CN114053478A - Preparation method of traditional Chinese medicine-loaded conductive hydrogel/titanium alloy composite stent - Google Patents
Preparation method of traditional Chinese medicine-loaded conductive hydrogel/titanium alloy composite stent Download PDFInfo
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- CN114053478A CN114053478A CN202111105131.2A CN202111105131A CN114053478A CN 114053478 A CN114053478 A CN 114053478A CN 202111105131 A CN202111105131 A CN 202111105131A CN 114053478 A CN114053478 A CN 114053478A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 30
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- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention provides a preparation method of a traditional Chinese medicine loaded conductive hydrogel/titanium alloy composite bracket, which comprises the following steps: s1), dissolving the pyrrole monomer in isopropanol, and storing at low temperature after uniform dissolution; s2), weighing an oxidant, dissolving the oxidant in deionized water, stirring and dissolving, adding traditional Chinese medicine molecules, and storing at low temperature after complete dissolution; s3), adding the solvent A into the template, putting the titanium bracket into the template, then adding the solvent B, uniformly mixing the two solvents, and standing. The invention takes the conductive polypyrrole as a main body, takes traditional Chinese medicine molecules as a doping agent, and compounds the conductive polypyrrole into hydrogel on a titanium alloy network to construct a biological scaffold material with pharmacological action, excellent mechanical strength and biocompatibility.
Description
Technical Field
The invention relates to the technical field of biomedical stent materials, in particular to a preparation method of a conductive hydrogel/titanium alloy composite stent loaded with traditional Chinese medicines.
Background
Bone defects caused by degenerative diseases, nosocomial and nosocomial infections, congenital and acquired deformities, benign and malignant tumors, wounds and the like are very common. Although titanium (Ti) alloy implants can repair bone defects at weight bearing sites, they are mechanically incompatible with natural bone and lack custom-made adaptability to irregular large weight bearing bone defects, resulting in implant fixation failure. (ACS Appl. Mater. interfaces 2018,10,49, 42146-. The tissue engineering technology is used in repairing bone defect, and the tissue engineering technology is one ideal treating method, including planting autogenous osteoblast, mesenchymal stem cell, etc. onto one biological rack, implanting the rack into bone defect, and integrating the cell with the peripheral tissue to repair bone tissue defect.
Tissue engineering consists of three elements, namely seed cells, growth factors and scaffold materials. The selection of the scaffold carrying the growth factors is a core problem to be solved. The stent material must have good biocompatibility, certain mechanical properties, proper porosity and the like.
Patent CN104368040A discloses a 3D printing porous metal bracket of a composite decalcified bone matrix and a preparation method thereof, wherein the 3D printing porous metal bracket of the composite decalcified bone matrix consists of a porous titanium alloy bracket and a three-dimensional micro-bracket which is positioned in the porous titanium alloy bracket and consists of the decalcified bone matrix.
Patent CN101229394B discloses a titanium alloy-collagen-hydroxyapatite bone repair material and a preparation method thereof, comprising the following steps:
1) according to certain morphological requirements, a titanium mesh bracket with certain morphology and pores is made of titanium alloy through a rapid forming process;
2) swelling collagen in 0.3% malonic acid solution to prepare a collagen swelling solution with a solid content of 0.5-1%;
3) weighing collagen swelling liquid and hydroxyapatite powder according to the weight ratio of 1: 1-5, adding the hydroxyapatite powder into the collagen swelling liquid, and uniformly dispersing the hydroxyapatite powder in the collagen solution by stirring at the stirring speed of 100-500 rpm for 5-10 minutes to obtain hydroxyapatite-collagen dispersion liquid;
4) immersing the titanium mesh support in hydroxyapatite-collagen dispersion liquid, and adjusting the pH value to be 7-10 to separate out collagen and hydroxyapatite on the surface of the titanium mesh support;
5) then placing the titanium mesh support at-20 ℃ to-60 ℃ for pre-freezing for 4 hours, and freeze-drying for 24 hours;
6) adding 0.25% glutaraldehyde crosslinking solution, crosslinking for 2 hours at room temperature, and then putting the crosslinked material into double distilled water for repeatedly cleaning for ten times so as to remove residual glutaraldehyde in the titanium mesh support;
7) pre-freezing the cleaned stent for 4 hours at the temperature of between 20 ℃ below zero and 60 ℃ below zero, and freeze-drying for 24 hours;
8) respectively filling the titanium alloy-collagen-hydroxyapatite bone repair material obtained in the step 7) into double-layer polyethylene film small bags, sealing the bags, and performing gamma-ray radiation sterilization with the irradiation intensity of 50-250 kaladar for 24-48 hours to obtain the titanium alloy-collagen-hydroxyapatite bone repair material with the pore diameter of 1-10 mm and the pore diameter of 50-300 mu m in the collagen-hydroxyapatite composite covered on the surface of the titanium mesh scaffold; in every 100mg of the titanium alloy-collagen-hydroxyapatite bone repair material, the weight of the collagen is 10mg, the weight of the hydroxyapatite is 10 mg-30 mg, and the weight of the titanium alloy is 80 mg-60 mg.
