CN105288743B - Mesoporous bioglass nano particle of radioisotope labeling and the preparation method and application thereof - Google Patents
Mesoporous bioglass nano particle of radioisotope labeling and the preparation method and application thereof Download PDFInfo
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- CN105288743B CN105288743B CN201410353907.6A CN201410353907A CN105288743B CN 105288743 B CN105288743 B CN 105288743B CN 201410353907 A CN201410353907 A CN 201410353907A CN 105288743 B CN105288743 B CN 105288743B
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Abstract
The invention discloses a kind of mesoporous bioglass nanoparticle radionuclide marked products and preparation method and application；The mesoporous bioglass nanoparticle label product can be prepared by following methods, and step is：Containing radionuclide45It is prepared by Ca sol solutions；Containing radionuclide45The preparation of the mesoporous bioglass nano particle of Ca；Silane coupling agent is to containing radionuclide45The mesoporous bioglass nano particle of Ca carries out amination surface modification.The present invention selects radionuclide45Ca, it has suitable half-life period, is 163.5 days.The mesoporous bioglass nano particle of radioisotope labeling provided by the invention, effectively mesoporous bioglass nano particle can be marked, internal distribution and the accumulation situation that can quantify and intuitively detect mesoporous bioglass nano particle, can be used for the body absorption of bio-vitric holder and the research of bio distribution.
Description
Technical field
The present invention relates to the mesoporous lifes of a kind of mesoporous bioglass nano particle more particularly to a kind of radioisotope labeling
Object glass nanoparticles and the preparation method and application thereof.
Background technology
Mesoporous bioglass (mesoporous bioactive glass, MBG) nano particle is with SiO2-CaO-P2O5
For basic constituent, the novel nano-material of the mesoporous channel design with high-sequential.Currently, by being induced certainly in evaporation
Different surfactants (such as cetab, polyethylene oxide-polycyclic oxygen third is added in assembling reaction process
Alkane-polyethylene oxide triblock copolymer etc.) mesoporous bioglass nanometer of the mesopore size within the scope of 2-10nm can be prepared
Grain, the range of specific surface area is in 300-1040m2/ g, Kong Rong can reach 0.36-1.54cm3/ g is the number of traditional biological glass
Ten times.Mesoporous bioglass nano particle has the special performance of nano material, shows small size, large specific surface area, surface
Good characteristics and the new functions such as activity is high, adsorption capacity is strong, and can selectively act on particular tissues and cell.Cause
This, has research using mesoporous bioglass nano particle as carrier, is applied to the research and development of slow releasing pharmaceutical；Also there is research by mesoporous life
Object glass nanoparticles are used for the various tumours of diagnosing and treating.In addition, mesoporous bioglass nano particle is not only with good
Biocompatibility and bioactivity also have the unique small-size effect of nano material and skin effect.By mesoporous bioglass
After nano particle is implanted in bone tissue, firm chemical bonds can be formed with bone tissue, and there is osteoinductive.This nanometer of material
Material is also one of emphasis and hot spot of bone renovating material research at present.
With the development of nanotechnology, nano material will increasingly extensively, about nanometer material in the application of biomedical sector
The biosafety issues of material also will be gradually valued by the people.And study the biological safety of nano material, it is therefore necessary to right
Application of the nano material in body carries out tracer, is received with studying biodistribution that nano material is metabolized in body and evaluation
Influence of the rice material to body function.It is research nano material vivo biodistribution credit to carry out radioisotope labeling to nano material
The important method of cloth.Can be to develop with mesoporous in addition, by the radioisotope labeling to mesoporous bioglass nano particle
Bio-vitric nano particle is that medicine, the bone renovating material etc. of carrier provide basis.
