CN102294039A - Preparation method of yolk-eggshell nanocapsule with fluorescence and magnetism - Google Patents
Preparation method of yolk-eggshell nanocapsule with fluorescence and magnetism Download PDFInfo
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- CN102294039A CN102294039A CN2011102410346A CN201110241034A CN102294039A CN 102294039 A CN102294039 A CN 102294039A CN 2011102410346 A CN2011102410346 A CN 2011102410346A CN 201110241034 A CN201110241034 A CN 201110241034A CN 102294039 A CN102294039 A CN 102294039A
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Abstract
The invention belongs to the filed of nanocomposite, in particular to a preparation method of yolk-eggshell nanocapsules with fluorescence and magnetism. Firstly, SPIO (Super Paramagnetic Iron Oxide) nanoparticles protected by hexadecyl trimethyl ammonium bromide molecules are prepared, then a silicon dioxide shell is formed on the outer layers of the nanoparticles with a sol-gel method, the thickness of the silicon dioxide shell can be adjusted through the addition of tetraethoxysilane. The outer layer of the silicon dioxide shell is wrapped with red fluorescent Y203:Eu, in this process, silicon dioxide is etched, thermal decomposition of urea thereof causes the solution thereof to be alkaline, OH- is used to etch the silicon dioxide, then centrifugation, drying and high-temperature calcination are performed, and finally, the nanocapsules with yolk-eggshell structures are formed. The method can realize the precise control of the magnetic performance, fluorescent performance, size of an internal cavity and shell thickness. Meanwhile, the obtained nanoparticles are good in dispersity and are uniform in size, and are suitable for the fields of biochemistry, clinical medicine and the like. The invention is simple, fast, safe, convenient in operation and good in repeatability, and has generality.
Description
Technical field
The invention belongs to field of nanocomposite materials, be specifically related to have concurrently the difunctional egg yolk-capsular preparation method of eggshell structure nano of fluorescence and magnetic.
Background technology
In recent years, the oxide of superparamagnetism ferrum (SPIO) nano-particle is owing to have special magnetic conductance tropism and an excellent biological compatibility, more and more causes people's attention at the applied research of biological field.In cancer, all there is the research report aspects such as the targeted therapy of diseases such as acquired immune deficiency syndrome (AIDS), bio-separation, enzyme or proteinic fixing, cell screening, nucleic acid purification and bio-sensing, sewage disposal.The magnetic particle more function is given in other nanoparticles and magnetic particle combination that people's expectation will have specific function, because rare earth oxide has unique optical property, the wherein rare earth oxide (Y of europium doped
2O
3: Eu) have very strong red fluorescence, has purposes very widely at aspects such as molecular marker, bio-imaging, ion detection, therefore have the dual-function nano particle of the high magnetic response performance of the optical property of rare-earth europium excellence and SPIO simultaneously, have potential significant application value aspect biological targeting labelling, cell separation and screening, medical diagnosis on disease and the treatment.In addition, be material of main part with the mesoporous silicon oxide, in conjunction with the guest materials of difference in functionality, can produce abundant Subjective and Objective effect.Wherein, preparation SPIO nano-particle is an egg yolk, red fluorescence Y
2O
3: Eu is the fluorescence and the difunctional SPIOY of superparamagnetism of eggshell
2O
3: the Eu composite, both had the separable character of magnetic, have the imageable character of fluorescence again, except field large-scale application such as separation, detection, imaging, this material also will be in more wider its potentiality of fields performance.(list of references: Zhang, F.; Braun, G, B.; Shi, Y, F.; Zhang, Y, C.; Sun, X, H.; Reich, N, O.; Zhao, D, Y.; Stucky, G., Fabrication of AgSiO
2Y
2O
3: Ernanostructures for bioimaging:tuning of the upconversion fluorescence with silver nanoparticles, J.Am.Chem.Soc.2010,132,2850-2851.).The nano-particle of this egg yolk-eggshell structure, outer shell Y
2O
3: the thickness of Eu can be regulated and control by the amount that adds different rare earth compound presomas in the reaction, and the big I in the space of internal cavity is by regulating and control by the thickness that changes silicon dioxide.At present, this difunctional SPIOY that has fluorescence and magnetic concurrently of preparation
2O
3: Eu egg yolk-capsular method of eggshell structure nano rarely has report, and therefore, the present invention proposes a kind of simple, general, difunctional SPIOY that is specifically related to have concurrently fluorescence and magnetic that controlled dimensions is big or small
2O
3: the Eu egg yolk-capsular preparation method of eggshell structure nano.
