CN112546304A - Preparation method of injectable bone repair material - Google Patents
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Abstract
The invention belongs to the technical field of biomedical materials, and particularly relates to a preparation method of an injectable bone repair material. The invention uses pig bones and cow bones as basic raw materials, can reduce the rejection phenomenon with human bone materials, secondly, partial foreign matters can be eliminated by hydrochloric acid soaking, then the mixture is mixed by additives, steam explosion is utilized, in the process, the porosity of the bone is increased by the additive, and then the bone is mixed with the mixture, the hydroxyapatite lime is formed by the mixture and is deposited in the pores, the fusion degree with the human bone is improved, secondly, the microelements are attached to the surface of the bone in a micro-encapsulation way, and the added microelements can effectively promote the repair and increase of the self bone, the lecithin can improve the combination of bones to self calcium ions and enhance the repair of the bones, and then the gum arabic is wrapped and microencapsulated, so that the water solubility and the dispersibility in water are improved, the injection performance is improved, and the repair effect is improved by a cross-linking agent.
Description
Technical Field
The invention belongs to the technical field of biomedical materials, and particularly relates to a preparation method of an injectable bone repair material.
Background
The repair of bone defects or bone injuries caused by bone tumors, congenital bone abnormalities, wounds and the like has been a difficult problem in clinical bone repair. Currently, the main repair modalities are autologous bone, allogeneic bone and artificial bone repair material transplantation. Since the autologous bone source is limited and the obtained material can cause the injury of the secondary operation to the patient, etc., the autologous bone transplantation operation can not meet the requirements of the patient with large-area bone defect. Allogeneic bone transplantation exposes the patient to secondary risks associated with immune rejection and the spread of serious disease. There is no doubt that the demand for artificial bone repair materials will be greater and greater due to the pressure of clinical bone repair.
Although the autogenous bone is an ideal bone defect repairing material, the bone taking process increases the trauma and pain of patients, the bone source is limited, the shaping is not easy, and the requirement of large-section bone transplantation is difficult to meet; allogeneic bone may transmit diseases and cause postoperative complications due to immunological rejection; the metal prosthesis has the problems of easy loosening, fracture, poor tissue compatibility, nondegradable property and the like. The theory and technology of injectable tissue engineering bone and minimally invasive surgery have the advantages of non-invasion or minimally invasive surgery, have good application prospect and are highly valued by the medical and materials communities. In recent years, the injectable bone repair materials to be studied are mainly ceramics, polymers and composites of the two.
The ceramic bone repair material mainly comprises calcium phosphate salts such as Hydroxyapatite (HA), calcium phosphate (CaP), Biphase Calcium Phosphate (BCP), CPC, calcium sulfate and the like. In the ceramic bone repair material, HA is the main component of natural bone, HAs good biocompatibility, can effectively stimulate bone conduction, can be slowly replaced by host bone after being implanted, and is probably the best bone repair material. However, since the block-shaped artificial HA is unsatisfactory in bone induction and is susceptible to loosening and cracking in clinical practice, researchers have developed porous HA blocks, particles and microspheres.
The single ceramic material is not easy to form in vivo or easy to loosen after forming, and the single gel material is easy to generate larger cavities due to degradation and can not meet the requirement of repairing larger bone defects. Therefore, inorganic-polymer composite-injectable ceramic/polymer composite materials with biomimetic nature have received great attention in recent years.
Currently, calcium sulfate has been widely studied and clinically used as an injectable bone repair material. Modern surgical grade calcium sulfate provides high initial strength and good injection handling properties. However, the pore size and porosity of the calcium sulfate material are small, which is not favorable for the migration of osteoblasts and angiogenesis. There is therefore a need for an injectable bone repair material that combines properties of suitable porosity, pore size, strength, etc.
Disclosure of Invention
The technical problems to be solved by the invention are as follows: aiming at the problem that the pore diameter and porosity of the existing calcium sulfate material are small and are not beneficial to the migration of osteoblasts and angiogenesis, the preparation method of the injectable bone repair material is provided.