Establish the pass that a kind of technology of preparing of the mesoporous bioglass nano particle of radioisotope labeling is research work
Key and premise.Mesoporous bioglass nano particle is and the isotope element of common silicon using calcium-silicon matrix as main constituents
(31Si half-life period) is 170 minutes, relatively short；And calcium isotope (45Ca half-life period) is then 163.5 days.In addition, calcium group
Point it is constituent important in MBG, this is mainly due to the variations of Calcium compounds can adjust the curvature of surface-active micella partly
Diameter, to influence the meso-hole structure of mesoporous bioglass.Therefore, it selects45Ca can effectively be kept away from labeled in situ synthesis MBG holders
The problem of exempting to destroy meso-hole structure due to using the introducing of exogenous nucleic.Meanwhile45Ca discharges β rays, and energy is
0.26MeV has relatively stable organizational standard curve and the rate of recovery, can be to its radioactive activity using homogeneous liquid scintillation technique
Carry out Accurate Determining.Therefore, it only selects45Ca carries out mark in situ as radionuclide to mesoporous bioglass nano particle
Note is just expected to reach the expected purpose for disclosing degradation characteristic and bio distribution in nano particle body.
Silane coupling agent is kind of the low molecule silanes with special construction, and the inorganic nanoparticles that kind is important
Surface modifying material.The general formula of silane coupling agent is RSiX3, and R represents amino, sulfydryl, vinyl, epoxy group, cyano and methyl
The groups such as the third ethylene acyloxy, X represent the group that can be hydrolyzed, such as halogen, alkoxy, acyloxy.Silane coupling agent is to nothing
The surface of machine nano material is modified mainly by forming chemical bond realization.There are hydroxyls for mesoporous bioglass nano grain surface
Base, it can form chemical bonds with groups such as alkoxy, acyloxy in silane coupling agent, relatively more steady so as to obtain
Fixed marked product provides investigative technique for imaging and biodistribution research in further mesoporous bioglass nano particle body
It supports.
Invention content
The present invention provides a kind of mesoporous bioglass nano particles of radioisotope labeling, wherein uses radioactivity
Mesoporous bioglass nano particle is marked in nucleic, and the radionuclide is31Si、32P、45In Ca any one or
Several combinations.
Preferably, the radionuclide is45Ca。
Preferably, the composition of the mesoporous bioglass porous support of the radioisotope labeling include CaO,
SiO2And P2O5, wherein the molar ratio of Ca, Si and P are (1-30):(50-100):(1-10).
Preferably, the molar ratio of Ca, Si and P are 15:80:5.
Preferably, the mesoporous bioglass nano particle size dimension is the spherical shape of 50-100nm.
Preferably, the mesoporous size of the mesoporous bioglass nano particle is 2.5nm.
The present invention also provides a kind of preparation method of the mesoporous bioglass nano particle of above-mentioned radioisotope labeling,
Include the following steps：
Step a prepares precursor sol liquid：In a solvent by the dissolving of silicon source, calcium source, phosphorus source and surfactant, alkalinity
Under the conditions of stir 12 hours after be added in ptfe autoclave, hydration reaction 48h is carried out under the conditions of 80 DEG C.Wherein,
The molar ratio of Ca, Si and P are 15 in the calcium source, silicon source and phosphorus source:80:5, wherein：
The silicon source containing radionuclide containing at least trace quantity in the silicon source, and/or
The calcium source containing radionuclide containing at least trace quantity in the calcium source, and/or
The phosphorus source containing radionuclide containing at least trace quantity in phosphorus source；
Step b will be sintered 5 hours at a temperature of step b treated 550 DEG C of precursor liquids, obtain the radionuclide mark
The mesoporous bioglass nano particle of note.
Step c, by what is obtained after step b sintering45The mesoporous bioglass nano particle of Ca labels is added to silane coupled
Dilution agent solution makes its silane amination.
Preferably, the silicon source is positive silicate class.
Preferably, the silicon source is selected from least one of ethyl orthosilicate, methyl orthosilicate and positive silicic acid propyl ester；
Preferably, the calcium source is inorganic calcium.
Preferably, the calcium source is selected from least one of calcium nitrate, calcium acetate and its hydrate.
Preferably, phosphorus source is organophosphorus compounds.
Preferably, phosphorus source is selected from least one of trimethyl phosphate and triethyl phosphate.
Preferably, the surfactant is cationic surfactant.
Preferably, the cationic surfactant is selected from CTAB.
The present invention has significant technique effect as a result of above technical scheme：
The mesoporous bioglass nano particle of radioisotope labeling provided by the invention, can be effectively to mesoporous biological glass
Glass nano particle is marked, and can quantify and the internal of intuitive detection mesoporous bioglass nano particle is distributed and accumulation feelings
Condition can be used for the body absorption of bio-vitric holder and the research of bio distribution.
