CN105860974A - PVP modified magnetic-fluorescent core-shell La1-xSrxMnO3 / ZnO nanocomposite particle and preparation method thereof - Google Patents
PVP modified magnetic-fluorescent core-shell La1-xSrxMnO3 / ZnO nanocomposite particle and preparation method thereof Download PDFInfo
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Abstract
The present invention belongs to the field of bio-medicine materials, and in particular relates to a PVP modified magnetic-fluorescent core-shell La1-xSrxMnO3 / ZnO nanocomposite particle and preparation method thereof. La1-xSrxMnO3 is used as a core, and ZnO is used as a shell; the shell surface is modified by a surfactant PVP; x satisfies the relation of: 0.1<=x<=0.8; the core diameter is 20-80 nm; and the shell thickness is 5-10nm. A preparation method is as below: under the effect of the surfactant PVP, a two-step continuous reaction is conducted to prepare the La1-xSrxMnO3 / ZnO nanocomposite particle. The nanocomposite particle prepared by the invention has excellent biocompatibility, chemical stability, magnetic properties, optical absorption performance and fluorescent activity, and has wide range of application in magnetic hyperthermia, drug delivery and release, biosensors and immunodiagnosis.
Description
Technical field
The invention belongs to biological medicine Material Field, modify magnetic-fluorescent core shell mould La particularly to a kind of PVP1-xSrxMnO3/ ZnO nano compound particle and preparation method thereof.
Background technology
Proposing magnetic thermotherapy concept from nineteen fifty-seven Gilchrist and prove that magnetic medium can be in calandria under alternating magnetic field after tumor tissues, magnetic thermotherapy just becomes a kind of oncotherapy new way with good prospect.Magnetic medium is mainly positioned tumor tissues by magnetic thermotherapy, then applies alternating magnetic field in outside, makes magnetic medium produce magnetic hysteresis, relaxation or inductive loop and be heated.These heats are delivered in periphery tumor tissues, by controlling the conditions such as the local concentration of alternating magnetic field intensity, magnetic-particle, make tumor tissues temperature reach and control in the range of 42-46 DEG C.Relative to traditional thermotherapy method, magnetic technique for hyperthermia has can treat deep tumor, targeting is high, side effect is little, the most noninvasive advantage of Wicresoft.
Magnetic nanoparticle is usually ferrum, nickel, cobalt or its alloy or its oxide etc..Owing to nickel, cobalt etc. exist certain toxicity, it is impossible to be widely used in fields such as biological medicines.Ferric oxide nano particles, that representative is Fe3O4With γ-Fe2O3Can be stored by degraded in tissue or excrete, there is good biological safety, it is expected to be applied to magnetic thermotherapy, but owing to their Curie temperature (Tc is at 773 more than K) is too high, after heating temperature can not automatic control, in magnetic hyperthermia process must by implant thermometer control heat up to avoid damage to organize normally.
La1-xSrxMnO3(0.175≤χ≤0.8) is that paramagnetic temperature (referred to as Curie temperature) scope 283-370 K is the widest from ferromagnetic transition, by changing the amount of mixing of Sr, Curie temperature can be regulated, at below Curie temperature Tc, LSMO nanoparticle display ferrum or the behavior Han ferromagnetism, during higher than this temperature, they are changing to paramagnetism, disappear when temperature is raised to Curie temperature above LSMO nanoparticle magnetic hysteresis, it is no longer heat up, there is the heating mechanism of itself controllable, do not have hot-spot and destroy health tissues around, there is in terms of the thermotherapy of tumor huge application potential.So far, LSMO nanoparticle has obtained studying the most widely, but the synthetic method of routine often complex steps, severe reaction conditions, the LSMO nano particle diameter size of preparation is uneven, and easily reunites.Time in vivo with medical applications, the size of nanoparticle and the accurately control of particle size distribution determine that the physical property of nanoparticle and the key factor of pharmacokinetic profile.Thus, the LSMO nano-particle synthesizing preferable uniform-dimension is still a difficult problem.Simultaneously, having good diffusibility and biocompatibility in aqueous phase is also to formulate synthesis at present and process the Critical policies of LSMO nano material, although processed diffusibility and the biocompatibility that can improve LSMO nano-particle by follow-up surface, but complex steps adds the pollution to environment simultaneously, do not meet the application for biomedicine requirement to green syt.The nanoparticle that preparation has that size is homogeneous, magnetic property is excellent, diffusibility in biocompatibility and aqueous phase is good is still the developing direction of the nano material of research LSMO, and prepare nano-complex particle based on LSMO, give its special physics and chemical characteristic, expand the powerful measure of its range especially, be also the study hotspot of current LSMO nano material.
