CN102921010B - Magnetic mesoporous bioactive glass drug delivery system and preparation method thereof - Google Patents
Magnetic mesoporous bioactive glass drug delivery system and preparation method thereof Download PDFInfo
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- CN102921010B CN102921010B CN201210480060.9A CN201210480060A CN102921010B CN 102921010 B CN102921010 B CN 102921010B CN 201210480060 A CN201210480060 A CN 201210480060A CN 102921010 B CN102921010 B CN 102921010B
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Abstract
The invention discloses a magnetic mesoporous bioactive glass drug delivery system and a preparation method thereof, and the preparation process is carried out with a surface active agent as a soft template by a sol-gel method. The magnetic mesoporous bioactive glass drug delivery system is provided with a specific surface area of the material of 300-1000 cm<2>/g and a mesoporous diameter of 2-50 nm, and the structure of the mesoporous is adjustable. Through loading gentamicin sulphate and other antibiotics on the surface of the material and carrying out drug sustained release, the results shows that the magnetic mesoporous bioactive glass drug delivery system has good drug loading efficiency and slow release performance, and is not influenced by the types of the loaded antibiotics and the like.
Description
Technical field
The present invention relates to Inorganic Non-metallic Materials and medical material tech field, be specially a kind of preparation of magnetic mesoporous bio-vitric drug delivery system.
Background technology
Bio-vitric is as the one of Bone Defect Repari and timbering material, be successfully applied to the postoperative tissue renovation material of various clinical, wherein most important reason is that its chemical composition and skeleton are closely similar, there is superior biocompatibility and self-degradation energy, can be combined closely with bone formation after implant into body, promote Bone Defect Repari quickly and effectively, thus there is good bone formation performance.And nowadays, the Cranial defect caused for diseases such as bone tumor requires that biomaterial effectively can not only carry out Bone Defect Repari, but also the relevant diseases induced function for the treatment of should be possessed.Research and development and the important directions be expanded into as biomedicine field bone renovating material of new and effective bio-vitric, also attracted increasing research worker and be absorbed in wherein.Wherein, bio-vitric has been made and has been mixed Sr calcium phosphorus bio-vitric compound a-tricalcium phosphate biological stephanoporate bone cement by Cai Shu etc. (patent No. CN102249728A), improve the comprcssive strength of bone cement by introducing Sr, and make it to form the more much higher pore structure of porosity; Chen Chuanzhong etc. (patent No. CN101549172A) are with hydroxyapatite or bio-vitric or both mixture for target body material, and deposition has prepared the hydroxylapatite-bioglass film of a kind of no cytotoxicity, good biocompatibility; The people such as Zhang Changqing (patent No. CN102247599A) provide a kind of slow release system for borate bioglass carried with antibiotic and preparation method thereof, make its preparation manipulation easy.Also existing procucts are applied to clinical even at present.But the functional material ubiquity structure of this traditional bio-vitric base is too closely knit, contact surface limitation, with body in conjunction with insufficient and problems such as the poor biocompatibility that causes.
Along with the expansion gradually of mesoporous material research field in recent years, the impact of meso-hole structure on performance is also paid close attention to by everybody gradually, especially its high-ratio surface sum ordered mesoporous pore canals, facilitate drug loading performance and the sustained release performance of biological mesoporous material, also substantially increase its biocompatibility and fungistatic effect simultaneously.Zhu Min etc. (patent No. CN 102188749A) use freezing abstraction technique, prepare a kind of three-dimensional porous rack with mesoporous bioglass coating by infusion process.Chang Jiang etc. (patent No. CN101623513A) have invented one-step method and have prepared mesoporous bioglass material, make the preparation method of mesoporous bioglass become simple and feasible.But their invention and preparation solve the relevant diseases induced problem caused after Bone Defect Repari is transplanted completely, this makes us have to the novel functional material system of deep structure to reaching the object reducing cytotoxicity and increase biocompatibility.
Meanwhile, magnetic Nano material has also shown unique advantage and application prospect potential in the regular period at biomedicine field, the classical magnetic nanoparticle especially headed by magnetic ferroferric oxide.Not only ferroso-ferric oxide itself is nontoxic to biological cell performance, also has targeting, can adsorb a large amount of DNA at material surface, can be used as good genophore and promote that the note of material surface cell echos propagation under additional the action of a magnetic field.Between this, in order to make the actual biologic applications problem of mesoporous bioglass be resolved targetedly, the present invention has prepared the nanometer biological glass drug delivery system with magnetic mesoporous structure.That is to say, magnetic particle is used as ferromagnetic thermoseed, and meso-hole structure material is used as pharmaceutical carrier, while significantly improving Biocompatibility, imparts the function that diseased region cancerous tumor cell etc. is killed in this biomaterial selective thermal radiation.Adopt the magnetic mesoporous bio-vitric drug delivery system of the pollution-free preparation of organic formwork method, and by load antibiotic etc and the test of corresponding sustained release performance, demonstrate meso-hole structure and magnetic particle to the effect of biocompatibility, biological activity and medicament slow release performance.
