CN111012951A - Injectable composite bone cement with photothermal effect and preparation method and application thereof - Google Patents
Injectable composite bone cement with photothermal effect and preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to injectable composite bone cement with photothermal effect, a preparation method and application thereof, wherein the bone cement comprises the following components in percentage by weight: 30-65% of bioglass powder, 5-30% of titanium nitride nano powder and 30-40% of sodium alginate mixed solution. Compared with the prior art, the bone cement has the characteristics of plasticity and easy operation, and has obvious photo-thermal effect, and the photo-thermal effect can be regulated and controlled by changing the adding amount of the titanium nitride nanoparticles; the process equipment for preparing the bone cement is simple, the operation is easy, the cost is low, no crosslinking agent is added, good injectability can be obtained, and minimally invasive treatment can be realized; can be used for preparing bone filler after resection of bone tumor, and can be applied to the fields of bone repair and regeneration in bone tissue engineering.
Description
Technical Field
The invention belongs to the technical field of biological materials, and particularly relates to injectable composite bone cement with a photothermal effect, and a preparation method and application thereof.
Background
Bone is a common metastatic site of malignant tumors. In secondary bone tumors, tumor cells release cytokines to activate osteoclasts, which results in osteolysis, thereby causing pathological fractures, hypercalcemia, pain and complications of spinal cord compression, greatly reducing the quality of life of patients and increasing the death rate of bone tumors. The current clinical method is surgical excision of focus assisted by radiotherapy and chemotherapy. The surgery treatment is easy to recur, and the radiotherapy and chemotherapy can kill normal cells. The photothermal therapy developed in recent years provides a new treatment approach for the treatment of tumors. The photothermal therapy technology is a minimally invasive therapy technology, utilizes materials with high light absorption and photothermal conversion efficiency to convert near-infrared laser light energy into heat energy, so that the local temperature of a tumor is raised to reach a certain temperature (above 42 ℃), thereby killing tumor cells, has the advantages of high speed, high efficiency, minimal invasion and small toxic and side effects, and has unique advantages in a plurality of cancer therapy methods. In addition, studies have shown that mild thermal stimulation induces differentiation of Mesenchymal Stem Cells into osteoblasts, thereby facilitating repair of defective bone tissue [ J Chen, Z D Shi, X YJi, et al. The research results show that the TiN nano-material is an ideal photothermal material photothermal preparation, has strong absorption in a near-infrared biological window I (750-.
The bone cement is a medical material used for orthopedic surgery, has the biggest characteristics of easy shaping and easy operation, is widely applied to bone injury diseases such as fracture surgery fixation, joint surgery fixation and the like, and shows better curative effect. The bone cement generally comprises solid-phase powder and liquid-phase components, which are mixed according to a certain proportion at room temperature, and then the bone cement slurry is injected into a bone defect part with a complex and irregular shape through an injector and is solidified in situ at the bone defect part. The injectability enables the bone cement to be implanted into the body in a minimally invasive manner, thereby reducing surgical trauma and pain of patients. The currently clinically used bone cements include polymethyl methacrylate (PMMA), calcium phosphate, calcium sulfate and the like, and the bone cements have single functions and only play roles in supporting, fixing and filling.
Disclosure of Invention
The present invention aims to overcome the defects of the prior art and provide an injectable composite bone cement with a photothermal effect, a preparation method and an application thereof. The composite bone cement not only has the characteristics of plasticity and easy operation, but also has obvious photo-thermal effect, and the photo-thermal effect can be regulated and controlled by changing the adding amount of the titanium nitride nano particles. The bone cement has the advantages of simple preparation process equipment, easy operation and low cost, can obtain good injectability without adding a cross-linking agent, and can realize minimally invasive treatment. The method can be used for preparing bone filler after resection of bone tumor, and can be applied to the fields of bone repair and regeneration in bone tissue engineering.
The purpose of the invention can be realized by the following technical scheme:
the invention provides an injectable composite bone cement with a photothermal effect, which comprises the following components in percentage by weight:
30-65% of biological glass powder,
5 to 30 percent of titanium nitride nano powder,
30-40% of sodium alginate mixed solution.
Preferably, the bioglass powder comprises silicate, borate or phosphate bioglass powder.
Preferably, the particle size of the bioglass powder is 50nm-40 μm.