Summary of the invention
It is an object of the invention to provide a kind of PVP and modify magnetic-fluorescent core shell mould La1-xSrxMnO3/ ZnO nano compound particle, this compound particle has biocompatibility, chemical stability, magnetic performance, absorbing properties and the fluorescence activity of excellence simultaneously, and in magnetic thermotherapy, medicine conveying and release, the field such as biosensor and immunologic diagnosis is widely used.
For achieving the above object, the technical scheme that the present invention takes is as follows:
PVP modifies magnetic-fluorescent core shell mould La1-xSrxMnO3/ ZnO nano compound particle: with La1-xSrxMnO3For core, with ZnO as shell, shell surface is modified with surfactant PVP；Wherein, 0.1≤χ≤0.8, nuclear diameter 20-80 nm, thickness of the shell 5-10 nm.
Preparation method: under the effect of surfactant PVP, prepares La by two step successive reactions1-xSrxMnO3/ ZnO nano compound particle.
Specifically: under (1) stirring, by the presoma of tri-kinds of metals of La, Sr and Mn and surfactant PVP and reducing agent 1,2-hexadecane diol mixes in solvent octyl ether, in 2 h, heat the mixture to 80-150 DEG C and be incubated 1-2 h, in 10 min, be warmed up to 250-300 DEG C afterwards and be incubated 48-72 h；(2) after the reactant liquor until (1) is cooled to room temperature, lower presoma and the surfactant PVP adding Zn of stirring, in 15 min, it is heated to 80-150 DEG C and is incubated 0.5-2 h, be warmed up in 15 min afterwards 250-300 DEG C and be incubated 1-5 h complete reaction, separating, wash, dry, 600-1000 DEG C of sintering 2-8 h obtains target product.
Preferably, the presoma of La is lanthanum acetylacetone or lanthanum acetate, and the presoma of Sr is acetylacetone,2,4-pentanedione strontium or strontium acetate, and the presoma of Mn is manganese acetylacetonate or manganese acetate, and the presoma of Zn is zinc acetylacetonate or zinc acetate.
Preferably, in step (1), the mol ratio of the presoma of La, Sr and Mn is measured by La Sr Mn=1-x x 1, it is in terms of 1 mmol by total consumption of La, Sr and Mn presoma, the consumption of 1,2-hexadecane diol is 0.1-10 mmol, and the consumption of PVP is 0.001-1 mmol；In step (2), counting with the consumption of Zn presoma for 1mmol, the consumption of PVP is 0-1mmol；The consumption of octyl ether i.e. guarantees to dissolve all reaction raw materials for dissolving equivalent.