Summary of the invention
The object of the present invention is to provide a kind of magnetic mesoporous bio-vitric drug delivery system and preparation method thereof, to obtain a kind of new bio glass drug delivery system with excellent biological activity, biocompatibility, drug loading and release performance.
Technical scheme of the present invention is as follows:
Take surfactant as soft template, pass through sol-gel process, a certain proportion of magnetic source and silicon source, phosphorus source, calcium source are carried out mixed catalytic hydrolysis, treat to add surfactant solution in the complete backward finely dispersed inorganic matter presoma of hydrolysis, carry out self assembly and form sol gel precursor, sintering just obtains magnetic mesoporous bio-vitric drug delivery system after removing masterplate, and concrete steps are as follows:
(1) by surfactant-dispersed in alcoholic solution, get a uniform mixture;
(2) in the ratio of setting, calcium source, silicon source, phosphorus source and magnetic nano-particle order are added to the water, use diluted acid catalyzing hydrolysis;
(3) step (1) gained mixed solution is fully mixed with step (2) gained solution, carry out soft mode version sealing self assembly, obtain collosol and gel;
(4) by collosol and gel dry and aging after, at 550-700 DEG C of temperature lower calcination 4-6h, obtain magnetic mesoporous bio-vitric drug delivery system.
Described surfactant is ionic surfactant: C
nh
2n+1n (R)
3x, n=10-20, R=CH
3, C
2h
5, X=Cl
-, Br
-, or Pluronic F-127 as hydrophilic block, long chain alkane as the nonionic surfactant of hydrophobic group, or Pluronic F-127 is as hydrophilic block, propylene oxide or the butadiene monoxide block macromolecular surfactant as hydrophobic block, and its molecular formula is EO
npO
meO
n, n=10-140, m=5-100, or molecular formula EO
nbO
meO
n, n=10-200, m=10-100, PO is propylene oxide here, and EO is oxireme, and BO is butadiene monoxide; Specifically comprise P123, F127, CTAB, P105, P104, P103, P85, P84, P75, P65, P38.
Described magnetic nano-particle comprises ferrospinel, magneto-plumbite type ferrite, garnet type ferrite, perovskite ferrite by lattice types classification, and silicon source is inorganic silicon source; Its phosphorus source is phosphoric acid ester, and its calcium source is soluble calcium salt; Preferably, magnetic nano-particle is ferrospinel Fe
3o
4, silicon source is tetraethyl orthosilicate, and phosphorus source is triethyl phosphate, and calcium source is four water-calcium nitrate or calcium chloride.
The magnetic mesoporous bio-vitric drug delivery system that said method is obtained, it consists of: (CaO)
x-(SiO
2)
y-(P
2o
5)
z-M
w, wherein M is magnetic components, CaO:SiO
2: P
2o
5: the mass ratio of M is (5-30): (50-90): (0-20): (2-20), preferably (5-20): (70-85): 5:(5-10); Its material specific surface area is at 300-1000cm
2/ g, mesoporous pore size is at 2-50nm, and meso-hole structure is adjustable.
Magnetic mesoporous bio-vitric drug delivery system provided by the invention has excellent drug loading and sustained release performance, biocompatibility and biological activity, has broad application prospects at the biomedicine field such as pharmaceutical carrier and bone renovating material;
Tool of the present invention has the following advantages:
Raw material is easy to get, synthetic method and equipment needed thereby easy, building-up process environmental protection, almost without three industrial wastes;
With the pore passage structure that meso-hole structure specific surface area is large and special, add material surface medicine appendix amount, facilitate drug-loading system sustained release performance in vivo;
Utilize magnetic material radiation heat release, give material this in implantable bioartificial body after, by magnetic field effect, kill defective bone site morbidity cell etc.
Accompanying drawing explanation
The small angle X-ray diffraction collection of illustrative plates of magnetic mesoporous bio-vitric drug delivery system prepared by Fig. 1 embodiment 1.
The hysteresis curve of magnetic mesoporous bio-vitric drug delivery system prepared by Fig. 2 embodiment 1.