In order to solve the technical problems, the invention adopts the following technical scheme:
a method for preparing an injectable bone repair material, the method comprising the steps of:
(1) soaking the mixed bone powder in a hydrochloric acid solution, ultrasonically vibrating, filtering, washing, drying, collecting a dried substance, uniformly mixing the dried substance, an additive and an ethanol solvent according to a mass ratio of 10: 1-3: 12, maintaining the pressure for 3min at 5-8 MPa, performing steam explosion, filtering, and collecting a filter cake;
(2) putting the filter cake into an oven, heating to 700-800 ℃ at a speed of 5 ℃/min, carrying out heat preservation drying, cooling, collecting the dried substance, and taking 130-150 parts of water, 70-80 parts of the dried substance, 20-25 parts of the mixture and 5-8 parts of a surfactant according to parts by weight;
(3) firstly, putting water, a dried substance and a mixture into a reactor, adjusting the pH value to 10-11, heating, stirring, adding a surfactant, continuously stirring, standing, filtering, washing, calcining, and collecting a calcined substance;
(4) uniformly stirring the calcined substance, the liquid paraffin and the trace substance according to the mass ratio of 6-10: 18:3, adding 1-3 times of Arabic gum by mass of the calcined substance, adjusting the pH to 4, stirring at 500r/min, adding water for diluting, cooling, adding a cross-linking agent accounting for 5-7% of the calcined substance, standing, and spray-drying to obtain the injectable bone repair material.
Preferably, the mixed bone powder in the step (1) is prepared by crushing pig bones and ox bones according to the mass ratio of 12: 4-7, sieving, and collecting sieved particles to obtain the mixed bone powder.
Preferably, the additive in the step (1) is prepared by uniformly mixing urea and sodium bicarbonate according to a mass ratio of 5: 2-3.
Preferably, the mixture is formed by mixing calcium nitrate and diammonium hydrogen phosphate according to the mass ratio of 1: 1.5-2.5.
Preferably, the surfactant is any one of sodium dodecyl benzene sulfonate and sodium dodecyl sulfate.
Preferably, the trace substance in the step (4) is vitamin D and lecithin which are uniformly mixed according to the mass ratio of 15:1, so that the trace substance is obtained.
Preferably, in the step (4), the cross-linking agent is any one of genipin and glutaraldehyde.
Compared with other methods, the method has the beneficial technical effects that:
the invention uses pig bones and cow bones as basic raw materials, can reduce the rejection phenomenon with human bone materials, can eliminate partial foreign matters through hydrochloric acid soaking, reduces certain bone hardness, then is mixed through additives, utilizes steam explosion, increases the porosity of bones through the additives in the process, then is mixed with the mixture, forms hydroxyapatite through the mixture to deposit in pores, can effectively control the pore diameter, can increase the bone strength, simultaneously improves the fusion degree with human bones, can improve the solidification among repairing materials through micro-encapsulation attaching on the bone surface through trace elements, further enhances the bone strength, simultaneously can effectively promote the repair increase of self bones by the added trace elements, and can improve the combination of bones to self calcium ions and enhance the bone repair, and finally, the curing effect and the repairing effect are improved through a cross-linking agent.
Detailed Description
The mixed bone powder is prepared by crushing pig bones and ox bones at a mass ratio of 12: 4-7 at a speed of 900r/min for 2h, sieving with a 500-mesh sieve, and collecting sieved particles to obtain the mixed bone powder.
The additive is prepared by uniformly mixing urea and sodium bicarbonate according to the mass ratio of 5: 2-3.
The mixture is formed by mixing calcium nitrate and diammonium hydrogen phosphate according to the mass ratio of 1: 1.5-2.5.
The surfactant is any one of sodium dodecyl benzene sulfonate and sodium dodecyl sulfate.
The trace substance is prepared by uniformly mixing vitamin D and lecithin according to the mass ratio of 15: 1.
The cross-linking agent is any one of genipin and glutaraldehyde.