Summary of the invention
The purpose of this invention is to provide a kind of difunctional SPIOY that has fluorescence and magnetic concurrently
2O
3: the Eu egg yolk-capsular preparation method of eggshell structure nano, synthetic method is simple, and is easy to operate, has regulatable internal cavity space size and outer casing thickness, can be used as the contrast medium of the double mode imaging of cancer (fluorescence imaging and nuclear magnetic resonance) diagnosis.
The present invention's preparation is an egg yolk to have superparamagnetism SPIO nanoparticle, outer layer thickness and internal cavity space adjustable size and the Y with red fluorescence character
2O
3: Eu is the Nano capsule of eggshell.
The solution of the present invention is: at first, the SPIO nano-particle of preparation cetyl trimethyl ammonium bromide (CTAB) molecule protection utilizes sol-gel process at its outer silica shell that forms then, and thickness can be by adding the amount regulation and control of ester (TEOS) of positive silicic acid.Afterwards, outside silica shell, coat Y with red fluorescence
2O
3: Eu, its thickness can be by adding the amount regulation and control of different rare earth compound presomas.Be accompanied by being etched of silicon dioxide in this process, its carbamide thermal decomposition makes its solution present alkalescence, the OH-etching silicon dioxide, and centrifugal then, dry, high-temperature calcination form the Nano capsule of egg yolk-eggshell structure at last.
Purpose of the present invention realizes by following proposal:
A kind of difunctional SPIOY that has fluorescence and magnetic concurrently
2O
3: the Eu egg yolk-capsular preparation method of eggshell structure nano comprises the steps:
One, the SPIO nano-particle of CTAB protection: get the SPIO nano-particle that the oleic acid protection is of a size of 25nm, list of references (list of references: Kim, J.; Kim, H.S.; Lee, N.; Kim, T.; Kim, H.; Yu, T.; Song, I.C.; Moon, W.K.; Hyeon; T.; Multifunctional uniform nanoparticles composed of a magnetite nanocrystal core and a mesoporous silica shell for magnetic resonance and fluorescence imaging and for drug delivery; Angew.Chem.Int.Ed.2008; 47,8438-8441) be converted into the SPIO nano-particle that CTAB protects.
Two, mesoporous silicon oxide coats the preparation method of SPIO nano-particle: the SPIO nano-particle of getting above-mentioned CTAB protection; be dispersed in the deionized water; the pH value that adds the NaOH solution regulator solution of 0.1M is 9～10; the positive silicic acid that adds 200～500 μ L 20% is the alcoholic solution of ester (TEOS); wherein the per 20～30min of the alcoholic solution of TEOS adds once, divides 4～10 addings.Then, mixed solution is continued to stir 24～36h down at 30～35 ℃.After reaction is finished, clean 5～7 times, remove unreacted matters and Surfactant CTAB molecule fully with ethanol.At last with the SPIOmSiO that makes
2Nanoparticulate dispersed stores for future use in ethanol.
Three, have the difunctional SPIOY of fluorescence and magnetic concurrently
2O
3: the Eu egg yolk-capsular preparation method of eggshell structure nano: with the product 1mL SPIOmSiO of step 2
2Nano-particle joins in the alcohol mixed solution of the water of 20mL and 20mL, and with 0.54～1.08g carbamide, 475～950 μ L Y (NO
3)
3, 25～50 μ L Eu (NO
3)
3The ultrasonic 20～30min of aqueous solution, restir 20min packs mixed solution after the politef reactor sealing of 50mL into, puts into baking oven, reacts 12～36h under 160～180 ℃ of conditions.With solution centrifugal, use washed with de-ionized water 2～3 times then, clean 2～3 times, obtain egg yolk-capsular predecessor of eggshell structure nano with ethanol.Afterwards, dry 6～10h in 60～80 ℃ of baking ovens is at last at 500～700 ℃ of heating 2～3h.Obtain having concurrently the difunctional SPIOY of fluorescence and magnetic this moment
2O
3: the Nano capsule of Eu egg yolk-eggshell structure.
The size of the SPIO nano-particle of the oleic acid protection in the described step 1 is about 25nm.
Obtaining with the SPIO nano-particle by method for preparing is egg yolk, the Y of photoluminescent property
2O
3: Eu is the Nano capsule of eggshell.