However, the above materials are slow to meet the requirements, and therefore, there is a need to research and search for an ideal bone scaffold material.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation method of a traditional Chinese medicine-loaded conductive hydrogel/titanium alloy composite scaffold.
The technical scheme of the invention is as follows: a preparation method of a traditional Chinese medicine loaded conductive hydrogel/titanium alloy composite scaffold is characterized in that conductive polypyrrole is used as a main body, traditional Chinese medicine molecules are used as a dopant, and the conductive polypyrrole and the traditional Chinese medicine molecules are compounded on a titanium alloy network to form hydrogel, so that a bone repair scaffold material with good biocompatibility and good osseointegration characteristics is constructed, and the preparation method specifically comprises the following steps:
s1), preparation of solvent A: dissolving pyrrole monomer in isopropanol, and storing at low temperature after dissolving uniformly;
s2), preparation of solvent B: weighing oxidant, dissolving in deionized water, stirring for dissolving, adding Chinese medicinal molecules, dissolving completely, and storing at low temperature;
s3), preparation of the composite scaffold: adding a solvent A into the template, putting the titanium bracket into the template, then adding a solvent B, uniformly mixing the two solvents, and standing;
the whole process needs to be carried out at low temperature, the template is taken out after gelling, and the template is soaked in deionized water to remove redundant reactants, so that the composite bracket is obtained.
Preferably, in step S1), the concentration of pyrrole monomer in the solution is in the range of 1mol/L to 2 mol/L.
Preferably, in step S2), the oxidizing agent is one or both of ammonium persulfate and iron oxide.
Preferably, in step S2), the Chinese medicinal molecules are one or more of baicalin, curcumin and ginsenoside.
Preferably, the molar ratio of the oxidant to the pyrrole is 1: 2-2: 1.
Preferably, the molar ratio of the traditional Chinese medicine molecules to the pyrrole is 1: 10-1: 25.
Preferably, in step S2), the oxidizing agent is ammonium persulfate, and the molar ratio of the ammonium persulfate to the pyrrole is 1:2 to 2: 1.
Preferably, the conductive hydrogel/titanium alloy composite scaffold is used for filling and repairing bone defects.
The invention has the beneficial effects that:
1. the invention uses the conductive polypyrrole hydrogel as the filler of the titanium alloy stent mesh, loads the traditional Chinese medicine molecules with bioactivity, and prepares the conductive hydrogel/titanium alloy stent loaded with the traditional Chinese medicine molecules, so that the conductive hydrogel/titanium alloy stent has good biocompatibility and osseointegration characteristics;
2. according to the invention, traditional Chinese medicine molecules are used as a doping agent to be synthesized into hydrogel with conductive polypyrrole, and the hydrogel is coated and embedded into a titanium alloy network, so that the scaffold has multiple pharmacological effects, and the bone repair scaffold with good biocompatibility and good osseointegration characteristics is constructed;
3. the conductive polypyrrole is adopted to modify the surface of the titanium alloy, has excellent electrochemical activity, can promote cell proliferation and adhesion, promote osteogenic differentiation, endow the implant with good osseointegration characteristics, and improve the biocompatibility of the implant while maintaining the excellent mechanical property of the titanium alloy;
4. according to the invention, the effects of bacteriostasis, anti-inflammation, hemostasis, osteogenesis promotion and the like of the traditional Chinese medicine molecules are utilized, so that the implant is better combined with surrounding tissues after being implanted into a human body, and adverse reactions such as inflammatory reaction, hemorrhagic reaction and the like are reduced;
5. the invention has simple preparation process and lower cost, can be prepared in large scale and is an ideal bone repair implantation bracket.
