CN104117090B - Mesoporous bioglass porous support of labelled with radioisotope and preparation method thereof - Google Patents
Mesoporous bioglass porous support of labelled with radioisotope and preparation method thereof Download PDFInfo
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- CN104117090B CN104117090B CN201310143666.8A CN201310143666A CN104117090B CN 104117090 B CN104117090 B CN 104117090B CN 201310143666 A CN201310143666 A CN 201310143666A CN 104117090 B CN104117090 B CN 104117090B
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Abstract
The invention provides the mesoporous bioglass porous support of a kind of labelled with radioisotope, wherein, use radiosiotope to be marked mesoporous bioglass porous support, described radiosiotope is31Si、32P、45Any one or a few combination in Ca.The mesoporous bioglass porous support of this labelled with radioisotope, effectively mesoporous bioglass porous support can be marked, the vivo degradation situation of mesoporous bioglass porous support be can quantitatively and intuitively detect, the body absorption of bio-vitric support and chorologic research may be used for.
Description
Technical field
The present invention relates to a kind of mesoporous bioglass porous support, particularly relate to a kind of labelled with radioisotope
Mesoporous bioglass porous support.
Background technology
Bio-vitric can realize specific biological, the glass of physiological function, has good biocompatibility, life
Thing degradability and mechanical property.Hench in 1971 etc. utilize fusion method first to prepare the life with Bone Defect Repari performance
Since thing glass (bioactive glass, BG) material, through 30 years of researches and development, bio-vitric
The fields such as osseous tissue displacement, bone defect healing, bone filler and biological coating it are applied to.
But research discovery dense form bio-vitric exists, and degradation speed is slow, biological activity is not enough, be unfavorable for skeletonization etc.
Problem.Then, it is attempted to by design porous support and in bio-vitric, introduces meso-hole structure to improve life
The biological activity of thing glass and degradation property.The i.e. mesoporous biological glass of bio-vitric porous support based on meso-hole structure
Glass porous support has high specific surface area and adjustable mesoporous passage, and it is at biomineralization and pharmaceutical carrier etc.
Aspect has important application potential.Such as CN102188749A discloses one and has mesoporous bioglass painting
The three-dimensional porous rack of layer, is incorporated into the big hole surface of three-dimensional polymer support by mesoporous bioglass coating,
Effectively increase the hydrophilicity of support, improve cellular affinity and the mechanical property of support, and be provided simultaneously with
Effectively support and transmit the function of anti-inflammatory drug, it is achieved support and the double effects of pharmaceutical carrier.And for example
CN102190428A discloses a kind of ordered mesoporous microsphere medicine carrier, uses emulsion technology, and preparation is containing aerobic
Compound CaO, SiO2And P2O5Oily bag alcohol-water emulsion, through rotary evaporation remove solvent, forge after ageing
Burn off goes template to obtain having bioactive mesoporous microsphere.The mesoporous glass microsphere prepared has controlled rule
Then profile, certain duct order, aperture that volume can regulate and specific surface area, surface can carry out chemistry
Modification, improves drug load, reaches more preferable sustained drug release effect.
But, about mesoporous bioglass porous support degradation characteristic in vivo, metabolic fate and to machine
The series of problems such as the impact of body locally and systemically histoorgan it be not immediately clear.Answer these problems, first
First must solve to occur to degrade and the spike problem of catabolite in support enters organism, and the premise of spike
Then need to determine that can this mesoporous bioglass porous support by effective labelling？Label is if appropriate for support
Degradation time？The stability of label itself how？Etc., up to now, also there is no the mesoporous life of a kind of labelling
The effective ways of thing glass frit support.
Summary of the invention
It is an object of the invention to overcome above-mentioned deficiency, it is provided that the mesoporous biological glass of a kind of labelled with radioisotope
Glass porous support, can be marked mesoporous bioglass porous support effectively, can quantitatively and intuitively detect
The vivo degradation situation of mesoporous bioglass porous support.
The invention provides the mesoporous bioglass porous support of a kind of labelled with radioisotope, wherein, use
Mesoporous bioglass porous support is marked by radiosiotope, and described radiosiotope is31Si、32P、45Any one or a few combination in Ca.
Preferably, described radiosiotope is45Ca。
Preferably, the composition of the mesoporous bioglass porous support of described labelled with radioisotope includes
CaO、SiO2And P2O5, wherein, the mol ratio of Ca, Si and P is (1-30): (50-100): (1-10).
