tissue regeneration for reconstruction of bones; weight-bearing implants
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Abstract
The invention discloses a kind of injection-type high-strength degradable porous calcium phosphate magnesium bone renovating materials, it includes solid phase, liquid phase and pore former, and wherein solid phase is mixed by sintered magnesia, hydrophosphate, calcium phosphate and retarder；Liquid phase is water soluble chitosan solution；Pore former is mixed by sweet dew alcohol crystals and sodium alginate；The additive amount of the pore former is the 10-30% of solid phase quality, and pore former and the solid-to-liquid ratio of solid phase gross mass and liquid phase are 0.5-2g/ml.Gained porous calcium phosphate magnesium bone renovating material of the invention ensures good mechanical property on the basis of introducing porous structure into Performances of Magnesium Phosphate Bone Cement repair materials system；And there is good syringeability, degradability and biocompatibility, concentrate the temperature of release low to surrounding, the stabilization for being conducive to itself Bone Defect Repari cell grows into and grows, and has important application value.
Description
Technical field
The invention belongs to medical material technical fields, and in particular to the high intensity Performances of Magnesium Phosphate Bone Cement of pore-forming in a kind of injectable body
Cement material and preparation method thereof.
Background technology
The conventional method of clinical treatment bone defect includes mainly that autologous bone transplanting, homogeneous allogenic bone transplantation and bone substitute material
Material implantation etc..Autotransplantation is since enough bone grafts are difficult to obtain, and postoperative the problems such as may occur in which complication at materials, cannot
Meet the medical demand of orthopedic implant.Homograft and heterograft are well to select, but infect and be immunized with disease
Repel equivalent risk.Synthetic bone graft replacement is the reasonable selection for catering to the orthopedic implant demand increased rapidly, at present clinically
Synthetic material for Bone Defect Repari includes mainly calcium sulfate, calcium phosphate, polymethyl methacrylate (PMMA) etc..Calcium phosphate
Although having good biocompatibility, its degradation is very slow, and intensity is relatively low, bonding force is poor.PMMA is ossified
Big calorimetric is discharged in the process, causes surrounding tissue downright bad, and PMMA non-degradables, bioactivity are poor.Magnesium phosphate cement is a kind of
Novel bone renovating material has the characteristics that early strength is high, degradable, has a good application prospect.
However, there is also some problems in application process for magnesium phosphate cement at present：1) reaction of magnesium phosphate cement
Amount of heat is discharged to surrounding in the process, causes tissue necrosis and local inflammation reaction, is had an adverse effect to bone tissue healing,
And setting time is short, is unfavorable for clinical practice operation；2) structure that slurry is formed in injecting bone defect after self-solidifying is finer and close, no
It is divided into osteoblast conducive to Bone Defect Repari process mescenchymal stem cell and early stage osteoblast arrival filling region and forms sclerotin,
There is inhibition to union；3) porous calcium phosphate magnesium strength of bone cement is insufficient, cannot meet the Initial stability in heavy burden area；
4) essential amino acid needed for local Bone Defect Repari can not be provided.
Invention content
In view of the deficiency of the prior art, the main purpose of the present invention is to provide one kind can in vivo pore-forming it is high-strength
Magnesium phosphate cement material is spent, effectively solves fine and close bone repairing support Bone Ingrowth, the problems such as Integrated implant is not good enough.
To achieve the above object, the technical solution adopted by the present invention is：
A kind of injection-type high-strength degradable porous calcium phosphate magnesium bone renovating material, including solid phase, liquid phase and pore former, wherein
Solid phase is mixed by sintered magnesia, hydrophosphate, calcium phosphate and compound retarder；Liquid phase is water soluble chitosan solution；
Pore former is mixed by sweet dew alcohol crystals and sodium alginate；The pore former is the 10-30% of solid phase quality, pore former and solid
The solid-to-liquid ratio of phase gross mass and liquid phase is 0.5-2g/ml.
In said program, each component and its shared mass percent include in the solid phase：Sintered magnesia 10-30%,
Hydrophosphate 60-80%, calcium phosphate 5-10%, retarder 1-10%.
In said program, a concentration of 5-25wt% of the water soluble chitosan solution.
In said program, the water soluble chitosan solution is chitosan lactate, chitosan quaternary ammonium salt, chitosan hydrochloric acid
Salt, hydroxypropyl chitosan or carboxymethyl chitosan solution etc..
In said program, each component and its shared mass percent include in the pore former：Sweet dew alcohol crystals 20-
80%, sodium alginate 20-80%.
In said program, the grain size of the sintered magnesia is 1~75 μm, the temperature by magnesium hydroxide at 1400-1800 DEG C
5~8h is calcined under the conditions of degree, ball milling is crossed 200 mesh sieve and obtained；Calcination time extends, and MgO activity can be improved；Gained magnesia
Powder diameter is smaller, and MgO activity is higher.