Drawings
FIG. 1 is a flow chart of a method for preparing a conductive traditional Chinese medicine titanium alloy composite stent of the invention;
FIG. 2 is a graph of 25 samples prepared by controlling the formulation of raw materials in an example of the present invention;
FIG. 3 is a diagram showing an example of sample No. 3 according to the embodiment of the present invention;
FIG. 4 is a surface topography of the electrically conductive polypyrrole hydrogel of sample No. 3 in the example of the present invention
FIG. 5 is a skeletal diagram of rat stem cells on the surface of a hydrogel composite scaffold according to an embodiment of the present invention;
Detailed Description
The following further describes embodiments of the present invention with reference to the accompanying drawings:
as shown in fig. 1, this embodiment provides a method for preparing a conductive hydrogel/titanium alloy composite stent loaded with traditional Chinese medicines, which includes the following steps:
s1), putting a large amount of ice blocks into the foam box, and carrying out the whole preparation process on the ice blocks to maintain a low-temperature environment;
s2), preparation of solvent A: transferring 85 μ L pyrrole monomer and Chinese medicinal molecules (baicalin, curcumin and ginsenoside are used herein respectively) into 1ml isopropanol, magnetically stirring, and cooling in ice block;
s3), preparation of solvent B: weighing ammonium persulfate powder, dissolving in 2ml of deionized water, adding traditional Chinese medicine powder, magnetically stirring to dissolve completely, and cooling in ice cubes for later use;
s4), adding 70 mu L of solvent A into a hole of a circular template, then putting the circular titanium alloy mesh (diameter is 1cm, thickness is 2mm), then quickly adding 140 mu L of solvent B, repeatedly blowing and beating by using a liquid transfer gun, standing, taking out after gelling, and soaking in deionized water to obtain the conductive traditional Chinese medicine titanium alloy composite stent. The pore size of the titanium alloy stent used herein was 400 μm.
In the embodiment, the molecular components and the dosage of the traditional Chinese medicine and the dosage of ammonium persulfate powder are regulated and controlled, and the specific formula is as follows:
the stable hydrogel titanium composite scaffold can be prepared by the formula. As shown in fig. 2, 25 samples were prepared, and the numbers at the bottom of the samples corresponded to the numbers in the table. The physical map of the sample No. 3 is shown in FIG. 3, and the sample is formed by filling hydrogel with a titanium alloy bracket serving as a framework, has certain mechanical properties and morphology stability, and can be freely clamped by tweezers. As shown in fig. 4, the surface topography of number 3 exhibited a typical hydrogel porosity with pore sizes in the range of 1-5 microns. As shown in fig. 5, after the sample of number 3 is freeze-dried, the sample is co-cultured with rat bone marrow mesenchymal stem cells for 24 hours, and the cells spread well on the surface of the material, which indicates that the composite scaffold has good cell compatibility.
Example 2
As shown in fig. 1, this embodiment provides a method for preparing a conductive hydrogel/titanium alloy composite stent loaded with traditional Chinese medicines, which includes the following steps:
s1), putting a large amount of ice blocks into the foam box, and carrying out the whole preparation process on the ice blocks to maintain a low-temperature environment;
s2), preparation of solvent A: transferring 85 μ L pyrrole monomer and Chinese medicinal molecules (baicalin, curcumin and ginsenoside are used herein respectively) into 1ml isopropanol, magnetically stirring, and cooling in ice block;
s3), preparation of solvent B: weighing ferric oxide powder, dissolving into 2ml deionized water, adding traditional Chinese medicine powder, magnetically stirring for dissolving completely, and cooling in ice block;
s4), adding 70 mu L of solvent A into a hole of a circular template, then putting the circular titanium alloy mesh (diameter is 1cm, thickness is 2mm), then quickly adding 140 mu L of solvent B, repeatedly blowing and beating by using a liquid transfer gun, standing, taking out after gelling, and soaking in deionized water to obtain the conductive traditional Chinese medicine titanium alloy composite stent.