A method for preparing an injectable bone repair material, the method comprising the steps of:
(1) soaking the mixed bone powder in 1.3mol/L hydrochloric acid solution for 6h, ultrasonically oscillating for 30min, filtering, washing with water to be neutral, drying, collecting dried substances, uniformly mixing the dried substances, additives and 1.2mol/L ethanol solvent according to the mass ratio of 10: 1-3: 12, maintaining the pressure for 3min at 5-8 MPa, performing steam explosion, filtering, and collecting filter cakes;
(2) putting the filter cake into an oven, heating to 700-800 ℃ at a speed of 5 ℃/min, carrying out heat preservation and drying for 6-9 h, cooling to room temperature, collecting the dried substance, and taking 130-150 parts of water, 70-80 parts of the dried substance, 20-25 parts of the mixture and 5-8 parts of surfactant according to parts by weight;
(3) firstly, putting water, a dried substance and a mixture into a reactor, adjusting the pH value to 10-11, heating to 50-60 ℃, stirring for 4h at 500r/min, adding a surfactant, continuously stirring for 3h, standing for 12h, filtering, washing, calcining for 2h at 600 ℃, and collecting a calcined substance;
(4) uniformly stirring the calcined substance, the liquid paraffin and the trace substance according to the mass ratio of 6-10: 18:3, adding Arabic gum with the mass of 1-3 times that of the calcined substance, adjusting the pH value to 4, stirring for 7 hours at 500r/min, adding water with the volume of 3 times that of the liquid paraffin for dilution, cooling to 5 ℃, adding a cross-linking agent with the mass of 5-7% that of the calcined substance, standing for 9 hours, and performing spray drying to obtain the injectable bone repair material.
Example 1
The mixed bone powder is prepared by pulverizing Os Sus Domestica and Os bovis Seu Bubali at a mass ratio of 12:7 at 900r/min for 2h, sieving with 500 mesh sieve, collecting sieved granule, and making into mixed bone powder.
The additive is prepared by uniformly mixing urea and sodium bicarbonate according to the mass ratio of 5: 3.
The mixture is formed by mixing calcium nitrate and diammonium hydrogen phosphate according to the mass ratio of 1: 2.5.
The surfactant is any one of sodium dodecyl benzene sulfonate and sodium dodecyl sulfate.
The trace substance is prepared by uniformly mixing vitamin D and lecithin according to the mass ratio of 15: 1.
The cross-linking agent is any one of genipin and glutaraldehyde.
A method for preparing an injectable bone repair material, the method comprising the steps of:
(1) soaking the mixed bone powder in 1.3mol/L hydrochloric acid solution for 6h, ultrasonically shaking for 30min, filtering, washing with water to neutrality, drying, collecting the dried product, uniformly mixing the dried product, additive and 1.2mol/L ethanol solvent according to the mass ratio of 10: 3:12, maintaining the pressure for 3min at 8MPa, performing steam explosion, filtering, and collecting the filter cake;
(2) putting the filter cake into an oven, heating to 800 ℃ at a speed of 5 ℃/min, carrying out heat preservation and drying for 9h, cooling to room temperature, collecting the dried substance, and taking 150 parts of water, 80 parts of the dried substance, 25 parts of the mixture and 8 parts of surfactant according to parts by weight;
(3) firstly, putting water, a dried substance and a mixture into a reactor, adjusting the pH value to 11, heating to 60 ℃, stirring for 4h at 500r/min, adding a surfactant, continuously stirring for 3h, standing for 12h, filtering, washing, calcining for 2h at 600 ℃, and collecting a calcined substance;
(4) uniformly stirring the calcined substance, the liquid paraffin and the trace substance according to the mass ratio of 10:18:3, adding 3 times of Arabic gum of the calcined substance, adjusting the pH to 4, stirring for 7 hours at 500r/min, adding 3 times of water of the volume of the liquid paraffin, diluting, cooling to 5 ℃, adding 7% of cross-linking agent of the calcined substance, standing for 9 hours, and spray-drying to obtain the injectable bone repair material.
Example 2
The mixed bone powder is prepared by pulverizing Os Sus Domestica and Os bovis Seu Bubali at a mass ratio of 12:6 at 900r/min for 2h, sieving with 500 mesh sieve, collecting sieved granule, and making into mixed bone powder.