Preferably, the mol ratio of Ca, Si and P is 15: 80: 2.5.
Wherein, radiosiotope45The average radiation intensity of the mesoporous bioglass porous support of Ca labelling is
185kBq。
Preferably, described mesoporous bioglass porous support has meso-hole structure and macropore communications and liaison structure.
Preferably, the macropore diameter in described macropore communications and liaison structure is 200-500 μm.
Present invention also offers the system of the mesoporous bioglass porous support of a kind of above-mentioned labelled with radioisotope
Preparation Method, comprises the following steps:
Step 1, prepares precursor sol liquid: silicon source, calcium source, phosphorus source and surfactant are dissolved in solvent
In, stir 8-48 hour, wherein, Ca, Si and P in described silicon source, calcium source and phosphorus source under acid condition
Mol ratio be (1-30): (50-100): (1-10), described surfactant with the mass ratio in calcium source is
(0.5-4): (0.2-1.4), described solvent is 30 with the mass ratio in calcium source: (0.2-1.4), wherein:
In described silicon source containing at least trace quantity containing radioisotopic silicon source, and/or
In described calcium source containing at least trace quantity containing radioisotopic calcium source, and/or
In phosphorus source containing at least trace quantity containing radioisotopic phosphorus source；
Step 2, is immersed in rack template in the precursor sol liquid that step 1 prepares, then takes out dry,
Repetitive operation；
Step 3, sinters 3-12 hour at a temperature of 500-900 ° of C of the rack template after step 2 being processed,
Mesoporous bioglass porous support to described labelled with radioisotope.
Preferably, described silicon source is positive silicate class.
Preferably, at least one in tetraethyl orthosilicate, methyl silicate and positive silicic acid propyl ester of described silicon source；
Preferably, described calcium source is inorganic calcium.
Preferably, at least one in calcium nitrate, calcium acetate and its hydrate of described calcium source.
Preferably, phosphorus source is organophosphorus compounds.
Preferably, at least one in trimethyl phosphate and triethyl phosphate of phosphorus source.
Preferably, described surfactant is block copolymer nonionic surfactant.
Preferably, described block copolymer nonionic surfactant selected from P123, P105, P104, P103,
P85、P84、P75、P65、P38、F127、F108、F98、F88、F87、F77、F68、
F38、L122、L121、L101、L92、L81、L72、L65、L64、L63、L62、L61、L44、
At least one in L43, L42, L35, L31 and FC-4；；
It is highly preferred that described silicon source is tetraethyl orthosilicate (TEP), described calcium source is calcium nitrate tetrahydrate, institute
Stating phosphorus source is triethyl phosphate (TEOS), and described block copolymer nonionic surfactant is P123.
Preferably, described radiosiotope is31Si、32P or45Ca。
It is highly preferred that described radiosiotope is45Ca。
It is further preferred that described calcium source is calcium nitrate tetrahydrate, containing at least trace quantity45Ca(NO3)2·4H2O。
Preferably, utilize sodium nitrate, containing trace quantity45CaCl2Calcium chloride be changed into containing trace quantity45Ca(NO3)2·4H2The calcium nitrate tetrahydrate of O, adds surplus calcium nitrate tetrahydrate, both described calcium source.
Preferably, in step 1, acid condition be by add concentration be the hydrochloric acid of 0.05-5mmol/L
Regulation pH value is to pH=1-6.
Preferably, concentration is that the salt acid for adjusting pH value of 0.1-1mmol/L is to pH=2-5.
Preferably, concentration is that the salt acid for adjusting pH value of 0.5mmol/L is to pH=3-4.
Wherein it is preferred to, in described silicon source, calcium source and phosphorus source, the mol ratio of Ca, Si and P is 15: 80:
5。
Preferably, in step 2, rack template is immersed at least 5min in the precursor sol liquid that step 1 prepares.
Preferably, in step 2, repetitive operation 3-20 time.
Preferably, in step 3, sintering temperature is 700 ° of C, and sintering time is 6 hours, and sintering heats up fast
Degree is 5 ° of C/min.
Wherein, solvent described in step 1 can be organic solvent, inorganic solvent or the mixture of the two.
Described inorganic solvent is preferably water.
Described organic solvent be preferably aliphatic hydrocarbon, aromatic hydrocarbon, chlorohydrocarbon, alcohol, ketone, aldehyde, ester, nitrile, carboxylic acid,
Sulfoxide, amide solvent.
The example of described aliphatic hydrocarbon includes: pentane, hexane, octane, hexamethylene etc..