Description of the drawings
Fig. 1 is that the silica gel thin-layer paper chromatography (ITLC/SG methods) of 1 gained mesoporous bioglass nano particle of embodiment marks
The qualification result figure of product；
Fig. 2 is transmission electron microscope (TEM) figure of 1 gained mesoporous bioglass nano particle of embodiment；
Fig. 3 is FTIR spectrum (FTIR) figure of 1 gained mesoporous bioglass nano particle of embodiment；
Fig. 4 is scanning electron microscope (SEM) figure of 1 gained mesoporous bioglass nano particle of embodiment.
Specific implementation mode
Radioisotope labeling tracer technique is using the compound of radionuclide or its label as tracer, application
Ray is determined to detect the distribution of tracer in conjunction with autoradiograph, the counting of micro- sem observation, liquid scintillation counter etc.
Property quantitative observation analysis method, have the characteristics that high sensitivity, method simplicity, positioning and quantitative it is accurate, therefore, using radioactivity
Isotope labeling tracer technique marks mesoporous bioglass nano particle, can be the bio distribution and in-vivo imaging of nano particle
Research provides important technological means.
Mesoporous bioglass nano particle is and the isotope element of common silicon using calcium-silicon matrix as main constituents
(31Si half-life period) is 170 minutes, relatively short；And calcium isotope (45Ca half-life period) is then 163.5 days, and45Ca discharges
β rays, energy 0.26MeV have relatively stable organizational standard curve and the rate of recovery, using homogeneous liquid scintillation technique energy
Accurate Determining is carried out to its radioactive activity.Therefore, it selects45Ca as radionuclide to mesoporous bioglass nano particle into
Row labeled in situ is effective key problem in technology for disclosing bio distribution and accumulation situation in nano particle body.
1-4 with reference to the accompanying drawings, the present invention is described in more detail with the following Examples, to more fully understand this hair
It is bright.
Embodiment 1
(1) contain radionuclide45The preparation of Ca sol solutions
First with 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, and it is 1.1g to make the total amount of calcium nitrate tetrahydrate.Then distinguish
The cetyl three of 0.56g triethyl phosphates (TEP), 5.22g ethyl orthosilicates (TEOS), 0.46g sodium hydroxides, 1.4g is added
The polyvinylpyrrolidone (PVP) of methyl bromide ammonium (CTAB) and 1g, stirring and dissolving is in the deionized water of 120ml (in solution
The molar ratio of Si, Ca and P are 80:15:5) it is added in ptfe autoclave after, reacting at room temperature 12 hours, at 80 DEG C
Carry out hydration reaction 48 hours.
Wherein, reagent calcium nitrate tetrahydrate, triethyl phosphate, ethyl orthosilicate, cetyl trimethylammonium bromide and poly-
Vinylpyrrolidone is purchased from Sigma.
(2) contain radionuclide45The preparation of the mesoporous bioglass nano particle of Ca
The product obtained after hydration reaction is sintered after washing 3 times with alcohol under air environment, sintering temperature 550
DEG C, sintering time is 5 hours, and sintering heating rate is 5 DEG C of min-1.After cooling to get to45The mesoporous biological of Ca labels
Glass nanoparticles.
(3) contain radionuclide45The silane amination of the mesoporous bioglass nano particle of Ca
Radionuclide will be contained45The mesoporous bioglass nano particle of Ca is placed in ethanol solution, under 59KHz frequencies
Ultrasonic 30min, it is spare after being cleaned repeatedly with absolute ethyl alcohol.It takes out 90mL ethanol solutions and (includes 200mg radionuclides45Ca is marked
The mesoporous bioglass nano particle of note), and 10mL is added
(molecular formula is (3- aminopropyls) triethoxysilane：H2N(CH2)3Si(OC2H5)3) solution (coupling agent：Second
Alcohol=1：5, V/V), 60 DEG C of stirred in water bath is reacted 4 hours, and it is 8 to keep reacting solution pH value.After reaction, second is used
Alcohol washs, and vacuum drying obtains amino modified containing radionuclide45The mesoporous bioglass nano particle of Ca.