The present invention first with polyvinylpyrrolidone (PVP) as surfactant, in nanoemulsions, prepare magnetic-fluorescent core shell mould La with metal complex for presoma by two step successive reactions1-xSrxMnO3/ ZnO nano compound particle.Select polyvinylpyrrolidone (PVP) be surfactant be the key preparing the LSMO Nano composite granules having good diffusion, biocompatibility good in uniform particle sizes, aqueous phase.Polyvinylpyrrolidone (polyvinyl pyrrolidone) is called for short PVP, is a kind of non-ionic macromolecule compound, and tasteless, low toxicity has excellent physiological inertia and biocompatibility, thus is widely used in biological medicine, pharmaceutical field.PVP is a kind of amphiphilic macromolecular, and hydrophilic and lipophile are the strongest.Therefore PVP is often widely used as surfactant.Selecting polyvinylpyrrolidone (PVP) is that magnetic-fluorescent core shell mould La prepared by surfactant1-xSrxMnO3/ ZnO nano compound particle; PVP molecule hydrophobic inner core is the nucleation of nanoparticle and growth provides a stable micro-reaction environment i.e. nanometer microreactor; PVP molecular modification in nanoparticle surface as stabilizer and protective agent; can effectively prevent particle coacervation or precipitation, PVP molecular hydrophylic makes nanoparticle can stably be present in aqueous solution or body fluid.PVP can be combined with other compounds containing active hydrogen atom such as a lot of hydroxyls, amino, sulfydryl, beneficially nanoparticle and the coupling of bioactive molecule.Therefore, the magnetic of synthesis-fluorescence La1-xSrxMnO3/ ZnO nano compound particle need not follow-up surface and modifies, and just can directly be diffused in aqueous phase and have good biocompatibility.
ZnO shell imparts biocompatibility, chemical stability, antibiotic property, absorbing properties and the fluorescence activity that LSMO magnetic nano-particle is unique.Nano-ZnO is a kind of important II-VI group direct band gap semiconductor material with wide forbidden band.Nano-ZnO has special optics and fluorescence activity, has been widely used in biosensor, medicine, catalysis material and medicine and other fields.Additionally, nano-ZnO exists stimulated emission and band edge luminescence is very strong at blue, bluish-green visible and ultraviolet band, it it is the luminescent material having very much potential value.Magnetic-fluorescent core shell mould La is prepared for shell parcel LSMO magnetic nano-particle with ZnO1-xSrxMnO3/ ZnO nano compound particle can widen the range of application of nanoparticle significantly.
PVP prepared by the present invention modifies magnetic-fluorescent core shell mould La1-xSrxMnO3/ ZnO nano compound particle has the advantage that
1) have magnetics and fluorescence property concurrently simultaneously；
2) aqueous phase has good diffusibility；
3) narrow diameter distribution, degree of crystallinity is high, composition and size controllable, ZnO shell thickness is adjustable；
4) bio-compatible excellent (PVP has excellent biocompatibility)；
5) easily and bioactive molecule coupling (character based on PVP)；
Relative to prior art, beneficial effects of the present invention is embodied in:
1, preparation method of the present invention is simple, and reaction condition is gentle, and solvent for use is environmentally friendly, it is simple to industrialized production, separately processes without follow-up surface, and environmental pollution is little, is a kind of green syt scheme.
2, the PVP that prepared by the present invention modifies magnetic-fluorescent core shell mould La1-xSrxMnO3/ ZnO nano compound particle, solves existing LSMO nanoparticle aqueous phase diffusibility and the problem of poor biocompatibility, gives bio-compatible performance, absorbing properties and the fluorescence activity that LSMO nanoparticle is excellent simultaneously.PVP modifies magnetic-fluorescence La1-xSrxMnO3/ ZnO nano compound particle has biocompatibility, chemical stability, magnetic performance, absorbing properties and the fluorescence activity of excellence simultaneously, and in magnetic thermotherapy, medicine conveying and release, the field such as biosensor and immunologic diagnosis is widely used.
Accompanying drawing explanation
Fig. 1 is that the PVP that embodiment 1 prepares modifies magnetic-fluorescence La1-xSrxMnO3The XRD figure spectrum of/ZnO nano compound particle.
Fig. 2 is that the PVP that embodiment 1 prepares modifies magnetic-fluorescence La1-xSrxMnO3The TEM photo of/ZnO nano compound particle.
Fig. 3 is that the PVP that embodiment 1 prepares modifies magnetic-fluorescence La1-xSrxMnO3/ ZnO nano compound particle (b) and PVP(a) infrared spectrum comparison diagram.
Fig. 4 is that the PVP that embodiment 1 prepares modifies magnetic-fluorescence La1-xSrxMnO3The UV-Vis collection of illustrative plates that/ZnO nano compound particle is diffused in water.