The example of described aromatic hydrocarbon includes: styrene, benzene,toluene,xylene etc..
The example of described chlorohydrocarbon includes: dichloromethane, chloroform, carbon tetrachloride, bromofom, chlorobenzene, dichloro-benzenes
(paracide, o-dichlorohenzene), sym-tetrachloroethane etc..
The example of described alcohol includes: methanol, ethanol, ethylene glycol, propanol, isopropanol, propylene glycol, the tert-butyl alcohol,
Glycerol, butanediol, pentanediol, glycol monoethyl ether, ethylene glycol monoethyl ether, ethylene glycol monobutyl ether etc..
The example of described ketone includes: acetone, butanone, methyl butyl ketone, Ketohexamethylene etc..
The example of described aldehyde includes: acetaldehyde, propionic aldehyde, glutaraldehyde, Biformyl etc..
The example of described ester includes: methyl acetate, ethyl acetate, propyl acetate, butyl acetate, pentyl acetate,
Methyl formate, Ethyl formate, butyl formate, amyl formate etc..
The example of described nitrile is such as: acetonitrile etc..
The example of described carboxylic acid includes: formic acid, acetic acid etc..
The example of described sulfoxide includes: dimethyl sulfoxide, thionyl chloride, diphenyl sulfoxide etc..
The example of described amide includes: N,N-dimethylformamide, N, N-diethylformamide etc..
Preferably, solvent described in step 1 includes methanol, ethanol, ethylene glycol, propanol, isopropanol, hexafluoro
Isopropanol, propylene glycol, the tert-butyl alcohol, glycerol, butanediol, pentanediol, glycol monoethyl ether, ethylene glycol list second
At least one in ether, ethylene glycol monobutyl ether etc..
Preferably, solvent described in step 1 also includes water.
Present invention also offers the mesoporous bioglass porous support of above-mentioned labelled with radioisotope at osseous tissue
Application in displacement, bone defect healing, bone filler and/or biological coating.
The mesoporous bioglass porous support of the labelled with radioisotope that the present invention provides, can be effectively to mesoporous
Bio-vitric porous support is marked, and can quantitatively and intuitively detect the internal of mesoporous bioglass porous support
Degraded situation, may be used for the body absorption of bio-vitric support and chorologic research.
Accompanying drawing explanation
Fig. 1 is the small angle x-ray diffraction (SAXD) figure of embodiment gained mesoporous bioglass porous support；
Fig. 2 is scanning electron microscope (SEM) figure of embodiment gained mesoporous bioglass porous support；
Fig. 3 is transmission electron microscope (TEM) figure of embodiment gained mesoporous bioglass porous support；
Fig. 4 is embodiment gained45The mesoporous bioglass porous support of Ca labelling45Release knot external for Ca
Fruit figure.
Detailed description of the invention
Radioisotope labeling tracer technique be the compound utilizing radionuclide or its labelling as tracer,
Application ray detects the distribution of tracer, and combines autoradiography, microscope observation counting, liquid scintillation
Calculating instruments etc. carry out the method for qualitative, quantitative observation analysis, have highly sensitive, method is easy, positioning and quantitative is accurate
True feature, therefore, uses radioisotope labeling tracer technique to carry out labelling mesoporous bioglass porous support,
Can be the bio distribution of internal timbering material and research that material lapses to provides important technological means.
Mesoporous bioglass porous support is with CaO-SiO2-P2O5Based on constituent, in vitro study proves
After this support soaks different time in simulated body fluid, can detect that substantial amounts of Ca, Si and P element, thus table
The catabolite of bright support is mainly these three element, the radiosiotope corresponding by analyzing them respectively
Find after label, conventional31The half-life of Si is 170 minutes,32The half-life of P is 14.3 days, and45Ca's
Half-life is then 163 days.Degradation time in vitro (about 90 days) according to mesoporous bioglass porous support,
Obviously most preferably select45Ca carries out labeled in situ as radionuclide to mesoporous bioglass porous support,
Reach to disclose degradation characteristic and chorologic expection purpose in stake body.
With reference to the accompanying drawings, the present invention is described in more detail in conjunction with the embodiments, to be more fully understood that the present invention.