In said program, the hydrophosphate includes ammonium di-hydrogen phosphate, disodium hydrogen phosphate, dipotassium hydrogen phosphate, biphosphate
One or more of potassium, sodium dihydrogen phosphate.
In said program, the calcium phosphate includes the one or both mixture in type alpha tricalcium phosphate, bata-tricalcium phosphate.
It is described in said program, the retarder be amino acids retarder, be lysine, tryptophan, phenylalanine,
The mixture of one or more of methionine, threonine, isoleucine, leucine, valine.
In said program, the sweet dew alcohol crystals preparation method is as follows：By mannitol and ethyl alcohol 1-3 by volume:1,50-
Heating stirring under the conditions of 80 DEG C fully after dissolving, stands cooling acquisition sweet dew alcohol crystals, sweet dew alcohol crystals is filtered by vacuum, are dried
It is dry, it is spare.
Compared with prior art, beneficial effects of the present invention are：
1) present invention can effectively reduce phosphorus by adding amino acids retarder during preparing magnesium phosphate cement
Sour magnesium bone cement hydration reaction speed and hydration reaction rate of heat release reduce the thermal damage to surrounding tissue；In addition, retarder
The intensity that not will be greatly reduced the magnesium phosphate cement is added, does not change the composition and structure of its hydrated product；Meanwhile amino
Essential amino acid needed for local Bone Defect Repari can also be provided in acids retarder；
2) present invention is during preparing magnesium phosphate cement by adding water soluble chitosan, by with magnesium calcium etc. from
The chelation of son increases considerably the intensity of the magnesium phosphate cement, and does not change microenvironment pH value simultaneously, maintains physiologic ring
Border stable state is conducive to growing into and growing for body itself Bone Defect Repari cell；
3) present invention is used as again by adding sweet dew alcohol crystals and sodium alginate during preparing magnesium phosphate cement
Pore creating material is closed, the characteristic of internal pore-forming is provided for magnesium phosphate cement, makes gained bone cement that there is guiding bone uptake and promotes bone
The potential grown into；The addition of sodium alginate can form gel in mannitol plane of crystal, protect mannitol not molten when preparing
Solution；And the gel formed is attached to hole wall, can increase pore-creating character and histocompatbility, be conducive to the migration and life of Bone Defect Repari cell
It is long；In addition, sweet dew alcohol crystals and sodium alginate are compounded, obtained by guarantee under the premise of bone renovating material porous performance,
Its strength character can further be improved.
Description of the drawings
Fig. 1 is the process flow diagram of porous calcium phosphate magnesium bone renovating material of the present invention；
Fig. 2 is the scanning electron microscope (SEM) photograph of cell growth on 1 gained bone renovating material of embodiment；
The curve graph that Fig. 3 porogen contents influence the compression strength of porous calcium phosphate magnesium bone renovating material；
The curve graph that Fig. 4 porogen contents influence the porosity characteristic of porous calcium phosphate magnesium bone renovating material；
Fig. 5 is the scanning electron microscope (SEM) photograph of cell growth on 1 gained bone renovating material of comparative example.
Specific implementation mode
It elaborates below to the embodiment of the present invention, the present embodiment is carried out lower based on the technical solution of the present invention
Implement, gives detailed embodiment and specific operating process, but protection scope of the present invention is not limited to following implementation
Example.
In following embodiment, the sintering oxidation magnesium powder of use calcines 8h at 1500 DEG C by magnesium hydroxide, and medical grade burning is made
Magnesia is tied, then obtains magnesium oxide powder through ball milling, the sieve of 200 mesh excessively and forms, grain size is about 1~75 μm；The magnesia crystal
With certain activity, the presence of activated magnesia contributes to magnesium phosphate cement to form skeleton structure.
The preparation method of the sweet dew alcohol crystals of use is as follows：By mannitol and ethyl alcohol 1-3 by volume:1 mixing, in 50-
It is stirred at 80 DEG C, fully after dissolving, stands cooling acquisition sweet dew alcohol crystals, sweet dew alcohol crystals are filtered by vacuum, are dried, sieving,
It is spare.