This Nano capsule is evenly distributed, good dispersion, and present red fluorescence and superparamagnetism simultaneously.The present invention has following advantage:
1, the synthetic first difunctional SPIOY that has fluorescence and magnetic concurrently of the present invention
2O
3: the Nano capsule of Eu egg yolk-eggshell structure.
2, the inventive method is simple, fast, safety, easy to operate, good reproducibility has versatility.
3, the nanoparticulate dispersed that obtains of the present invention is good, Stability Analysis of Structures, and can regulate and control internal cavity size and shell thickness between egg yolk and the eggshell according to needs, promptly to regulate and control its fluorescence and magnetic saturation intensity.
4, SPIOY of the present invention
2O
3: the Nano capsule of Eu egg yolk-eggshell structure combines egg yolk and two kinds of functions of eggshell, make it both have the separation function of superparamagnetism, also have the fluorescent tracing function, have excellent biological compatibility simultaneously, can be applicable to fields such as cell separation, fluorescent labeling and medical diagnosis.
5, etching silicon dioxide of the present invention with wrap the 3rd layer of Y with red fluorescence
2O
3: Eu finishes in step experiment and obtains, and has simplified experimental procedure, directly can obtain SPIOY
2O
3: Eu egg yolk-eggshell Nano capsule structure, improved synthetic efficient.
The invention provides the SPIOY of New-type bifunctional
2O
3: the controllable method for preparing of the Nano capsule of Eu egg yolk-eggshell structure, can realize the accurately controlled of the size of its magnetic property, fluorescence property, internal cavities and outer casing thickness.The nanoparticulate dispersed that obtains simultaneously is good, the size homogeneous, both can be used for fluoroscopic examination, can realize product separation and orientation again, is applicable to fields such as biochemistry, molecular biology, clinical medicine.
Description of drawings
Accompanying drawing 1, the silicon dioxide thickness for preparing for the present invention are the transmission electron microscope picture of the SPIO nano-particle that coats of the mesoporous silicon oxide of 10 ± 2nm;
Accompanying drawing 2, the internal cavity size for preparing for the present invention are that 43 ± 2nm, shell thickness are the difunctional SPIOY that has fluorescence and magnetic concurrently of 19 ± 2nm
2O
3: the Eu egg yolk-capsular transmission electron microscope picture of eggshell structure nano;
Accompanying drawing 3, the silicon dioxide thickness for preparing for the present invention are the transmission electron microscope picture of SPIO nano-particle of the mesoporous silicon oxide parcel of 20 ± 2nm;
Accompanying drawing 4, the internal cavity size for preparing for the present invention are that 63 ± 2nm, shell thickness are the difunctional SPIOY that has fluorescence and magnetic concurrently of 19 ± 2nm
2O
3: the Eu egg yolk-capsular transmission electron microscope picture of eggshell structure nano;
Accompanying drawing 5, the internal cavity size for preparing for the present invention are that 63 ± 2nm, shell thickness are the difunctional SPIOY that has fluorescence and magnetic concurrently of 26 ± 2nm
2O
3: the Eu egg yolk-capsular transmission electron microscope picture of eggshell structure nano;
Accompanying drawing 6, the difunctional SPIOY that has fluorescence and magnetic concurrently for preparing for the present invention
2O
3: the Eu egg yolk-capsular fluorogram of eggshell structure nano, wherein A is that the Nano capsule of accompanying drawing 2, Nano capsule, the C that B is accompanying drawing 4 are the Nano capsule of accompanying drawing 5;
Accompanying drawing 7, the difunctional SPIOY that has fluorescence and magnetic concurrently for preparing for the present invention
2O
3: Eu egg yolk-eggshell structure nano is capsular to have or not the photo that reaches under the externally-applied magnetic field effect under daylight and ultra violet lamp;
The specific embodiment
Embodiment 1:
The internal cavity size is that 43 ± 2nm, shell thickness are the difunctional SPIOY that has fluorescence and magnetic concurrently of 19 ± 2nm
2O
3: the Eu egg yolk-capsular preparation of eggshell structure nano:
(1) the SPIO nano-particle of synthetic CTAB protection: get 400 μ L, 10mg mL
-1The 25nm SPIO nano-particle and the 8mL of oleic acid protection, 0.2M CTAB mixes, concrete list of references (list of references: Kim, J.; Kim, H.S.; Lee, N.; Kim, T.; Kim, H.; Yu, T.; Song, I.C.; Moon, W.K.; Hyeon; T.; Multifunctional uniform nanoparticles composed of a magnetite nanocrystal core and a mesoporous silica shell for magnetic resonance and fluorescence imaging and for drug delivery; Angew.Chem.Int.Ed.2008; 47; 8438-8441), be converted into the SPIO nano-particle of CTAB protection.