The additive is prepared by uniformly mixing urea and sodium bicarbonate according to the mass ratio of 5: 2.5.
The mixture is formed by mixing calcium nitrate and diammonium phosphate according to the mass ratio of 1: 2.
The surfactant is any one of sodium dodecyl benzene sulfonate and sodium dodecyl sulfate.
The trace substance is prepared by uniformly mixing vitamin D and lecithin according to the mass ratio of 15: 1.
The cross-linking agent is any one of genipin and glutaraldehyde.
A method for preparing an injectable bone repair material, the method comprising the steps of:
(1) soaking the mixed bone powder in 1.3mol/L hydrochloric acid solution for 6h, ultrasonically shaking for 30min, filtering, washing with water to neutrality, drying, collecting the dried product, uniformly mixing the dried product, additive and 1.2mol/L ethanol solvent according to the mass ratio of 10:2:12, maintaining the pressure for 3min at 7MPa, performing steam explosion, filtering, and collecting the filter cake;
(2) putting the filter cake into an oven, heating to 750 ℃ at the speed of 5 ℃/min, carrying out heat preservation and drying for 8h, cooling to room temperature, collecting the dried substance, and taking 140 parts of water, 75 parts of the dried substance, 23 parts of the mixture and 7 parts of surfactant according to parts by weight;
(3) firstly, putting water, a dried substance and a mixture into a reactor, adjusting the pH value to 10.5, heating to 55 ℃, stirring for 4h at 500r/min, adding a surfactant, continuously stirring for 3h, standing for 12h, filtering, washing, calcining for 2h at 600 ℃, and collecting a calcined substance;
(4) uniformly stirring the calcined substance, the liquid paraffin and the trace substance according to the mass ratio of 8:18:3, adding Arabic gum with the mass 2 times that of the calcined substance, adjusting the pH to 4, stirring for 7 hours at 500r/min, adding water with the volume 3 times that of the liquid paraffin for dilution, cooling to 5 ℃, adding a cross-linking agent with the mass 6% that of the calcined substance, standing for 9 hours, and performing spray drying to obtain the injectable bone repair material.
Example 3
The mixed bone powder is prepared by pulverizing Os Sus Domestica and Os bovis Seu Bubali at a mass ratio of 12:4 at 900r/min for 2h, sieving with 500 mesh sieve, collecting sieved granule, and making into mixed bone powder.
The additive is prepared by uniformly mixing urea and sodium bicarbonate according to the mass ratio of 5:2.
The mixture is formed by mixing calcium nitrate and diammonium phosphate according to the mass ratio of 1: 1.5.
The surfactant is any one of sodium dodecyl benzene sulfonate and sodium dodecyl sulfate.
The trace substance is prepared by uniformly mixing vitamin D and lecithin according to the mass ratio of 15: 1.
The cross-linking agent is any one of genipin and glutaraldehyde.
A method for preparing an injectable bone repair material, the method comprising the steps of:
(1) soaking the mixed bone powder in 1.3mol/L hydrochloric acid solution for 6h, ultrasonically shaking for 30min, filtering, washing with water to neutrality, drying, collecting the dried product, uniformly mixing the dried product, additive and 1.2mol/L ethanol solvent according to the mass ratio of 10:1:12, maintaining the pressure for 3min at 5MPa, performing steam explosion, filtering, and collecting the filter cake;
(2) putting the filter cake into an oven, heating to 700 ℃ at a speed of 5 ℃/min, carrying out heat preservation and drying for 6h, cooling to room temperature, collecting the dried substance, and taking 130 parts of water, 70 parts of the dried substance, 20 parts of the mixture and 5 parts of a surfactant according to parts by weight;
(3) firstly, putting water, a dried substance and a mixture into a reactor, adjusting the pH value to 10, heating to 50 ℃, stirring for 4h at 500r/min, adding a surfactant, continuously stirring for 3h, standing for 12h, filtering, washing, calcining for 2h at 600 ℃, and collecting a calcined substance;
(4) uniformly stirring the calcined substance, the liquid paraffin and the trace substance according to the mass ratio of 6:18:3, adding Arabic gum with the mass of 1 time of the calcined substance, adjusting the pH to 4, stirring for 7 hours at 500r/min, adding water with the volume of 3 times of the liquid paraffin for dilution, cooling to 5 ℃, adding a cross-linking agent with the mass of 5% of the calcined substance, standing for 9 hours, and performing spray drying to obtain the injectable bone repair material.