Silica gel thin-layer paper chromatography is used to the identification of gained mesoporous bioglass nanoparticle label product
(ITLC/SG methods) is identified.With Flash silica thin-layer chromatography paper (ITLC/SG) for carrier, it is unfolded with physiological saline, then will
Every chromatographic paper is cut into the equidistant small paper slips of 1cm, is put into radioactivity survey test tube and is measured.The results are shown in Figure 1,45Ca-Rf values are all in 0.80~1.00 range, and marked mesoporous bioglass nano particle Rf values are 0.00, in paper chromatography
Origin is motionless.Through obtained marked product radio-chemical purity >=95% of above method identification.
Tem observation is carried out to gained mesoporous bioglass nano particle, the results are shown in Figure 2, it is seen that nanochannel structure,
Granular size size is 50-100nm.FTIR observation gained mesoporous bioglass nano particles, the results are shown in Figure 3, modified
The infrared curve 2979.4cm of nano particle-1There is the characteristic absorption peak of coupling agent in place, illustrates that coupling agent has been attached to nanometer
Particle surface.The visible mesoporous bioglass nano particle of SEM observations is spherical in shape, the visible certain meso-hole structure in surface.
The present embodiment selects radionuclide45Ca, it has suitable half-life period, is 163.5 days, can be used for mesoporous life
Object glass nanoparticles absorb in vivo and the research of bio distribution.Radioactive pollution is easily controllable and handles.Pass through radioactivity
Nucleic45Ca can be quantified and the internal degradation situation of intuitive detection mesoporous bioglass nano particle.It utilizes45The characteristic of Ca,
The research of vivo biodistribution credit cloth can be carried out to mesoporous bioglass nano particle with liquid scintillation technology by tissue digestion.
The mesoporous bioglass nano particle of radioisotope labeling provided by the invention, can be effectively to mesoporous biological glass
Glass nano particle is marked, and can quantify and the internal of intuitive detection mesoporous bioglass nano particle is distributed and accumulation feelings
Condition can be used for the body absorption of bio-vitric holder and the research of bio distribution.
Specific embodiments of the present invention are described in detail above, but it is intended only as example, the present invention is simultaneously unlimited
It is formed on particular embodiments described above.To those skilled in the art, it is any to the equivalent modifications that carry out of the present invention and
It substitutes also all among scope of the invention.Therefore, without departing from the spirit and scope of the invention made by impartial conversion and
Modification, all should be contained within the scope of the invention.
Claims (8)
1. a kind of mesoporous bioglass nano particle of radioisotope labeling, it is characterised in that：The mesoporous bioglass
There is label, the radionuclide is on nano particle45Ca；The mesoporous bioglass nanoparticle size
For 50-100nm, and there is meso-hole structure；The composition of the mesoporous bioglass nano particle of the radioisotope labeling at
Part includes CaO, SiO2And P2O5；Wherein, the molar ratio of Ca, Si and P are (1-30):(50-100):(1-10)；
The preparation method of the mesoporous bioglass nano particle, includes the following steps：
Step a：Prepare precursor sol liquid：In a solvent by the dissolving of silicon source, calcium source, phosphorus source and surfactant, alkaline condition
Lower stirring is added to after 12 hours in ptfe autoclave, and hydration reaction 48h is carried out under the conditions of 80 DEG C；Wherein, described
The molar ratio of Ca, Si and P are (1-30) in calcium source, silicon source and phosphorus source:(50-100):(1-10), containing at least in the calcium source
Trace quantity contains radionuclide45The calcium source of Ca, wherein：
The silicon source containing radionuclide containing at least trace quantity in the silicon source, and/or
The phosphorus source containing radionuclide containing at least trace quantity in phosphorus source；
Step b：By step a, treated that precursor liquid is sintered 5 hours at a temperature of 550 DEG C, obtains the radioisotope labeling
Mesoporous bioglass nano particle；
Step c：By what is obtained after step b sintering45It is dilute that the mesoporous bioglass nano particle of Ca labels is added to silane coupling agent
Solution is released, its silane amination is made；
The surfactant is CTAB.
