CN105148320A - Preparing method and application of medicine carrying hydroxyapatite porous microspheres - Google Patents
Preparing method and application of medicine carrying hydroxyapatite porous microspheres Download PDFInfo
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- CN105148320A CN105148320A CN201510625608.8A CN201510625608A CN105148320A CN 105148320 A CN105148320 A CN 105148320A CN 201510625608 A CN201510625608 A CN 201510625608A CN 105148320 A CN105148320 A CN 105148320A
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Abstract
The invention discloses a preparing method of medicine carrying hydroxyapatite porous microspheres. The preparing method includes the steps that hydroxyapatite is added into a chitosan solution and mixed, the mixed solution is put into an injector, voltage is loaded on a syringe needle of the injector, the mixed solution is injected into curing liquid to obtain chitosan/hydroxyapatite microspheres, the chitosan/hydroxyapatite microspheres stand and are filtered, washed and dried to obtain chitosan/hydroxyapatite composite microspheres, the chitosan/hydroxyapatite composite microspheres are heated to 600 DEG C with the temperature rising speed of 2-5 DEG C/min, kept at the temperature for 1-2 h and cooled, and hydroxyapatite porous microspheres are soaked in a chemical solution for 12-24 h, then filtered, frozen with liquid nitrogen and freeze-dried for 24-48 h to obtain the medicine carrying hydroxyapatite porous microspheres. According to the preparing method, no organic solvent or micromolecular toxic substances are added in the production process, the raw materials are easy to obtain, the technology is simple, the production cycle is short, and the problem that the preparing technology of the hydroxyapatite microspheres is complex is solved.
Description
Technical field
The present invention relates to a kind of preparation method and application thereof of medicine carrying hydroxyapatite porous microsphere, belong to biology medical material technical field.
Background technology
Hydroxyapatite (hydroxyapatite, HA) be the main inorganic composition of human body hard tissue, there is good biocompatibility, be widely used in reparation and the replacement of biological hard tissue clinically, as the filling of Cranial defect, ear ossiculum are replaced and vertebrae replacement etc.In addition, HA has good chemical stability and extremely strong absorbability, with many medicines or albumen all Fails To Responds, therefore at catalyst carrier, bio-separation medium, especially also receives in fields such as slow releasing carrier of medication and pays close attention to widely.Natural hydroxyapatite is present in the sclerous tissues such as skeleton, tooth of human body and animal with needle form, and the hydroxyapatite shape of synthetic has bar-shaped, needle-like, lamellar and spherical etc.Irregular needle-like and lamellar morphology exist that fragility is high, poor mechanical property, easily in human body, introduce the shortcomings such as inflammation, and particle diameter be the spherical nanometer hydroxyapatite microsphere of 50nm-2mm for the form such as needle-like and lamellar, the easy advantage such as absorption in good, the regeneration object of shape, affinity with good mobility, rule.
There are some researches show: the interior porosity that hydroxyapatite micro-sphere is higher and hollow structure are conducive to increasing the specific surface area of material, thus obtain higher drug loading, therefore, have loose structure HA microsphere be considered to a kind of desirable pharmaceutical carrier.At present, the preparation method of hydroxyapatite micro-sphere has hydro-thermal method, nebulization, sol-gal process, template, microemulsion method etc., but, utilize these methods to prepare porous hydroxyapatite microsphere comparatively to bother, as microemulsion method, in last handling process, oil phase is difficult to clean up completely, easy formation remains, affect the quality of porous microsphere, template synthesis technique is comparatively loaded down with trivial details, is unfavorable for large-scale production.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of medicine carrying hydroxyapatite porous microsphere.Do not add any organic solvent and micromolecule noxious substance in this preparation method production process, raw material is easy to get, and technique is simple, and the production cycle is shorter, solves hydroxyapatite micro-sphere in the comparatively complicated problem of preparation technology.