Preferably, the particle size of the titanium nitride nano powder is 10-40 nm.
Preferably, the sodium alginate mixed solution is prepared from the following components in percentage by mass:
preferably, the injection rate of the composite bone cement is controlled under the conditions that the pressure is 0-100N and the extrusion speed is 5mm/min>70 percent, and the initial setting time is 10-40 min; the composite bone cement has a wavelength of 1064nm and a power density of 0.8W/cm2The temperature rises by 40-55 ℃ within 6min under the laser irradiation.
The second aspect of the present invention provides a method for preparing the injectable composite bone cement having a photothermal effect, comprising the steps of:
(1) uniformly mixing the bioglass powder and the titanium nitride nano powder to obtain mixed powder of the bioglass powder and the titanium nitride nano powder, namely a bone cement solid phase;
(2) preparing a sodium alginate mixed solution, namely a bone cement liquid phase;
(3) and uniformly mixing the bone cement solid phase and the bone cement liquid phase to obtain the composite bone cement.
Preferably, in step (1), the mixing is performed by grinding. Further preferably, in the step (1), the mixture is ground at room temperature for 3 to 5 min.
Preferably, in the step (2), sodium alginate, gluconolactone and disodium hydrogen phosphate are respectively added into deionized water and uniformly mixed to obtain a sodium alginate mixed solution. Further preferably, in the step (2), the mixture is mixed by magnetic stirring for 1 to 3 hours at normal temperature.
Preferably, after the composite bone cement obtained in the step (3) is hardened and solidified, a bone cement product is obtained. More preferably, the composite bone cement obtained in the step (3) is hardened and cured for 10-40min to obtain a bone cement product.
The third aspect of the invention also provides the application of the injectable composite bone cement with the photothermal effect, which is used for preparing a filling material for bone tumor surgery or/and a bone defect repairing material.
The invention provides injectable composite bone cement with photothermal effect, which can be used as a filling material after bone tumor operation, and the photothermal effect can kill cancer cells which are not removed in the operation and prevent tumor recurrence; meanwhile, the components of the bone cement cooperate with the photo-thermal effect to induce osteogenic differentiation of bone marrow mesenchymal stem cells, so that the repair of defective bone tissues is promoted, namely, the dual functions of treatment and repair are realized.
Compared with the prior art, the invention has the following beneficial effects:
1. TiN nano-particles are introduced into the bone cement, and the good photothermal effect of the TiN nano-particles is utilized to kill cancer cells which are not removed in bone tumor operation, so that tumor recurrence is prevented. The research results show that the TiN nano-material has strong absorption in the near-infrared biological window I (750-. In addition, the photothermal effect can also induce osteogenic differentiation of bone marrow mesenchymal stem cells and promote repair of defective bone tissues.
2. After being degraded, the bioglass powder in the bone cement can release active ions for promoting the growth and angiogenesis of new bone tissues, and the repair and wound healing of the bone tissues are promoted.
3. Calcium ions released in the degradation process of the bioglass powder and α -L-guluronic acid (α -L-guluronic acid) units on a molecular chain of sodium alginate are subjected to ion crosslinking reaction to form gel in situ, so that good injectability can be obtained without adding a crosslinking agent and a complex crosslinking process, minimally invasive treatment is realized, and the influence of the use of the crosslinking agent on the biological safety of the bone cement is avoided.
4. The photothermal effect of the composite bone cement can be regulated and controlled by changing the adding amount of the titanium nitride nano powder in the solid phase, the power density of near infrared light and the irradiation time, so that different clinical requirements are met.
Drawings
Fig. 1 is a scanning electron microscope image of a field emission microscope of an injectable composite bone cement solidified body having a photothermal effect prepared in example 1 of the present invention, in which large particles are bioglass powder and small particles are TiN nanoparticles, and solid phases composed of the two components are bonded together by sodium alginate.
Fig. 2 is a photograph showing that injectable composite bone cement having a photothermal effect prepared in example 1 of the present invention is extruded from a syringe, illustrating that the bone cement has good injectability.
FIG. 3 is a graph showing the wavelength of 1064nm and the power density of 0.8W/cm for injectable composite bone cements having photothermal effects prepared in examples 1 and 2 of the present invention2The temperature rise curve of irradiating for 6min under the near-infrared laser shows that the bone cement has good photothermal effect, and the photothermal property of the bone cement can be regulated and controlled by changing the adding amount of TiN.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments.