Fig. 5 is that the PVP that embodiment 1 prepares modifies magnetic-fluorescence La1-xSrxMnO3/ ZnO nano compound particle is diffused in the fluorescence spectrum in water.
Fig. 6 is that the PVP that embodiment 1 prepares modifies magnetic-fluorescence La1-xSrxMnO3/ ZnO nano the compound particle hysteresis curve when 300K.
Detailed description of the invention
With specific embodiment, technical scheme is described below, but protection scope of the present invention is not limited to this.
Embodiment 1
1) by polyvinylpyrrolidone (PVP) (0.009 mmol in 250 ml there-necked flasks, 0.5 g), lanthanum acetylacetone (1.3500 mmol, 0.5889 g), acetylacetone,2,4-pentanedione strontium (0.4498 mmol, 0.1285 g), manganese acetylacetonate (1.7998 mmol, 0.6340g) three kinds of presomas, 1, (1.504 mmol, 0.3887 g) and octyl ether (C for 2-hexadecane diol8H17OC8H17,
95%) (100 ml) magnetic agitation uniformly mixes, and the mixture obtained is heated in 2 h 120 DEG C and is incubated 2 h, afterwards in 10 min within be brought rapidly up 280 DEG C and be incubated 72 h.
2) during parcel ZnO shell, treat 1) mixture that obtains is cooled to room temperature and adds zinc acetylacetonate (5 mmol, 1.3168 g) and polyvinylpyrrolidone (PVP) (0.009 mmol, 0.5 g), heat the mixture to 120 DEG C under magnetic agitation within 10 min and be incubated 1 h, be brought rapidly up within afterwards in 15 min 280 DEG C and be incubated 1 h complete reaction, separate, wash, dry, gained nano-particle 600 DEG C sintering 3 h prepare PVP modify hud typed La1-xSrxMnO3/ ZnO nano compound particle.
The PVP obtained modifies hud typed La1-xSrxMnO3Structure and the performance of/ZnO nano compound particle are shown in Fig. 1-5.
Fig. 1 is the XRD figure spectrum of the nano-complex particle that embodiment 1 prepares.XRD diffracting spectrum shows the La formed1-xSrxMnO3/ ZnO nano compound particle degree of crystallinity is higher.It is observed that belong to La in XRD figure spectrum1-xSrxMnO3Diffraction maximum with ZnO: stronger diffraction maximum at 31.769 °, 34.421 °, 36.252 °, 47.538 °, 56.602 °, 62.862 °, 66.593 °, 67.961 ° and 69.184 °, corresponding to (100), (002), (101), (102), (110), (103), (200), (112) and (201) crystal face of hexagonal crystal system ZnO；Weak diffraction maximum at 32.576 °, 40.447 °, 46.776 °, 58.386 °, 72.773 °, 77.173 ° and 81.573 ° simultaneously, corresponding to rhombus La0.8Sr0.2MnO3(104), (006), (024), (018), (306), (134) and (042) crystal face.XRD figure analysis of spectrum indicates La1-xSrxMnO3The coreshell type structure of/ZnO nano compound particle.
Fig. 2 is the TEM photo of the nano-complex particle that embodiment 1 prepares.Can be seen that nano particle diameter prepared by embodiment 1 is evenly distributed from Fig. 2, size is about 70 nm, wherein nuclear diameter 59 nm, thickness of the shell 6 nm.
Fig. 3 is infrared spectrum (b) and the PVP(a of the nano-complex particle that embodiment 1 prepares) infrared spectrum comparison diagram.Understand by contrast: b in Fig. 3, it is observed that C=O and the C-N stretching vibration peak of PVP, illustrates that nano-complex particle surface exists PVP.