For solving the problems of the technologies described above, the present invention by the following technical solutions:
A preparation method for medicine carrying hydroxyapatite porous microsphere, step is as follows:
(1) hydroxyapatite is joined in chitosan solution stir 2-4h, then the mixed liquor of chitosan and hydroxyapatite is loaded in syringe, and on the syringe needle of syringe on-load voltage, be expelled in consolidation liquid with the speed of 20-60mL/h and obtain chitosan/hydroxyapatite microsphere, chitosan/hydroxyapatite porous microsphere is left standstill 4-6h in consolidation liquid, filter, wash, after drying, obtain chitosan/hydroxyapatite complex microsphere;
(2) chitosan/hydroxyapatite complex microsphere is put into high temperature sintering furnace, be warming up to 600 DEG C with the heating rate of 2-5 DEG C/min, insulation 1-2h, is placed on natural cooling in stove and obtains hydroxyapatite porous microsphere;
(3) be dipped in medicinal liquid by hydroxyapatite porous microsphere, soak time is 12-24h, is filtered by the hydroxyapatite porous microsphere soaking medicinal liquid, then uses liquid nitrogen freezing, and lyophilization 24-48h, obtain medicine carrying hydroxyapatite porous microsphere.
In described step (1), the concentration of chitosan is 0.1mol/L-0.3mol/L.
In described step (1), the mass ratio of chitosan and hydroxyapatite is 1:2-1:5.
The voltage loaded in described step (1) is 5-15kV.
Consolidation liquid concentration used in described step (1) is 0.1mol/L-1mol/L, and wherein consolidation liquid is NaOH solution, NaHCO
3wherein one in solution, KOH or ammonia.
The concentration of the medicinal liquid in described step (3) is 10-100mg/mL.
Dry powder drug in described step (3) medicinal liquid and the mass ratio of hydroxyapatite porous microsphere are 0.5-2:100.
Dry powder drug in described step (3) medicinal liquid is wherein a kind of in the antibacterial or anti-inflammatory drug such as vancomycin, azithromycin, ciprofloxacin, amoxicillin.
Application in the prevention and therapy of the infection of the medicine carrying hydroxyapatite porous microsphere obtained according to the preparation method of above-mentioned medicine carrying hydroxyapatite porous microsphere in the reparation and bone defect healing process of Cranial defect.
The present invention utilizes electrostatic drop generation first to prepare CS(chitosan)/HA(hydroxyapatite) (wherein CS is putative natural macromolecular material to microsphere, there is good biocompatibility, be widely used in bioengineered tissue), can by regulating CS(chitosan) with HA(hydroxyapatite) ratio, the height of voltage, the size of speed etc. is advanced to regulate the diameter of microsphere, then the method for sintering is utilized to prepare hydroxyapatite porous microsphere, the drug loading of porous microsphere can also be regulated simultaneously, the medicine carrying hydroxyapatite porous microsphere that profit is prepared in this way can meet different indications, the prevention and therapy field of infecting in the reparation of Cranial defect and bone defect healing process can be applied in widely.
Beneficial effect of the present invention: 1, do not add any harmful organic solvent and micromolecule noxious substance in preparation method production process of the present invention, post processing is simple, and without any residual, the biocompatibility of material is good.2, raw material is easy to get, and technique is simple, and the production cycle is shorter, and preparation condition is gentle, substantially reduces the response time, improves preparation efficiency, solves hydroxyapatite micro-sphere in the comparatively complicated problem of preparation technology.The size of the hydroxyapatite 3, utilizing method of the present invention to prepare and porosity can regulate accordingly according to the applicable cases of reality, thus have widened its range of application.4, the process of medicine carrying have employed cryodesiccated mode, effectively remains the activity of medicine, and application prospect is comparatively wide.5, the medicine carrying hydroxyapatite porous microsphere that prepared by the present invention solves medicine in process of clinical application, discharges too fast problem, improves the utilization rate of medicine.
Accompanying drawing explanation
Fig. 1 is the chitosan/hydroxyapatite complex microsphere structure chart before sintering that the embodiment of the present invention 1 prepares.
Fig. 2 is the SEM figure of the overall pattern of hydroxyapatite micro-sphere that the embodiment of the present invention 1 prepares.
Fig. 3 is the SEM figure of surface topography of HA porous microsphere that hydroxyapatite micro-sphere amplification that the embodiment of the present invention 1 prepares is respectively 150 × and 500 × time.
Fig. 4 is the XRD spectra of the hydroxyapatite micro-sphere that the embodiment of the present invention 1 prepares.