Example 1
(1) Preparing mixed powder of bioglass powder and titanium nitride nano powder (bone cement solid phase)
Preparing the following bone cement solid phases in percentage by mass: the particle size is 30-40 microns, and the silicate bioactive glass prepared by a melting method is 45S5(45SiO2-24.5Na2O-24.5CaO-6P2O5Wt%) 60% of powder material and 10% of titanium nitride nano powder material. 6g of bioglass powder and 1g of titanium nitride nano powder (the average particle size is 20nm) are placed in a mortar, and are ground and mixed for 3min at room temperature, so that the bone cement solid phase is obtained.
(2) Preparation of sodium alginate Mixed solution (bone Cement liquid phase)
Preparing the following bone cement liquid phase by mass percent: 3% of sodium alginate, 2% of gluconolactone, 3% of disodium hydrogen phosphate and 92% of deionized water. Sequentially adding 3g of sodium alginate, 2g of gluconolactone and 3g of disodium hydrogen phosphate into 92g of deionized water, magnetically stirring at room temperature for 1h to ensure that the solution is clear and transparent, and preparing a sodium alginate mixed solution, namely the bone cement liquid phase.
(3) Preparation of injectable composite bone cement (slurry) with photothermal effect:
and mixing the bone cement solid phase formed by the silicate bioglass powder and the titanium nitride nano powder with the sodium alginate mixed solution according to the mass percentage of 70 percent to 30 percent, fully grinding in a mortar for 3min at room temperature, and uniformly mixing to obtain the injectable composite bone cement (slurry) with the photothermal effect.
The initial setting time of the bone cement was determined according to ISO 9917-1.
The injectability of the composite bone cement is determined according to the following steps: (1) the bone cement prepared in example 1 was transferred to a 2ml syringe (needle diameter 1.7mm), and the mass M0 of the empty syringe and the total mass M1 of the syringe after the bone cement was added were recorded, respectively; (2) fixing the injector on an electronic universal testing machine, applying pressure at a loading rate of 5mm/min to extrude the bone cement from the injector, stopping pressurizing until the pressure value reaches 100N, and recording the mass M2 of the injector at the moment; (3) the injection rate of the bone cement was calculated according to the following formula, and each group of samples was tested 4 times, and the average value of the test results was taken as the injectable rate of the bone cement.
The injectable rate is%
Thus, the injectable rate of the composite bone cement prepared in example 1 was 98%, and the initial setting time was 10 min.
Measuring the photo-thermal property of the bone cement: placing the cured bone cement at a wavelength of 1064nm and a power density of 0.8W/cm2The temperature rise curve is shown as curve a in figure 3, the temperature of the bone cement rises from 25 ℃ to 67 ℃, and the temperature rises to 42 ℃ after the irradiation is carried out for 6 min.
Example 2
(1) Mixed powder for preparing biological glass powder and titanium nitride nano powder
Preparing the following bone cement solid phases in percentage by mass: fusion-prepared borate bioactive glass (6 Na) with particle size of 20-40 microns2O-8K2O-22CaO-8MgO-54B2O3-2P2O5Wt%) powder 50%, titanium nitride sodium20 percent of rice flour. 5g of borate bioglass powder and 2g of titanium nitride nano powder (the average particle size is 20nm) are placed in a mortar, and are ground and mixed for 5min at room temperature, so that the bone cement solid phase is obtained.
(2) Preparation of sodium alginate Mixed solution
Preparing the following bone cement liquid phase by weight percent of each component: 3% of sodium alginate, 4% of gluconolactone, 4% of disodium hydrogen phosphate and 89% of deionized water. Sequentially adding 3g of sodium alginate, 4g of gluconolactone and 4g of disodium hydrogen phosphate into 89g of deionized water, magnetically stirring at room temperature for 1h to ensure that the solution is clear and transparent, and preparing a sodium alginate mixed solution, namely the bone cement complex liquid phase.
(3) Preparation of injectable composite bone cement slurry with photothermal effect:
the solid phase formed by the borate bioglass powder and the titanium nitride nano powder and the sodium alginate mixed solution are mixed according to the mass percentage of 70 percent: mixing the components in a proportion of 30 percent, fully grinding the mixture in a mortar for 2min at room temperature, and obtaining the bone cement slurry after uniform mixing.