(2) thickness is the preparation of the mesoporous silicon oxide shell coating SPIO nano-particle of 10 ± 2nm: the SPIO nano-particle 8mL that gets the CTAB protection of step (1) preparation adds 20mL deionized water and ultra-sonic dispersion.PH value with 0.1M NaOH solution regulator solution is 9, adds 200 μ L then, 20% TEOS alcoholic solution, and wherein TEOS divides 4 addings, the 20min of at every turn being separated by.Mixed solution is continued to stir 24h down for 30 ℃.Centrifugal collection product, and clean 5 times with ethanol.Be that the SPIO core-shell nano that 10 ± 2nm mesoporous silicon oxide shell coats is dispersed in the 4mL ethanol store for future use (accompanying drawing 1) at last with the thickness that makes.
(3) the internal cavity size is that 43 ± 2nm, shell thickness are the difunctional SPIOY that has fluorescence and magnetic concurrently of 19 ± 2nm
2O
3: Eu egg yolk-eggshell structure nano capsule preparation: the SPIOmSiO that gets step (2) preparation
2Nano-particle 1mL, 0.1M, 475 μ L Y (NO
3)
3, 0.1M, 25 μ L Eu (NO
3)
3Join in 20mL deionized water and the 20mL alcohol mixed solution with 0.54g carbamide, ultrasonic 20min, restir 20min after the politef reactor sealing of the 50mL that then mixed solution packed into, puts into baking oven, reacts 12h under 160 ℃ of conditions.With solution centrifugal, use washed with de-ionized water 2 times then, clean 2 times, obtain egg yolk-capsular predecessor of eggshell structure nano with ethanol.Afterwards, dry 10h in 60 ℃ of baking ovens puts into 500 ℃ of heating of tube furnace 2h.Obtaining the internal cavity size at last is that 43 ± 2nm, shell thickness are the difunctional SPIOY that has fluorescence and magnetic concurrently of 19 ± 2nm
2O
3: the Nano capsule of Eu egg yolk-eggshell structure (accompanying drawing 2).
Embodiment 2:
The internal cavity size is that 63 ± 2nm, shell thickness are the difunctional SPIOY that has fluorescence and magnetic concurrently of 19 ± 2nm
2O
3: Eu egg yolk-eggshell structure nano capsule preparation:
(1) the SPIO nano-particle of synthetic CTAB protection: the process of the SPIO nano-particle of preparation CTAB protection is identical among step and the embodiment 1.
(2) thickness is the preparation of the mesoporous silicon oxide shell coating SPIO nano-particle of 20 ± 2nm: the SPIO nano-particle 8mL that gets the CTAB protection of step (1) preparation adds 20mL deionized water and ultra-sonic dispersion.PH value with 0.1M NaOH solution regulator solution is 10, adds 500 μ L then, 20% TEOS alcoholic solution, and wherein TEOS divides 10 addings, the 30min of at every turn being separated by.Mixed solution is continued to stir 36h down for 35 ℃.Centrifugal collection product, and clean 7 times with ethanol.To make thickness at last is the mesoporous silicon oxide shell coating SPIO nano-particle of 20 ± 2nm, and it is dispersed in the 4mL ethanol store for future use (accompanying drawing 3).
(3) the internal cavity size is that 63 ± 2nm, shell thickness are the difunctional SPIOY that has fluorescence and magnetic concurrently of 19 ± 2nm
2O
3: the Eu egg yolk-capsular preparation of eggshell structure nano: the SPIOmSiO that gets step (2) preparation
2Nano-particle 1mL, 0.1M, 475 μ L Y (NO
3)
3, 0.1M, 25 μ L Eu (NO
3)
3Join in 20mL water and the 20mL alcohol mixed solution with 0.864g carbamide, ultrasonic 30min, restir 20min after the politef reactor sealing of the 50mL that then mixed solution packed into, puts into baking oven, reacts 24h under 170 ℃ of conditions.With solution centrifugal, use washed with de-ionized water 2 times then, clean 2 times, obtain egg yolk-capsular predecessor of eggshell structure nano with ethanol.Afterwards, dry 8h in 70 ℃ of baking ovens puts into 600 ℃ of heating of tube furnace 3h.Obtaining the internal cavity size at last is that 63 ± 2nm, shell thickness are the difunctional SPIOY that has fluorescence and magnetic concurrently of 19 ± 2nm
2O
3: the Nano capsule of Eu egg yolk-eggshell structure (accompanying drawing 4).