The transmission electron microscope photo of magnetic mesoporous bio-vitric drug delivery system prepared by Fig. 3 embodiment 1.
Drug release patterns after magnetic mesoporous bio-vitric drug delivery system Gentamicin Sulfate-loaded prepared by Fig. 4 embodiment 8.
Detailed description of the invention
Embodiment 1-6
First 4gP123 is placed in 50mL ethanol vigorous stirring, obtains uniform surfactant ethanol dispersion soln; Prepare inorganic matter presoma again, for obtaining by SiO shown in table 1
2: CaO:P
2o
5: Fe
3o
4the magnetic mesoporous bio-vitric drug delivery system of mass ratio, add inorganic matter in order respectively, wherein first group of embodiment is specially: 1.25g four water-calcium nitrate, 8.6mL (8g) tetraethyl orthosilicate (TEOS), 0.35mL(0.37g) triethyl phosphate (TEP), 0.142g nanometer Fe
3o
4particle, then adds rare HNO of 1-3mL
3(1mol/L) solution catalyzing hydrolysis under 40 DEG C of reaction temperatures; After the hydrolysis of inorganic matter presoma is uniformly dispersed, add surfactant ethanol dispersion soln, abundant hybrid reaction is carried out the sealing of soft mode version and is self-assembled into collosol and gel, product is in 60 DEG C of baking oven inner drying 1-3 days, by the gel that obtains after aging at 550-700 DEG C of temperature lower calcination 5-6h, just obtain the orderly magnetic mesoporous bio-vitric drug delivery system with two-dimentional hexagonal mesoporous structure, its corresponding small angle X-ray diffraction collection of illustrative plates, saturation magnetization hysteresis curve and transmission electron microscope picture respectively as Figure 1-3.
The prepared each component S iO of MMBG in table 1 embodiment 1-6
2: CaO:P
2o
5: Fe
3o
4mass ratio
Embodiment 7
By the step in embodiment 1, do not add magnetic nanoparticle, other technical process is identical with embodiment 1 with condition, finally obtains not having magnetic mesoporous bioglass drug delivery system, is blank group.
Embodiment 8
Select the magnetic mesoporous bio-vitric drug delivery system that embodiment 1 is obtained, carry out drug loading and slow release experiment.
(1) drug loading: take 30mg powder body gentamycin sulfate under inert gas shielding in glove box, is dissolved in 50mL deionized water the gentamicin sulfate solution being configured to 600 μ g/mL; Get 0.5g sample and be placed in solution, constant temperature vigorous stirring 24h under 37 DEG C of conditions.8000r/min centrifugalize, is placed in lower sediment in 37 DEG C of vacuum drying ovens and dries, and supernatant stays and does drug loading test.
(2) drug release: take the sample 0.2g after medicine carrying, the thin slice that diameter is 2-3cm is pressed into tablet machine, deionized water print being put into 100mL soaks, and respectively in different time points, adopts the drug level in ultraviolet-visible spectrophotometer detection solution.Its drug release patterns as shown in Figure 4.
Embodiment 9
By the step in embodiment 8, the antibiotic such as institute's carrying medicament vancomycin, amycin are replaced, other technical process is identical with embodiment 1 with condition, close in the drug loading efficiencies finally obtained and release profiles and embodiment 8, illustrate that this magnetic mesoporous bio-vitric drug delivery system is little by the impact of institute's load Antibiotics, all show good medicine carrying efficiency and sustained release performance.
Above-described embodiment is the present invention's preferably embodiment; but embodiments of the present invention are not restricted to the described embodiments; change, the modification done under other any does not deviate from spirit of the present invention and principle, substitute, combine, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (3)
1. a preparation method for magnetic mesoporous bio-vitric drug delivery system, described magnetic mesoporous bio-vitric drug delivery system its consist of: (CaO)
x-(SiO
2)
y-(P
2o
5)
z-M
w, wherein M is Fe
3o
4magnetic nano-particle, CaO:SiO
2: P
2o
5: the mass ratio of M is (5-30): (50-90): (0-20): (2-20); Its material specific surface area is at 300-1000cm
2/ g, mesoporous pore size is at 2-50nm, and meso-hole structure is adjustable, it is characterized in that, concrete steps are as follows:
(1) by surfactant-dispersed in alcoholic solution, get a uniform mixture;
(2) in the ratio of setting, calcium source, silicon source, phosphorus source and magnetic nano-particle order are added to the water, use diluted acid catalyzing hydrolysis;
(3) step (1) gained mixed solution is fully mixed with step (2) gained solution, carry out soft mode version sealing self assembly, obtain collosol and gel;
(4) by collosol and gel dry and aging after, at 550-700 DEG C of temperature lower calcination 4-6h, obtain magnetic mesoporous bio-vitric drug delivery system.