Thus, the injectable rate of the composite bone cement prepared in example 3 was 85%, and the initial setting time was 25 min.
Measuring the photo-thermal property of the bone cement: placing the cured bone cement at a wavelength of 1064nm and a power density of 0.8W/cm2The temperature rise curve is shown as curve b in figure 3, the temperature of the bone cement rises from 25 ℃ to 71 ℃, and the temperature rises to 46 ℃.
Example 3
(1) Mixed powder for preparing biological glass powder and titanium nitride nano powder
Preparing the following bone cement solid phases in percentage by mass: bioactive silicate glass (30CaO-70 SiO) with particle size of 50-100 nm prepared by sol-gel method2Wt%) 30% of powder material and 30% of titanium nitride nano powder material. 3g of silicate bioglass powder and 3g of titanium nitride nano powder (the average particle size is 20nm) are placed in a mortar, and are ground and mixed for 3min at room temperature, so that the solid phase of the composite bone cement is obtained.
(2) Preparation of sodium alginate Mixed solution
Preparing the following bone cement liquid phase by weight percent of each component: 4% of sodium alginate, 4% of gluconolactone, 4% of disodium hydrogen phosphate and 88% of deionized water. Sequentially adding 4g of sodium alginate, 4g of gluconolactone and 4g of disodium hydrogen phosphate into 88g of deionized water, magnetically stirring at room temperature for 1h to ensure that the solution is clear and transparent, and preparing a sodium alginate mixed solution, namely the composite bone cement liquid phase.
(3) Preparation of injectable composite bone cement slurry with photothermal effect:
mixing the solid phase formed by the borate bioglass powder and the titanium nitride nano powder with the sodium alginate mixed solution according to the mass percentage of 60 percent: mixing the components in a proportion of 40 percent, fully grinding the mixture in a mortar for 2min at room temperature, and obtaining the bone cement slurry after uniform mixing.
Thus, the injectable rate of the composite bone cement prepared in example 3 was 90%, and the initial setting time was 10 min.
Measuring the photo-thermal property of the bone cement: placing the cured bone cement at a wavelength of 1064nm and a power density of 0.8W/cm2The temperature rise curve is shown as curve c in figure 3, the temperature of the bone cement rises from 25 ℃ to 77 ℃, and the temperature rises to 52 ℃.
Comparative example
(1) Preparation of bioglass powder (bone cement solid phase)
Preparing the following bone cement solid phases in percentage by mass: fusion-prepared borate bioactive glass (6 Na) with particle size of 20-40 microns2O-8K2O-22CaO-8MgO-54B2O3-2P2O5Wt.%) powder.
(2) Preparation of sodium alginate Mixed solution (bone Cement liquid phase)
Preparing the following bone cement liquid phase by weight percent of each component: 3% of sodium alginate, 4% of gluconolactone, 4% of disodium hydrogen phosphate and 89% of deionized water. Sequentially adding 3g of sodium alginate, 4g of gluconolactone and 4g of disodium hydrogen phosphate into 89g of deionized water, magnetically stirring at room temperature for 1h to ensure that the solution is clear and transparent, and preparing a sodium alginate mixed solution, namely the bone cement complex liquid phase.
(3) Preparation of injectable composite bone cement paste
Mixing the borate bioglass powder with the sodium alginate mixed solution according to the mass percentage of 70%: mixing the components in a proportion of 30 percent, fully grinding the mixture in a mortar for 3min at room temperature, and obtaining the bone cement slurry after uniform mixing.
The injectable rate of the composite bone cement prepared by the comparative example is 88%, and the initial setting time is 15 min.
Measuring the photo-thermal property of the bone cement: placing the cured bone cement at a wavelength of 1064nm and a power density of 0.8W/cm2Irradiating for 6min under the near infrared laser, wherein the temperature rise curve is as the curve control in figure 3, the temperature of the bone cement is raised from 25 ℃ to 32 ℃, and the temperature is raised to 7 ℃.
Example 4
This example is substantially the same as example 1, except that in this example, phosphate bioglass (25 Na) was used as bioglass powder2O-25CaO-50P2O5) And (3) powder lot.