Embodiment 1
A kind of injection-type high-strength degradable porous calcium phosphate magnesium bone renovating material, process flow diagram are shown in Fig. 1, specifically
Preparation process is as follows：
1) by 100 parts of (parts by weight, similarly hereinafter) sintering oxidation magnesium powders, 400 parts of phosphate, 50 parts of calcium phosphate, 20 parts of retarder
(each 10 parts of L-lysine, L-Trp) is uniformly mixed, and obtains magnesium phosphate cement solid phase；
2) chitosan lactate is added in deionized water, compound concentration is the water soluble chitosan solution of 10wt%, shake
It swings uniformly, obtains liquid phase；
3) sweet dew alcohol crystals and sodium alginate are pressed 1:2 mass ratio mixing, obtains pore former；
4) pore former is first added in solid phase, the additive amount of pore former is the 10% of solid phase quality；Then according to solid-to-liquid ratio
Solid-liquid two-phase is successively added to by 1g/ml (solid-to-liquid ratio refers to the ratio between above-mentioned magnesium phosphate cement solid phase quality and liquid phase volume herein)
In capsule, glass bar stirs 1-2min, forms uniform slurry, to get the porous calcium phosphate magnesium Bone Defect Repari material after its solidification
Material.
The final setting time of porous calcium phosphate magnesium bone renovating material obtained by the present embodiment is 11.8min, has good injectable
Performance；And 55.3 DEG C of the reaction maximum temperature monitored；Compression strength is 47.2MPa；Porosity is 24.9%；Transplanting is real in vivo
Verification can reach 25.3% degradation rate when 12 weeks real.
The cell growth schematic diagram of porous calcium phosphate magnesium bone renovating material obtained by the present embodiment is shown in Fig. 2, as seen from Figure 2 institute
Bone renovating material good biocompatibility is obtained, cell is successfully colonized in material surface.
Additive amount by adjustment hole agent with respect to solid phase, gained porogen content resist porous calcium phosphate magnesium bone renovating material
The curve graph that Compressive Strength influences and porosity characteristic influences is shown in Fig. 3 and Fig. 4 respectively.
Embodiment 2
The preparation method of porous calcium phosphate magnesium bone renovating material described in the present embodiment is roughly the same with embodiment 1, difference
It is：In step 1) solid phase by 100 parts of sintering oxidation magnesium powders, 400 parts of phosphate, 50 parts of calcium phosphate, (L- relies ammonia to 40 parts of retarder
Acid, each 20 parts of L-Trp) mix, a concentration of 15wt% of chitosan lactate solution, pore former are by sweet dew alcohol crystals
With sodium alginate 2:1 mass ratio mixes, the additive amount of pore former is the 15% of solid phase quality, solid-to-liquid ratio 2g/ml.
The final setting time of porous calcium phosphate magnesium bone renovating material obtained by the present embodiment is 17.5min；React maximum temperature 43.7
℃；Compression strength is 43.6MPa；Porosity is 29.5%.
Embodiment 3
The preparation method of porous calcium phosphate magnesium bone renovating material described in the present embodiment is roughly the same with embodiment 1, difference
It is：In step 1) solid phase by 100 parts of sintering oxidation magnesium powders, 400 parts of phosphate, 50 parts of calcium phosphate, (L- relies ammonia to 40 parts of retarder
Acid, each 20 parts of L-Trp) mix, a concentration of 15wt% of chitosan hydrochloride solution, pore former are by sweet dew alcohol crystals
With sodium alginate 1:1 mass ratio mixes, the additive amount of pore former is the 20% of solid phase quality, solid-to-liquid ratio 2g/ml.
The final setting time of porous calcium phosphate magnesium bone renovating material obtained by the present embodiment is 18.4min；React maximum temperature 44.8
℃；Compression strength is 37.8MPa；Porosity is 33.7%.
Comparative example 1
A kind of bone renovating material, specific preparation process are as follows：
1) by 100 parts of sintering oxidation magnesium powders, 400 parts of phosphate, 50 parts of calcium phosphate, 20 parts of compound retarders (L-lysine,
Each 10 parts of L-Trp) it is uniformly mixed, obtain magnesium phosphate cement solid phase；
2) water soluble chitosan is added in deionized water, compound concentration is the water soluble chitosan solution of 10wt%, shake
It swings uniformly, obtains liquid phase；
3) only using sweet dew alcohol crystals as pore former；
4) pore former is first added in solid phase, the additive amount of pore former is the 10% of solid phase quality；Then according to solid-to-liquid ratio
Solid-liquid two-phase is successively added to by 1g/ml (solid-to-liquid ratio refers to the ratio between above-mentioned magnesium phosphate cement solid phase quality and liquid phase volume herein)
In capsule, glass bar stirs 1-2min, forms uniform slurry, to get the bone renovating material after its solidification.
The final setting time of porous calcium phosphate magnesium bone renovating material obtained by this comparative example is 11.2min；The reaction highest monitored
56.0 DEG C of temperature；Compression strength is 33.6MPa；Porosity is 22.6%；Compared with Example 1, illustrate that the present invention is ensureing institute
Under the premise of obtaining bone renovating material porous performance, its strength character can be also further promoted.