Fig. 4 is that nano-complex particle 10 mg that embodiment 1 prepares is diffused in 100 ml water UV, visible light (UV-Vis) spectrum obtained.As can be seen from Figure 4 La1-xSrxMnO3/ ZnO nano compound particle has obvious absworption peak at 365 nm, shows the characteristic absorption of nano-ZnO structure, simultaneously it is observed that La at 446 nm1-xSrxMnO3Middle Mn3+D-d transition absorption, due to parcel and the La of ZnO shell1-xSrxMnO3And the interaction between ZnO, La1-xSrxMnO3Absworption peak wider.La1-xSrxMnO3The uv-vis spectra that/ZnO nano compound particle is diffused in water illustrates La1-xSrxMnO3The coreshell type structure of/ZnO nano compound particle, shows that this nanoparticle has good diffusibility in water simultaneously.
Fig. 5 is that nano-complex particle 10 mg that embodiment 1 prepares is diffused in 100 ml water, at room temperature uses the light of xenon lamp 380 nm wavelength to excite, produced fluorescence emission spectrum.From Fig. 5 it is observed that have obvious emission peak at 442 nm, 467 nm, 480 nm and 553 nm, La is described1-xSrxMnO3/ ZnO nano compound particle has good fluorescence activity.
Fig. 6 is the embodiment 1 prepared nano-complex particle hysteresis curve when 300K, it can be observed that La1-xSrxMnO3Nano-complex particle shows superparamagnetism when 300K.
Hud typed La prepared by Fig. 4,5, the 6 explanation present invention1-xSrxMnO3Nano-complex particle has diffusion good in optical absorption, fluorescent emission, magnetic performance and the water of excellence concurrently.
Embodiment 2
1) by polyvinylpyrrolidone (PVP) (0.09 mmol in 500 ml there-necked flasks, 5 g), lanthanum acetylacetone (0.8993 mmol, 0.3923 g), acetylacetone,2,4-pentanedione strontium (0.9026 mmol, 0.2580 g), manganese acetylacetonate (1.7998 mmol, 0.6340g) three kinds of presomas, 1, (1.504 mmol, 0.3887 g) and octyl ether (C for 2-hexadecane diol8H17OC8H17,
95%) (300 ml) magnetic agitation uniformly mixes, and the mixture obtained is heated in 2 h 150 DEG C and is incubated 2 h, afterwards in 10 min within be brought rapidly up 280 DEG C and be incubated 50 h.
2) during parcel ZnO shell, treat 1) mixture that obtains is cooled to room temperature and adds zinc acetylacetonate (5 mmol, 1.3168 g) and polyvinylpyrrolidone (PVP) (0.09 mmol, 5 g), magnetic agitation heats the mixture to 150 DEG C and is incubated 1 h within lower 10 minutes, being brought rapidly up 280 DEG C within afterwards in 15 min and be incubated 3 h and complete reaction, separating, wash, dry, gained nano-particle prepares, at 800 DEG C of sintering 5 h, PVP that mean diameter is 48 nm and modifies hud typed La1-xSrxMnO3/ ZnO nano compound particle.
Embodiment 3
1) by polyvinylpyrrolidone (PVP) (0.009 mmol in 250 ml there-necked flasks, 0.5 g), lanthanum acetylacetone (1.5789 mmol, 0.5248 g), acetylacetone,2,4-pentanedione strontium (2.0207 mmol, 0.5794 g), manganese acetylacetonate (3.5996 mmol, 1.2580 g) three kinds of presomas, 1, (3.008 mmol, 0.7774 g) and octyl ether (C for 2-hexadecane diol8H17OC8H17,
95%) (150 ml) magnetic agitation uniformly mixes, and the mixture obtained is heated in 2 h 80 DEG C and is incubated 2 h, afterwards in 10 min within be brought rapidly up 290 DEG C and be incubated 62 h.
2) during parcel ZnO shell, treat 1) mixture that obtains is cooled to room temperature and adds zinc acetylacetonate (10 mmol, 2.6336 g) and polyvinylpyrrolidone (PVP) (0.009 mmol, 0.5 g), magnetic agitation heats the mixture to 80 DEG C and is incubated 1 h within lower 10 minutes, be brought rapidly up within afterwards in 15 min 290 DEG C and be incubated 5 h complete reaction, separating, wash, dry, it is that 80 nm PVP modify hud typed La that gained nano-particle prepares mean diameter at 600 DEG C of sintering 8 h1-xSrxMnO3/ ZnO nano compound particle.