Detailed description of the invention
Embodiment 1
The preparation method of the medicine carrying hydroxyapatite porous microsphere of the present embodiment, step is as follows:
(1) compound concentration is the chitosan solution of 0.1mol/L, then hydroxyapatite is joined in chitosan solution with the ratio of m (CS): m (HA)=1:2, stir 2h, then the mixed liquor of chitosan and hydroxyapatite is loaded in syringe, and on the syringe needle of syringe, load the high pressure of 5kV, then mixed liquor is expelled to the speed of 20ml/h in the NaOH solution of 0.1mol/L and namely obtains chitosan/hydroxyapatite complex microsphere, then obtained complex microsphere is left standstill 4h, it is made fully to solidify, then microsphere is filtered, with distilled water wash, and namely natural drying obtains chitosan/hydroxyapatite complex microsphere,
(2) chitosan/hydroxyapatite complex microsphere obtained above is put into high temperature sintering furnace, be warming up to 600 DEG C with the heating rate of 2 DEG C/min, insulation 1h, is placed on natural cooling in stove and namely obtains hydroxyapatite porous microsphere;
(3) compound concentration is the aqueous solution of the vancomycin of 10mg/ml, by hydroxyapatite porous microsphere obtained above so that m (vancomycin): m (HA porous microsphere)=1:200 ratio is dipped in medicinal liquid, soak time is 12h, the hydroxyapatite porous microsphere soaking medicinal liquid is filtered, then liquid nitrogen freezing is used, and lyophilization 24h.
Fig. 4 is the XRD spectra of the hydroxyapatite micro-sphere that the embodiment of the present invention 1 prepares, as can be seen from Figure 4, the diffraction maximum of hydroxyapatite porous microsphere is consistent with the position of the diffraction peak-to-peak of standard spectrogram, illustrate that hydroxyapatite porous microsphere its crystal formation in the process of preparation does not change, also do not change its distinctive performance.
Embodiment 2
The preparation method of the medicine carrying hydroxyapatite porous microsphere of the present embodiment, step is as follows:
(1) compound concentration is the chitosan solution of 0.2mol/L, then hydroxyapatite is joined in chitosan solution with the ratio of m (CS): m (HA)=1:3, stir 3h, then the mixed liquor of chitosan and hydroxyapatite is loaded in syringe, and on the syringe needle of syringe, load the high pressure of 10kV, then mixed liquor is expelled to the speed of 40ml/h in the NaOH solution of 0.5mol/L and namely obtains chitosan/hydroxyapatite complex microsphere, then by obtained complex microsphere at standing 6h, it is made fully to solidify, then microsphere is filtered, with distilled water wash, and namely natural drying obtains chitosan/hydroxyapatite complex microsphere,
(2) chitosan/hydroxyapatite complex microsphere obtained above is put into high temperature sintering furnace, be warming up to 600 DEG C with the heating rate of 3 DEG C/min, insulation 1.5h, is placed on natural cooling in stove and namely obtains hydroxyapatite porous microsphere;
(3) compound concentration is the aqueous solution of the vancomycin of 50mg/ml, by hydroxyapatite porous microsphere obtained above so that m (vancomycin): m (HA porous microsphere)=1:100 ratio is dipped in medicinal liquid, soak time is 12h, the hydroxyapatite porous microsphere soaking medicinal liquid is filtered, then liquid nitrogen freezing is used, and lyophilization 24h.
Embodiment 3
The preparation method of the medicine carrying hydroxyapatite porous microsphere of the present embodiment, step is as follows:
(1) compound concentration is the chitosan solution of 0.3mol/L, then hydroxyapatite is joined in chitosan solution with the ratio of m (CS): m (HA)=1:5, stir 4h, then the mixed liquor of chitosan and hydroxyapatite is loaded in syringe, and on the syringe needle of syringe, load the high pressure of 10kV, then mixed liquor is expelled to the speed of 40ml/h in the NaOH solution of 1mol/L and namely obtains chitosan/hydroxyapatite complex microsphere, then obtained complex microsphere is left standstill 6h in consolidation liquid, it is made fully to solidify, then microsphere is filtered, with distilled water wash, and namely natural drying obtains chitosan/hydroxyapatite complex microsphere,
(2) chitosan/hydroxyapatite complex microsphere obtained above is put into high temperature sintering furnace, be warming up to 600 DEG C with the heating rate of 3 DEG C/min, insulation 1.5h, is placed on natural cooling in stove and namely obtains hydroxyapatite porous microsphere;
(3) compound concentration is the aqueous solution of the vancomycin of 100mg/ml, by hydroxyapatite porous microsphere obtained above so that m (vancomycin): m (HA porous microsphere)=1:100 ratio is dipped in medicinal liquid, soak time is 12h, the hydroxyapatite porous microsphere soaking medicinal liquid is filtered, then liquid nitrogen freezing is used, and lyophilization 24h.