The foregoing embodiments and description have been presented only to illustrate the principles and preferred embodiments of the invention, and various changes and modifications may be made therein without departing from the spirit and scope of the invention as hereinafter claimed.
Claims (8)
1. A preparation method of a traditional Chinese medicine loaded conductive hydrogel/titanium alloy composite scaffold is characterized in that the method takes conductive polypyrrole as a main body and traditional Chinese medicine molecules as a dopant to be compounded on a titanium alloy network to form hydrogel so as to construct a bone repair scaffold material with good biocompatibility and good osseointegration characteristics, and specifically comprises the following steps:
s1), preparation of solvent A: dissolving pyrrole monomer in isopropanol, and storing at low temperature after dissolving uniformly;
s2), preparation of solvent B: weighing oxidant, dissolving in deionized water, stirring for dissolving, adding Chinese medicinal molecules, dissolving completely, and storing at low temperature;
s3), preparation of the composite scaffold: adding a solvent A into the template, putting the titanium bracket into the template, then adding a solvent B, uniformly mixing the two solvents, and standing;
the whole process needs to be carried out at low temperature, the template is taken out after gelling, and the template is soaked in deionized water to remove redundant reactants, so that the composite bracket is obtained.
2. The preparation method of the traditional Chinese medicine-loaded conductive hydrogel/titanium alloy composite stent according to claim 1, characterized in that: in the step S1), the concentration range of the pyrrole monomer in the solution is 1 mol/L-2 mol/L.
3. The preparation method of the traditional Chinese medicine-loaded conductive hydrogel/titanium alloy composite stent according to claim 1, characterized in that: in step S2), the oxidant is one or both of ammonium persulfate and iron oxide.
4. The preparation method of the traditional Chinese medicine-loaded conductive hydrogel/titanium alloy composite stent according to claim 1, characterized in that: in the step S2), the Chinese medicinal molecules are one or more of baicalin, curcumin and ginsenoside.
5. The preparation method of the traditional Chinese medicine-loaded conductive hydrogel/titanium alloy composite stent according to claim 1, characterized in that: the molar ratio of the oxidant to the pyrrole is 1: 2-2: 1.
6. The preparation method of the traditional Chinese medicine-loaded conductive hydrogel/titanium alloy composite stent according to claim 1, characterized in that: the molar ratio of the traditional Chinese medicine molecules to the pyrrole is 1: 10-1: 25.
7. The preparation method of the traditional Chinese medicine-loaded conductive hydrogel/titanium alloy composite stent according to claim 1, characterized in that: in the step S2), the oxidant is ammonium persulfate, and the molar ratio of the ammonium persulfate to the pyrrole is 1: 2-2: 1.
8. The preparation method of the traditional Chinese medicine-loaded conductive hydrogel/titanium alloy composite stent according to claim 1, characterized in that: the conductive hydrogel/titanium alloy composite scaffold is used for filling and repairing bone defects.
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|---|---|---|---|---|
| CN101279109A (en) * | 2008-05-27 | 2008-10-08 | 厦门大学 | Artificial joint medium layer and method of preparing the same |
| CN105543924A (en) * | 2015-12-21 | 2016-05-04 | 广东工业大学 | Preparation method of titanium-based conductive hydrogel composite coating material |
| CN112353754A (en) * | 2020-10-26 | 2021-02-12 | 华南理工大学 | Conductive polypyrrole/traditional Chinese medicine composite hydrogel and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101279109A (en) * | 2008-05-27 | 2008-10-08 | 厦门大学 | Artificial joint medium layer and method of preparing the same |
| CN105543924A (en) * | 2015-12-21 | 2016-05-04 | 广东工业大学 | Preparation method of titanium-based conductive hydrogel composite coating material |
| CN112353754A (en) * | 2020-10-26 | 2021-02-12 | 华南理工大学 | Conductive polypyrrole/traditional Chinese medicine composite hydrogel and preparation method and application thereof |
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