(1) containing radiosiotope45Prepared by the sol solutions of Ca
First with sodium nitrate, utilize sodium nitrate, containing trace quantity45CaCl2Calcium chloride be changed into containing
Trace quantity45Ca(NO3)2·4H2The calcium nitrate tetrahydrate of O, adds surplus calcium nitrate tetrahydrate, makes four
The total amount of nitric hydrate calcium is 0.7g.It is then respectively adding 0.365g TEP, 3.35g TEOS, 0.5g's
The P123 of 0.5mol/L HCl and 2.0g, stirring and dissolving in the ethanol of 30g (in solution, Si, Ca and
The mol ratio of P is 80: 15: 5), after stirring one day under room temperature, obtain containing radionuclide45Ca's is molten
Glue.
Wherein, reagent calcium nitrate tetrahydrate, TEOS, TEP and P123(MW=5800) all it is purchased from Sigma.
(2) containing radiosiotope45Prepared by the mesoporous bioglass porous support of Ca
With dehydrated alcohol the small cylinder polyurethane sponge of diameter 3mm, high 3mm embathed 3 times, after drying
Standby.Take a certain amount of small cylinder polyurethane sponge and be immersed in gained containing radionuclide45In the sol solutions of Ca,
Keeping 15 minutes under room temperature, period constantly extrudes small cylinder polyurethane sponge, to guarantee that sol solutions penetrates into
In whole sponge structure；Taking-up small cylinder polyurethane sponge is to glass dish, and is placed on fume hood in room temperature
Under be dried 24 hours.For ensureing that the hole of support opens and coating uniform, take out small cylinder polyurethane sponge
After glass dish, be by unnecessary sol solutions extrusion.Repeat said process 8 times.
Being sintered under air ambient by polyurethane sponge after above-mentioned process, sintering temperature is 700 ° of C, burns
The knot time is 6 hours, and sintering heating rate is 5 ° of C min-1.After cooling, both must be with45Jie of Ca labelling
Hole bio-vitric porous support.
Gained mesoporous bioglass porous support is carried out X-ray diffraction observation, and result is as it is shown in figure 1, in figure
There is obvious diffraction maximum, show that mesoporous bioglass porous support has ordered mesopore structure；Under scanning electron microscope
Observing gained mesoporous bioglass porous support, result is as shown in Figure 2, it is seen that macropore communications and liaison structure；Transmission electricity
Microscopic observation mesoporous bioglass porous support, result is as shown in Figure 3, it is seen that orderly nanochannel structure.
Measure45The radioactive intensity of the mesoporous bioglass porous support of Ca labelling: will45Ca labelling mesoporous
Bio-vitric porous support is after HF digests, then measures each with liquid scintillator measuring apparatus45Jie of Ca labelling
The radioactivity amount (DPM, radioactive decay number of times per minute) of hole bio-vitric porous support, calculates it and puts down
All radioactive intensities are 185kBq.
To gained45The mesoporous bioglass porous support of Ca labelling carries out extracorporeal releasing experiment: take 8 gained45The mesoporous bioglass porous support of Ca labelling, is respectively put in each little plastic tube, then is separately added into 2ml
SBF solution is in each pipe.After separated in time (1,3,6,24 and 48 hours etc.), take out 1ml
Solution, 0.22um membrane filtration, then with after the 1ml washed filter of SBF solution, merge filtrate, use liquid
Flicker measuring instrument measure gained liquid radioactivity amount, result as shown in Figure 4,45Ca 24 days flat in vitro
All adding up release rate is 19.52%.
The present embodiment selects radiosiotope45Ca, it has the suitable half-life, is 163 days, permissible
Absorb in vivo and chorologic research for mesoporous bioglass porous support.Radioactive pollution is easily controllable
And process.Pass through radiosiotope45Ca can quantitatively and intuitively detect mesoporous bioglass porous support
Vivo degradation situation.Utilize45The characteristic of Ca, can pass through tissue digestion, by liquid scintillation technology to Jie
Hole bio-vitric support carries out the research of vivo biodistribution credit cloth.
By containing45The CaCl of Ca2Mesoporous bioglass porous support is carried out directly by building-up process
Labeled in situ, by the marked product obtained by this labeling method45Ca is stable, may be used for mesoporous biological
The body absorption of glass supporter and chorologic research.
Being described in detail the specific embodiment of the present invention above, but it is intended only as example, the present invention is also
It is not restricted to particular embodiments described above.To those skilled in the art, any the present invention is carried out
Equivalent modifications and substitute the most all among scope of the invention.Therefore, without departing from the spirit of the present invention and model
Enclose lower made impartial conversion and amendment, all should contain within the scope of the invention.