Embodiment 4
The preparation method of the medicine carrying hydroxyapatite porous microsphere of the present embodiment, step is as follows:
(1) compound concentration is the chitosan solution of 0.3mol/L, then hydroxyapatite is joined in chitosan solution with the ratio of m (CS): m (HA)=1:3, stir 4h, then the mixed liquor of chitosan and hydroxyapatite is loaded in syringe, and on the syringe needle of syringe, load the high pressure of 15kV, then mixed liquor is expelled to the NaHCO of 0.1mol/L with the speed of 20ml/h
3namely obtain chitosan/hydroxyapatite complex microsphere in solution, then obtained complex microsphere is left standstill 6h in consolidation liquid, make it fully solidify, then filtered by microsphere, with distilled water wash, and namely natural drying obtains chitosan/hydroxyapatite complex microsphere;
(2) chitosan/hydroxyapatite complex microsphere obtained above is put into high temperature sintering furnace, be warming up to 600 DEG C with the heating rate of 5 DEG C/min, insulation 2h, is placed on natural cooling in stove and namely obtains hydroxyapatite porous microsphere;
(3) compound concentration is the aqueous solution of 10mg/ml azithromycin, by hydroxyapatite porous microsphere obtained above so that m (azithromycin): m (HA porous microsphere)=1:50 ratio is dipped in medicinal liquid, soak time is 24h, the hydroxyapatite porous microsphere soaking medicinal liquid is filtered, then liquid nitrogen freezing is used, and lyophilization 48h.
Embodiment 5
The preparation method of the medicine carrying hydroxyapatite porous microsphere of the present embodiment, step is as follows:
(1) compound concentration is the chitosan solution of 0.2mol/L, then hydroxyapatite is joined in chitosan solution with the ratio of m (CS): m (HA)=1:2, stir 4h, then the mixed liquor of chitosan and hydroxyapatite is loaded in syringe, and on the syringe needle of syringe, load the high pressure of 5kV, then mixed liquor is expelled to the speed of 40ml/h in the KOH solution of 0.5mol/L and namely obtains chitosan/hydroxyapatite complex microsphere, then obtained complex microsphere is left standstill 6h in consolidation liquid, it is made fully to solidify, then microsphere is filtered, with distilled water wash, and namely natural drying obtains chitosan/hydroxyapatite complex microsphere,
(2) chitosan/hydroxyapatite complex microsphere obtained above is put into high temperature sintering furnace, be warming up to 600 DEG C with the heating rate of 3 DEG C/min, insulation 2h, is placed on natural cooling in stove and namely obtains hydroxyapatite porous microsphere;
(3) compound concentration is the aqueous solution of 50mg/ml ciprofloxacin, by hydroxyapatite porous microsphere obtained above so that m (ciprofloxacin): m (HA porous microsphere)=1:50 ratio is dipped in medicinal liquid, soak time is 24h, the hydroxyapatite porous microsphere soaking medicinal liquid is filtered, then liquid nitrogen freezing is used, and lyophilization 24h.
Embodiment 6
The preparation method of the medicine carrying hydroxyapatite porous microsphere of the present embodiment, step is as follows:
(1) compound concentration is the chitosan solution of 0.2mol/L, then hydroxyapatite is joined in chitosan solution with the ratio of m (CS): m (HA)=1:2, stir 4h, then the mixed liquor of chitosan and hydroxyapatite is loaded in syringe, and on the syringe needle of syringe, load the high pressure of 5kV, then mixed liquor is expelled to the speed of 40ml/h in the ammonia spirit of 1mol/L and namely obtains chitosan/hydroxyapatite complex microsphere, then obtained complex microsphere is left standstill 6h in consolidation liquid, it is made fully to solidify, then microsphere is filtered, with distilled water wash, and namely natural drying obtains chitosan/hydroxyapatite complex microsphere,
(2) chitosan/hydroxyapatite complex microsphere obtained above is put into high temperature sintering furnace, be warming up to 600 DEG C with the heating rate of 3 DEG C/min, insulation 2h, is placed on natural cooling in stove and namely obtains hydroxyapatite porous microsphere;
(3) compound concentration is the aqueous solution of 50mg/ml amoxicillin, by hydroxyapatite porous microsphere obtained above so that m (amoxicillin): m (HA porous microsphere)=1:50 ratio is dipped in medicinal liquid, soak time is 24h, the hydroxyapatite porous microsphere soaking medicinal liquid is filtered, then liquid nitrogen freezing is used, and lyophilization 24h.