Above-described embodiment is the preferred embodiment of the present invention, but embodiments of the present invention being not restricted to the described embodiments, other any change made without departing from the present invention all should be the substitute mode of equivalence, within being included in protection scope of the present invention.
Claims (5)
1.PVP modifies magnetic-fluorescent core shell mould La1-xSrxMnO3/ ZnO nano compound particle, it is characterised in that: with La1-xSrxMnO3For core, with ZnO as shell, shell surface is modified with surfactant PVP；Wherein, 0.1≤χ≤0.8, nuclear diameter 20-80 nm, thickness of the shell 5-10 nm.
2. prepare PVP as claimed in claim 1 and modify magnetic-fluorescent core shell mould La1-xSrxMnO3The method of/ZnO nano compound particle, it is characterised in that under the effect of surfactant PVP, prepares La by two step successive reactions1-xSrxMnO3/ ZnO nano compound particle.
3. preparation method as claimed in claim 2, it is characterized in that described two step successive reactions are: under (1) stirring, by the presoma of tri-kinds of metals of La, Sr and Mn and surfactant PVP and reducing agent 1,2-hexadecane diol mixes in solvent octyl ether, in 2 h, heat the mixture to 80-150 DEG C and be incubated 1-2 h, in 10 min, be warmed up to 250-300 DEG C afterwards and be incubated 48-72 h；(2) after the reactant liquor until (1) is cooled to room temperature, lower presoma and the surfactant PVP adding Zn of stirring, in 15 min, it is heated to 80-150 DEG C and is incubated 0.5-2 h, be warmed up in 15 min afterwards 250-300 DEG C and be incubated 1-5 h complete reaction, separating, wash, dry, 600-1000 DEG C of sintering 2-8 h obtains target product.
4. preparation method as claimed in claim 3, it is characterized in that: the presoma of La is lanthanum acetylacetone or lanthanum acetate, the presoma of Sr is acetylacetone,2,4-pentanedione strontium or strontium acetate, and the presoma of Mn is manganese acetylacetonate or manganese acetate, and the presoma of Zn is zinc acetylacetonate or zinc acetate.
5. the preparation method as described in claim 3 or 4, it is characterized in that: in step (1), the mol ratio of the presoma of La, Sr and Mn is measured by La Sr Mn=1-x x 1, it is in terms of 1 mmol by total consumption of La, Sr and Mn presoma, 1, the consumption of 2-hexadecane diol is 0.1-10 mmol, and the consumption of PVP is 0.001-1 mmol；In step (2), counting with the consumption of Zn presoma for 1mmol, the consumption of PVP is 0-1mmol；The consumption of octyl ether is for dissolving equivalent.
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| CN101055895A (en) * | 2007-05-11 | 2007-10-17 | 北京工业大学 | CaTiO3 structure La-Mn oxide/zinc oxide heterogeneous p-n junction and its making method |
| US20110151255A1 (en) * | 2009-12-23 | 2011-06-23 | Korea Institute Of Science And Technology | Nanofiber and preparation method thereof |
| US20130243699A1 (en) * | 2011-12-07 | 2013-09-19 | Regents Of The University Of Minnesota | Biodegradable Magnetic Nanoparticles and Related Methods |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101055895A (en) * | 2007-05-11 | 2007-10-17 | 北京工业大学 | CaTiO3 structure La-Mn oxide/zinc oxide heterogeneous p-n junction and its making method |
| US20110151255A1 (en) * | 2009-12-23 | 2011-06-23 | Korea Institute Of Science And Technology | Nanofiber and preparation method thereof |
| US20130243699A1 (en) * | 2011-12-07 | 2013-09-19 | Regents Of The University Of Minnesota | Biodegradable Magnetic Nanoparticles and Related Methods |
Non-Patent Citations (2)
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| MICHAL KACENKA，等: "Dual imaging probes for magnetic resonance imaging and fluorescence microscopy based on perovskite manganite nanoparticles", 《J. MATER. CHEM.》 * |
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