Comparative example 1
The mixed bone powder is prepared by pulverizing Os Sus Domestica and Os bovis Seu Bubali at a mass ratio of 12:6 at 900r/min for 2h, sieving with 500 mesh sieve, collecting sieved granule, and making into mixed bone powder.
The additive is prepared by uniformly mixing urea and sodium bicarbonate according to the mass ratio of 5: 2.5.
The mixture is formed by mixing calcium nitrate and diammonium phosphate according to the mass ratio of 1: 2.
The surfactant is any one of sodium dodecyl benzene sulfonate and sodium dodecyl sulfate.
The cross-linking agent is any one of genipin and glutaraldehyde.
A method for preparing an injectable bone repair material, the method comprising the steps of:
(1) soaking the mixed bone powder in 1.3mol/L hydrochloric acid solution for 6h, ultrasonically shaking for 30min, filtering, washing with water to neutrality, drying, collecting the dried product, uniformly mixing the dried product, additive and 1.2mol/L ethanol solvent according to the mass ratio of 10:2:12, maintaining the pressure for 3min at 7MPa, performing steam explosion, filtering, and collecting the filter cake;
(2) putting the filter cake into an oven, heating to 750 ℃ at the speed of 5 ℃/min, carrying out heat preservation and drying for 8h, cooling to room temperature, collecting the dried substance, and taking 140 parts of water, 75 parts of the dried substance, 23 parts of the mixture and 7 parts of surfactant according to parts by weight;
(3) firstly, putting water, a dried substance and a mixture into a reactor, adjusting the pH value to 10.5, heating to 55 ℃, stirring for 4h at 500r/min, adding a surfactant, continuously stirring for 3h, standing for 12h, filtering, washing, calcining for 2h at 600 ℃, and collecting a calcined substance;
(4) uniformly stirring the calcined substance and the liquid paraffin according to the mass ratio of 8:18, adding Arabic gum with the mass 2 times that of the calcined substance, adjusting the pH value to 4, stirring for 7 hours at the speed of 500r/min, adding water with the volume 3 times that of the liquid paraffin for dilution, cooling to 5 ℃, adding a cross-linking agent with the mass 6% of the calcined substance, standing for 9 hours, and performing spray drying to obtain the injectable bone repair material.
Comparative example 2
The mixed bone powder is prepared by pulverizing Os Sus Domestica and Os bovis Seu Bubali at a mass ratio of 12:6 at 900r/min for 2h, sieving with 500 mesh sieve, collecting sieved granule, and making into mixed bone powder.
The additive is prepared by uniformly mixing urea and sodium bicarbonate according to the mass ratio of 5: 2.5.
The mixture is formed by mixing calcium nitrate and diammonium phosphate according to the mass ratio of 1: 2.
The surfactant is any one of sodium dodecyl benzene sulfonate and sodium dodecyl sulfate.
The trace substance is prepared by uniformly mixing vitamin D and lecithin according to the mass ratio of 15: 1.
The cross-linking agent is any one of genipin and glutaraldehyde.