Claims (9)
1. a preparation method for medicine carrying hydroxyapatite porous microsphere, is characterized in that step is as follows:
(1) hydroxyapatite is joined in chitosan solution stir 2-4h, then the mixed liquor of chitosan and hydroxyapatite is loaded in syringe, and on the syringe needle of syringe on-load voltage, be expelled in consolidation liquid with the speed of 20-60mL/h and obtain chitosan/hydroxyapatite microsphere, chitosan/hydroxyapatite porous microsphere is left standstill 4-6h in consolidation liquid, filter, wash, after drying, obtain chitosan/hydroxyapatite complex microsphere;
(2) chitosan/hydroxyapatite complex microsphere is put into high temperature sintering furnace, be warming up to 600 DEG C with the heating rate of 2-5 DEG C/min, insulation 1-2h, is placed on natural cooling in stove and obtains hydroxyapatite porous microsphere;
(3) be dipped in medicinal liquid by hydroxyapatite porous microsphere, soak time is 12-24h, is filtered by the hydroxyapatite porous microsphere soaking medicinal liquid, then uses liquid nitrogen freezing, and lyophilization 24-48h, obtain medicine carrying hydroxyapatite porous microsphere.
2. the preparation method of medicine carrying hydroxyapatite porous microsphere according to claim 1, is characterized in that: in described step (1), the concentration of chitosan is 0.1mol/L-0.3mol/L.
3. the preparation method of medicine carrying hydroxyapatite porous microsphere according to claim 1, is characterized in that: in described step (1), the mass ratio of chitosan and hydroxyapatite is 1:2-1:5.
4. the preparation method of medicine carrying hydroxyapatite porous microsphere according to claim 1, is characterized in that: the voltage loaded in described step (1) is 5-15kV.
5. the preparation method of medicine carrying hydroxyapatite porous microsphere according to claim 1, it is characterized in that: consolidation liquid concentration used in described step (1) is 0.1mol/L-1mol/L, wherein consolidation liquid is NaOH solution, NaHCO
3wherein one in solution, KOH or ammonia.
6. the preparation method of medicine carrying hydroxyapatite porous microsphere according to claim 1, is characterized in that: the concentration of the medicinal liquid in described step (3) is 10-100mg/mL.
7. the preparation method of medicine carrying hydroxyapatite porous microsphere according to claim 1, is characterized in that: the dry powder drug in described step (3) medicinal liquid and the mass ratio of hydroxyapatite porous microsphere are 0.5-2:100.
8. the preparation method of medicine carrying hydroxyapatite porous microsphere according to claim 1, is characterized in that: the dry powder drug in described step (3) medicinal liquid is the wherein one in vancomycin, azithromycin, ciprofloxacin or amoxicillin.
9. the application in the prevention and therapy of the infection of medicine carrying hydroxyapatite porous microsphere in the reparation and bone defect healing process of Cranial defect utilizing the preparation method of the arbitrary described medicine carrying hydroxyapatite porous microsphere of claim 1 ~ 8 to obtain.
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Cited By (3)
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| CN109106986A (en) * | 2018-09-14 | 2019-01-01 | 广州润虹医药科技股份有限公司 | A kind of medicine controlled releasing calcium phosphate bone cement complex microsphere, preparation method and application |
| CN109549928A (en) * | 2017-09-26 | 2019-04-02 | 清华大学深圳研究生院 | A kind of compound microballoon of Chitosan-Thiolated Polymers/calcium carbonate and preparation method thereof |
| CN115920830A (en) * | 2022-12-19 | 2023-04-07 | 江苏海普功能材料有限公司 | Suspension polymerization calcium hydroxy phosphate defluorination adsorbent and preparation method and application thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109549928A (en) * | 2017-09-26 | 2019-04-02 | 清华大学深圳研究生院 | A kind of compound microballoon of Chitosan-Thiolated Polymers/calcium carbonate and preparation method thereof |
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| CN109106986B (en) * | 2018-09-14 | 2020-12-25 | 广州润虹医药科技股份有限公司 | Medicine controlled-release calcium phosphate bone cement composite microsphere, preparation method and application thereof |
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