Claims (8)
1. the preparation method of the mesoporous bioglass porous support of a labelled with radioisotope, it is characterised in that
Comprise the following steps:
Step 1, prepares precursor sol liquid: silicon source, calcium source, phosphorus source and surfactant are dissolved in a solvent,
Stirring 8-48 hour under acid condition, wherein, in described silicon source, calcium source and phosphorus source, Ca, Si and P's rubs
Your ratio is (1-30): (50-100): (1-10), and described surfactant is (0.5-4) with the mass ratio in calcium source:
(0.2-1.4), described solvent is 30:(0.2-1.4 with the mass ratio in calcium source), wherein:
In described silicon source containing at least trace quantity containing radioisotopic silicon source, and/or
In described calcium source containing at least trace quantity containing radioisotopic calcium source, and/or
In phosphorus source containing at least trace quantity containing radioisotopic phosphorus source；
Step 2, is immersed in rack template in the precursor sol liquid that step 1 prepares, then takes out dry, repeats
Operation；
Step 3, sinters 3-12 hour at a temperature of the rack template after step 2 being processed 500-900 DEG C, obtains institute
State the mesoporous bioglass porous support of labelled with radioisotope.
Preparation method the most according to claim 1, it is characterised in that in step 1, described silicon source is positive silicon
Esters of gallic acid；Described calcium source is inorganic calcium；Phosphorus source is organophosphorus compounds.
Preparation method the most according to claim 2, it is characterised in that described silicon source selected from tetraethyl orthosilicate,
At least one in methyl silicate and positive silicic acid propyl ester；Described calcium source is selected from calcium nitrate, calcium acetate and its hydration
At least one in thing；At least one in trimethyl phosphate and triethyl phosphate of phosphorus source.
4. according to the preparation method described in claim 1,2 or 3, it is characterised in that described calcium source is four hydrations
Calcium nitrate, containing at least trace quantity45Ca(NO3)2·4H2O。
Preparation method the most according to claim 4, it is characterised in that utilize sodium nitrate, containing trace quantity45CaCl2Calcium chloride be changed into containing trace quantity45Ca(NO3)2·4H2The calcium nitrate tetrahydrate of O, adds
Surplus calcium nitrate tetrahydrate, both described calcium source.
6. a mesoporous bioglass porous support for the labelled with radioisotope that prepared by method described in claim 1,
It is characterized in that, use radiosiotope that mesoporous bioglass porous support is marked, described radioactivity
Isotope is31Si、32P、45Any one or a few combination in Ca.
The mesoporous bioglass porous support of labelled with radioisotope the most according to claim 6, its feature
Being, described radiosiotope is45Ca。
The mesoporous bioglass porous support of labelled with radioisotope the most according to claim 6, its feature
Being, described mesoporous bioglass porous support has meso-hole structure and macropore communications and liaison structure.
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| CN107522389B (en) * | 2017-07-26 | 2020-06-19 | 华南理工大学 | Micro-nano bioactive glass microsphere with surface nano-pore structure and preparation method thereof |
| CN108083618A (en) * | 2017-12-15 | 2018-05-29 | 华南理工大学 | A kind of micro-nano bioactivity glass microballoon prepared using microemulsion technology and preparation method thereof |
| CN110101904B (en) * | 2019-06-20 | 2020-07-28 | 北京幸福益生再生医学科技有限公司 | Degradable regenerative medical material for promoting tissue in-situ regeneration and preparation method thereof |
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| CN101643645A (en) * | 2009-07-24 | 2010-02-10 | 华中科技大学 | Calcium phosphate material marked by fluorescein isothiocyanate and preparation method thereof |
| CN102526797A (en) * | 2012-02-08 | 2012-07-04 | 同济大学 | Preparation method of high-strength biological glass bone bracket with regular-hole distribution |
| CN102921010A (en) * | 2012-11-22 | 2013-02-13 | 上海师范大学 | Magnetic mesoporous bioactive glass drug delivery system and preparation method thereof |
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Patent Citations (3)
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|---|---|---|---|---|
| CN101643645A (en) * | 2009-07-24 | 2010-02-10 | 华中科技大学 | Calcium phosphate material marked by fluorescein isothiocyanate and preparation method thereof |
| CN102526797A (en) * | 2012-02-08 | 2012-07-04 | 同济大学 | Preparation method of high-strength biological glass bone bracket with regular-hole distribution |
| CN102921010A (en) * | 2012-11-22 | 2013-02-13 | 上海师范大学 | Magnetic mesoporous bioactive glass drug delivery system and preparation method thereof |
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