A method for preparing an injectable bone repair material, the method comprising the steps of:
(1) soaking the mixed bone powder in 1.3mol/L hydrochloric acid solution for 6h, ultrasonically shaking for 30min, filtering, washing with water to neutrality, drying, and collecting the dried product;
(2) putting the dried substance into a drying oven, heating to 750 ℃ at the speed of 5 ℃/min, carrying out heat preservation and drying for 8h, cooling to room temperature, collecting the dried substance, and taking 140 parts of water, 75 parts of the dried substance, 23 parts of the mixture and 7 parts of surfactant according to parts by weight;
(3) firstly, putting water, a dried substance and a mixture into a reactor, adjusting the pH value to 10.5, heating to 55 ℃, stirring for 4h at 500r/min, adding a surfactant, continuously stirring for 3h, standing for 12h, filtering, washing, calcining for 2h at 600 ℃, and collecting a calcined substance;
(4) uniformly stirring the calcined substance, the liquid paraffin and the trace substance according to the mass ratio of 8:18:3, adding Arabic gum with the mass 2 times that of the calcined substance, adjusting the pH to 4, stirring for 7 hours at 500r/min, adding water with the volume 3 times that of the liquid paraffin for dilution, cooling to 5 ℃, adding a cross-linking agent with the mass 6% that of the calcined substance, standing for 9 hours, and performing spray drying to obtain the injectable bone repair material.
The injectable bone repair materials in the embodiments 1-3 and the comparative examples 1-2 are respectively mixed with distilled water or normal saline according to a solid-to-liquid ratio of 1: 1.5-2.5, injected and cured for 30-40 min, and detected according to the traditional detection standard, wherein the detection is as follows:
| compressive strength/MPa | Porosity/% | Pore size/. mu.m | |
| Example 1 | 38.6 | 40 | 90 |
| Example 1 | 43.5 | 45 | 108 |
| Example 1 | 39.6 | 43 | 98 |
| Comparative example 1 | 31.8 | 36 | 20 |
| Comparative example 2 | 34.8 | 32 | 5 |
In conclusion, the injectable bone repair material prepared by the invention has better performance and is worthy of popularization.
Claims (7)
1. A method for preparing an injectable bone repair material, the method comprising the steps of:
(1) soaking the mixed bone powder in a hydrochloric acid solution, ultrasonically vibrating, filtering, washing, drying, collecting a dried substance, uniformly mixing the dried substance, an additive and an ethanol solvent according to a mass ratio of 10: 1-3: 12, maintaining the pressure for 3min at 5-8 MPa, performing steam explosion, filtering, and collecting a filter cake;
(2) putting the filter cake into an oven, heating to 700-800 ℃ at a speed of 5 ℃/min, carrying out heat preservation drying, cooling, collecting the dried substance, and taking 130-150 parts of water, 70-80 parts of the dried substance, 20-25 parts of the mixture and 5-8 parts of a surfactant according to parts by weight;
(3) firstly, putting water, a dried substance and a mixture into a reactor, adjusting the pH value to 10-11, heating, stirring, adding a surfactant, continuously stirring, standing, filtering, washing, calcining, and collecting a calcined substance;
(4) uniformly stirring the calcined substance, the liquid paraffin and the trace substance according to the mass ratio of 6-10: 18:3, adding 1-3 times of Arabic gum by mass of the calcined substance, adjusting the pH to 4, stirring at 500r/min, adding water for diluting, cooling, adding a cross-linking agent accounting for 5-7% of the calcined substance, standing, and spray-drying to obtain the injectable bone repair material.
2. The preparation method of the injectable bone repair material according to claim 1, wherein the mixed bone powder in the step (1) is prepared by crushing pig bones and cow bones in a mass ratio of 12: 4-7, sieving, and collecting sieved particles to obtain the mixed bone powder.
3. The preparation method of the injectable bone repair material according to claim 1, wherein the additive in the step (1) is prepared by uniformly mixing urea and sodium bicarbonate according to a mass ratio of 5: 2-3.
4. The preparation method of the injectable bone repair material according to claim 1, wherein the mixed material is prepared by mixing calcium nitrate and diammonium phosphate according to a mass ratio of 1: 1.5-2.5.
5. The method for preparing an injectable bone repair material according to claim 1, wherein the surfactant is any one of sodium dodecylbenzenesulfonate and sodium dodecylsulfate.
6. The method for preparing an injectable bone repair material according to claim 1, wherein the trace substance in the step (4) is vitamin D and lecithin which are uniformly mixed according to a mass ratio of 15:1 to obtain the trace substance.
7. The method for preparing an injectable bone repair material according to claim 1, wherein the cross-linking agent in the step (4) is any one of genipin and glutaraldehyde.
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