2. the preparation method of magnetic mesoporous bio-vitric drug delivery system according to claim 1, is characterized in that, described surfactant is ionic surfactant: C
nh
2n+1n (R)
3x, n=10-20, R=CH
3, C
2h
5, X=Cl
-, Br
-, or Pluronic F-127 as hydrophilic block, long chain alkane as the nonionic surfactant of hydrophobic group, or Pluronic F-127 is as hydrophilic block, propylene oxide or the butadiene monoxide block macromolecular surfactant as hydrophobic block, and its molecular formula is EO
npO
meO
n, n=10-140, m=5-100, or molecular formula EO
nbO
meO
n, n=10-200, m=10-100, PO is propylene oxide here, and EO is oxireme, and BO is butadiene monoxide.
3. according to the preparation method of magnetic mesoporous bio-vitric drug delivery system according to claim 1, it is characterized in that, described magnetic nano-particle is ferrospinel Fe
3o
4, silicon source is tetraethyl orthosilicate, and phosphorus source is triethyl phosphate, and calcium source is four water-calcium nitrate or calcium chloride.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103127506B (en) * | 2013-02-28 | 2015-09-23 | 苏州大学 | Magnetic mesoporous bioactivity glass micro-sphere material of core/shell structure and preparation method thereof |
| CN104117090B (en) * | 2013-04-24 | 2016-08-10 | 上海交通大学医学院附属第九人民医院 | Mesoporous bioglass porous support of labelled with radioisotope and preparation method thereof |
| CN103626396A (en) * | 2013-12-13 | 2014-03-12 | 天津工业大学 | Preparation method of titanium-containing mesoporous bioglass |
| CN104069543B (en) * | 2014-06-26 | 2015-09-30 | 浙江大学 | A kind of preparation method with the bio-vitric nanofiber of magnetic function |
| CN105327397B (en) * | 2015-11-17 | 2018-07-13 | 上海纳米技术及应用国家工程研究中心有限公司 | A kind of preparation of the degradable implantation material of the mesoporous calcium silicates coating of medical magnesium alloy surface |
| CN107007878A (en) * | 2017-05-11 | 2017-08-04 | 芜湖扬展新材料科技服务有限公司 | A kind of preparation method of VEGF transfecting biologicals activity glass tissue renovation material |
| CN109620955B (en) * | 2018-10-31 | 2021-08-20 | 东莞理工学院 | Biodegradable mesoporous nano magnetic material and preparation method thereof |
| CN109574507B (en) * | 2019-01-21 | 2022-07-05 | 河南理工大学 | Nano-scale spherical bioactive glass and preparation method thereof |
| CN110548214B (en) * | 2019-08-26 | 2021-08-31 | 北京理工大学 | Preparation method of miniature intelligent calcium alginate hydrogel end manipulator |
| CN113429127B (en) * | 2021-07-29 | 2022-10-04 | 武汉大学中南医院 | Magnetic bioactive glass and preparation method and application thereof |
| CN113975410A (en) * | 2021-10-21 | 2022-01-28 | 浙江中医药大学 | Fluorescent targeting nano-drug carrier, targeting drug and preparation method thereof |
| CN114130315B (en) * | 2021-11-23 | 2022-10-25 | 清华大学 | Surfactant gel-induced micro-nano particle self-assembly structure and preparation method thereof |
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| CN101623513A (en) * | 2009-01-22 | 2010-01-13 | 中国科学院上海硅酸盐研究所 | One-step method for preparing mesoporous bioglass material |
| CN101966344A (en) * | 2010-10-29 | 2011-02-09 | 中国科学院上海硅酸盐研究所 | Hollow core-shell nanometer mesoporous medicament carrying system with magnetism and luminescent performance, preparation method and application thereof |
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|---|---|---|---|---|
| CN1554607A (en) * | 2003-12-22 | 2004-12-15 | 复旦大学 | Nano mesoporous and mesoporous-macroporous composite biological glass and its preparing method |
| CN101623513A (en) * | 2009-01-22 | 2010-01-13 | 中国科学院上海硅酸盐研究所 | One-step method for preparing mesoporous bioglass material |
| CN101966344A (en) * | 2010-10-29 | 2011-02-09 | 中国科学院上海硅酸盐研究所 | Hollow core-shell nanometer mesoporous medicament carrying system with magnetism and luminescent performance, preparation method and application thereof |
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