Example 5
The present example is substantially the same as example 1, except that in the present example, the mass percentage of the bioglass powder is 65%, the mass percentage of the titanium nitride nano powder is 5%, and the mass ratio of the sodium alginate mixed solution is 30%. The sodium alginate mixed solution comprises the following components in percentage by mass: 5% of sodium alginate, 3% of glucolactone, 6% of disodium hydrogen phosphate and 86% of deionized water.
Example 6
The present example is substantially the same as example 1, except that in the present example, the mass percentage of the bioglass powder is 45%, the mass percentage of the titanium nitride nano powder is 20%, and the mass ratio of the sodium alginate mixed solution is 35%. The sodium alginate mixed solution comprises the following components in percentage by mass: 3% of sodium alginate, 3% of glucolactone, 5% of disodium hydrogen phosphate and 89% of deionized water.
Example 7
This example is substantially the same as example 1, except that the titanium nitride nanopowder in this example has an average particle size of 10-20 nm.
Example 8
This example is substantially the same as example 1, except that the titanium nitride nanopowder in this example has an average particle size of 30-40 nm.
Example 9
This example is substantially the same as example 1, except that in the process of preparing the mixed powder of bioglass powder and titanium nitride nanopowder, the mixing condition was room temperature grinding and mixing for 5 minutes.
Example 10
This example is substantially the same as example 1, except that in the process of preparing the mixed powder of bioglass powder and titanium nitride nanopowder, the mixing condition was room temperature grinding and mixing for 4 minutes.
Example 11
This example is substantially the same as example 1, except that in this example, the mixing condition was magnetic stirring at room temperature for 3 hours during the preparation of the sodium alginate mixed solution.
Example 12
This example is substantially the same as example 1, except that in this example, the mixing condition was magnetic stirring at room temperature for 2 hours during the preparation of the sodium alginate mixed solution.
The embodiments described above are intended to facilitate the understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (10)
1. An injectable composite bone cement with a photothermal effect, characterized by comprising the following components in percentage by weight:
30-65% of biological glass powder,
5 to 30 percent of titanium nitride nano powder,
30-40% of sodium alginate mixed solution.
2. The injectable composite bone cement with photothermal effect according to claim 1, characterized in that said bioglass powder comprises silicate, borate or phosphate bioglass powder.
3. The injectable composite bone cement with photothermal effect according to claim 1 or 2, characterized in that the particle size of the bioglass powder is 50nm-40 μm.
4. The injectable composite bone cement with photothermal effect according to claim 1, wherein said titanium nitride nanopowder has a particle size of 10-40 nm.
6. the injectable composite bone cement with photothermal effect according to claim 1, wherein the injection rate of the composite bone cement is controlled at a pressure of 0-100N and an extrusion speed of 5mm/min>70 percent, and the initial setting time is 10-40 min; the composite bone cement has a wavelength of 1064nm and a power density of 0.8W/cm2The temperature rises by 40-55 ℃ within 6min under the laser irradiation.
7. The method for preparing injectable composite bone cement with photothermal effect according to any of claims 1 to 6, comprising the following steps:
(1) uniformly mixing the bioglass powder and the titanium nitride nano powder to obtain mixed powder of the bioglass powder and the titanium nitride nano powder, namely a bone cement solid phase;
(2) preparing a sodium alginate mixed solution, namely a bone cement liquid phase;
(3) and uniformly mixing the bone cement solid phase and the bone cement liquid phase to obtain the composite bone cement.
8. Method for the preparation of injectable composite bone cement with photothermal effect according to claim 7, characterized in that it comprises any one or more of the following conditions:
(i) in the step (1), mixing in a grinding mode;
(ii) in the step (2), adding sodium alginate, gluconolactone and disodium hydrogen phosphate into deionized water respectively, and uniformly mixing to obtain a sodium alginate mixed solution;
(iii) and (4) hardening and curing the composite bone cement obtained in the step (3) to obtain a bone cement product.
9. Method for the preparation of injectable composite bone cement with photothermal effect according to claim 8, characterized in that it comprises any one or more of the following conditions:
(i) grinding at normal temperature for 3-5min and mixing in the step (1);
(ii) in the step (2), magnetically stirring for 1-3h at normal temperature for mixing;
(iii) and (4) hardening and curing the composite bone cement obtained in the step (3) for 10-40min to obtain a bone cement product.
10. Use of the injectable composite bone cement with photothermal effect according to any of claims 1 to 6 for the preparation of a filling material for bone tumor surgery or/and a bone defect repair material.
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