Fig. 5 is cells grown figure under the conditions of same as Example 1 on bone renovating material obtained by this comparative example, can be seen
Go out, due to lacking the protection of sodium alginate, cell is colonized that quantity is few, poor morphology, is unfavorable for Bone Defect Repari.
The foregoing is merely the preferred embodiment of the present invention, it is noted that comes for those of ordinary skill in the art
It says, without departing from the concept of the premise of the invention, makes several modifications and variations, these belong to the protection model of the present invention
It encloses.
Claims (10)
1. a kind of injection-type high-strength degradable porous calcium phosphate magnesium bone renovating material, which is characterized in that including solid phase, liquid phase and at
Hole agent, wherein solid phase are mixed by sintered magnesia, hydrophosphate, calcium phosphate and compound retarder；Liquid phase is water soluble shells
Glycan solution；Pore former is mixed by sweet dew alcohol crystals and sodium alginate；The additive amount of the pore former is solid phase quality
10-30%, pore former and the solid-to-liquid ratio of solid phase gross mass and liquid phase are 0.5-2g/ml.
2. injection-type high-strength degradable porous calcium phosphate magnesium bone renovating material according to claim 1, which is characterized in that institute
Stating each component and its shared mass percent in solid phase includes：Sintered magnesia 10-30%, hydrophosphate 60-80%, calcium phosphate
5-10%, retarder 1-10%.
3. injection-type high-strength degradable porous calcium phosphate magnesium bone renovating material according to claim 1, which is characterized in that institute
State a concentration of 5-25wt% of water soluble chitosan solution.
4. injection-type high-strength degradable porous calcium phosphate magnesium bone renovating material according to claim 1, which is characterized in that institute
It is 1 to state the mass ratio of sweet dew alcohol crystals and sodium alginate in pore former:(0.25~4).
5. injection-type high-strength degradable porous calcium phosphate magnesium bone renovating material according to claim 1, which is characterized in that institute
The grain size for stating sintered magnesia is 1-75 μm.
6. injection-type high-strength degradable porous calcium phosphate magnesium bone renovating material according to claim 5, which is characterized in that institute
It states after sintered magnesia calcines 5~8h, ball milling by magnesium hydroxide under 1400-1800 DEG C of temperature condition and crosses the sieve acquisition of 200 mesh.
7. injection-type high-strength degradable porous calcium phosphate magnesium bone renovating material according to claim 1, which is characterized in that institute
It includes one kind in ammonium di-hydrogen phosphate, disodium hydrogen phosphate, dipotassium hydrogen phosphate, potassium dihydrogen phosphate, sodium dihydrogen phosphate to state hydrophosphate
Or it is several.
8. injection-type high-strength degradable porous calcium phosphate magnesium bone renovating material according to claim 1, which is characterized in that institute
It includes the one or both mixture in type alpha tricalcium phosphate, bata-tricalcium phosphate to state calcium phosphate.
9. injection-type high-strength degradable porous calcium phosphate magnesium bone renovating material according to claim 1, which is characterized in that institute
It is amino acids retarder to state retarder.
10. injection-type high-strength degradable porous calcium phosphate magnesium bone renovating material according to claim 1, which is characterized in that
The sweet dew alcohol crystals preparation method is as follows：By mannitol and ethyl alcohol 1-3 by volume:1, and heated under the conditions of 50-80 DEG C
Stirring fully after dissolving, stands cooling and obtains sweet dew alcohol crystals, sweet dew alcohol crystals are filtered by vacuum, dry, spare.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110251722A (en) * | 2019-07-31 | 2019-09-20 | 华东理工大学 | Phosphoric acid magnesium-based bone renovating material, feedstock composition and preparation method thereof, application |
| CN111110929A (en) * | 2020-02-15 | 2020-05-08 | 王雯雯 | High-biosafety heart stent and manufacturing method thereof |
| CN111330086A (en) * | 2020-03-05 | 2020-06-26 | 广东省中医院（广州中医药大学第二附属医院、广州中医药大学第二临床医学院、广东省中医药科学院） | Bionic artificial bone scaffold material and preparation method thereof |
| CN113209369A (en) * | 2021-04-29 | 2021-08-06 | 西安理工大学 | Preparation method of high-porosity magnesium phosphate bone cement composite porous scaffold |
| CN113398333A (en) * | 2021-06-01 | 2021-09-17 | 南京方拓新材料科技有限责任公司 | Hydrogel-based calcium magnesium phosphate material and application thereof as bone repair material |
| CN114917397A (en) * | 2022-06-13 | 2022-08-19 | 北京纳通医学研究院有限公司 | Solid phase composition of bone adhesive and bone adhesive |
| CN115448635A (en) * | 2022-09-05 | 2022-12-09 | 沈阳理工大学 | Composite retarder for magnesium potassium phosphate cement and use method thereof |
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