2. a kind of preparation method of the mesoporous bioglass nano particle of radioisotope labeling as described in claim 1, special
Sign is, includes the following steps：
Step a：Prepare precursor sol liquid：In a solvent by the dissolving of silicon source, calcium source, phosphorus source and surfactant, alkaline condition
Lower stirring is added to after 12 hours in ptfe autoclave, and hydration reaction 48h is carried out under the conditions of 80 DEG C；Wherein, described
The molar ratio of Ca, Si and P are (1-30) in calcium source, silicon source and phosphorus source:(50-100):(1-10), containing at least in the calcium source
Trace quantity contains radionuclide45The calcium source of Ca, wherein：
The silicon source containing radionuclide containing at least trace quantity in the silicon source, and/or
The phosphorus source containing radionuclide containing at least trace quantity in phosphorus source；
Step b：By step a, treated that precursor liquid is sintered 5 hours at a temperature of 550 DEG C, obtains the radioisotope labeling
Mesoporous bioglass nano particle；
Step c：By what is obtained after step b sintering45It is dilute that the mesoporous bioglass nano particle of Ca labels is added to silane coupling agent
Solution is released, its silane amination is made；
The surfactant is CTAB.
3. preparation method according to claim 2, it is characterised in that：In step a, the silicon source is positive silicate class；Institute
It is inorganic calcium to state calcium source；Phosphorus source is organophosphorus compounds.
4. preparation method according to claim 3, it is characterised in that：The silicon source is selected from ethyl orthosilicate, positive silicic acid first
At least one of ester and positive silicic acid propyl ester；The calcium source is selected from calcium nitrate, calcium acetate, nitric acid hydrate of calcium, calcium acetate hydration
At least one of object；Phosphorus source is selected from least one of trimethyl phosphate and triethyl phosphate.
5. according to the preparation method described in claim 2,3 or 4, it is characterised in that：The calcium source is calcium nitrate tetrahydrate, is contained
At least trace quantity45Ca(NO3)2·4H2O。
6. preparation method according to claim 5, it is characterised in that：The preparation method of the calcium source is as follows：Utilize nitric acid
Sodium, containing trace quantity45CaCl2Calcium chloride be changed into containing trace quantity45Ca(NO3)2·4H2The calcium nitrate tetrahydrate of O, then
Surplus calcium nitrate tetrahydrate is added to get the calcium source.
7. preparation method according to claim 2, it is characterised in that：Silane coupling agent is (3- aminopropans in the step c
Base) triethoxysilane.
8. preparation method according to claim 2, it is characterised in that：In the step c in silane coupling agent dilute solution
Constituent proportioning is coupling agent：Ethyl alcohol=1：5V/V.
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| CN106316108A (en) * | 2016-08-19 | 2017-01-11 | 上海交通大学医学院附属第九人民医院 | Mesoporous bioglass nanosphere with radial pore channels and preparation method of mesoporous bioglass nanosphere with radial pore channels |
| DE102016119239A1 (en) * | 2016-10-10 | 2018-04-12 | Oncobeta International Gmbh | Particles and compositions comprising rhenium compounds and processes for obtaining such products |
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| CN101314039A (en) * | 2008-07-03 | 2008-12-03 | 华南理工大学 | Biological activity glass mesoporous microsphere and preparation method thereof |
| CN101757644A (en) * | 2008-12-23 | 2010-06-30 | 李树义 | Structure of radioactive micro balls and preparation method |
| CN101829341A (en) * | 2009-03-13 | 2010-09-15 | 上海交通大学医学院附属第九人民医院 | Hydroxyapatite nanoparticle radionuclide marked product and preparation method thereof |
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| US9114162B2 (en) * | 2004-10-25 | 2015-08-25 | Celonova Biosciences, Inc. | Loadable polymeric particles for enhanced imaging in clinical applications and methods of preparing and using the same |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101314039A (en) * | 2008-07-03 | 2008-12-03 | 华南理工大学 | Biological activity glass mesoporous microsphere and preparation method thereof |
| CN101757644A (en) * | 2008-12-23 | 2010-06-30 | 李树义 | Structure of radioactive micro balls and preparation method |
| CN101829341A (en) * | 2009-03-13 | 2010-09-15 | 上海交通大学医学院附属第九人民医院 | Hydroxyapatite nanoparticle radionuclide marked product and preparation method thereof |
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| "A quantitative method for evaluating the degradation of biologic scaffold materials";Thomas W. Gilbert等;《Biomaterials》;20060901;第28卷;147-150 * |
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