Embodiment 3:
The internal cavity size is that 63 ± 2nm, shell thickness are the difunctional SPIOY that has fluorescence and magnetic concurrently of 26 ± 2nm
2O
3: the Eu egg yolk-capsular preparation of eggshell structure nano:
(1) the SPIO nano-particle of synthetic CTAB protection: the process of the SPIO nano-particle of preparation CTAB protection is identical among step and the embodiment 1.
(2) thickness is the preparation of the shell coating SPIO nano-particle of 20 ± 2nm mesoporous silicon oxide: prepare SPIOmSiO among step and the embodiment 2
2Process identical.
(3) the internal cavity size is that 63 ± 2nm, shell thickness are the difunctional SPIOY that has fluorescence and magnetic concurrently of 26 ± 2nm
2O
3: the Eu egg yolk-capsular preparation of eggshell structure nano: the SPIOSiO that gets step (2) preparation
2Nano-particle 1mL, 0.1M, 950 μ L Y (NO
3)
3, 0.1M, 50 μ L Eu (NO
3)
3Join in 20mL water and the 20mL alcohol mixed solution with 1.08g carbamide, ultrasonic 30min, restir 20min after the politef reactor sealing of the 50mL that then mixed solution packed into, puts into baking oven, reacts 36h under 180 ℃ of conditions.With solution centrifugal, use washed with de-ionized water 3 times then, clean 3 times, obtain egg yolk-capsular predecessor of eggshell structure nano with ethanol.Afterwards, dry 6h in 80 ℃ of baking ovens puts into 700 ℃ of heating of tube furnace 3h.Obtaining the internal cavity size at last is that 63 ± 2nm, shell thickness are the difunctional SPIOY that has fluorescence and magnetic concurrently of 26 ± 2nm
2O
3: the Nano capsule of Eu egg yolk-eggshell structure (accompanying drawing 5).
Claims (2)
1. have the preparation method of the egg yolk-eggshell Nano capsule of fluorescence and magnetic concurrently, it is characterized in that comprising the steps:
One, the SPIO nano-particle of CTAB protection: get the SPIO nano-particle that the oleic acid protection is of a size of 25nm, press list of references (Kim, J.; Kim, H.S.; Lee, N.; Kim, T.; Kim, H.; Yu, T.; Song, I.C.; Moon, W.K.; Hyeon, T., Multifunctional uniform nanoparticles composed of a magnetite nanocrystal core and a mesoporous silica shell for magnetic resonance and fluorescence imaging and for drug delivery, Angew.Chem.Int.Ed.2008,47,8438-8441) be converted into the SPIO nano-particle that CTAB protects;
Two; mesoporous silicon oxide coats the preparation method of SPIO nano-particle: the SPIO nano-particle of getting above-mentioned CTAB protection; be dispersed in the deionized water; the pH value that adds the NaOH solution regulator solution of 0.1M is 9-10; the positive silicic acid that adds 200-500 μ L 20% is the alcoholic solution of ester (TEOS); wherein the every 20-30min of the alcoholic solution of TEOS adds once; dividing 4-10 time adds; then; mixed solution is continued to stir 24～36h down at 30-35 ℃; after reaction is finished; clean 5-7 time with ethanol, remove unreacted matters and Surfactant CTAB molecule fully, at last with the SPIOmSiO that makes
2Nanoparticulate dispersed stores for future use in ethanol;
Three, have the difunctional SPIOY of fluorescence and magnetic concurrently
2O
3: the Eu egg yolk-capsular preparation method of eggshell structure nano: with the product 1mL SPIOmSiO of step 2
2Nano-particle joins in the alcohol mixed solution of the water of 20mL and 20mL, and with 0.54-1.08g carbamide, 475-950 μ L Y (NO
3)
3, 25-50 μ L Eu (NO
3)
3The ultrasonic 20-30min of aqueous solution, restir 20min packs mixed solution after the politef reactor sealing of 50mL into, put into baking oven, react 12-36h under the 160-180 ℃ of condition,, use washed with de-ionized water 2-3 time then with solution centrifugal, clean 2-3 time with ethanol, obtain egg yolk-capsular predecessor of eggshell structure nano, afterwards, dry 6-10h in 60-80 ℃ of baking oven, at 500-700 ℃ of heating 2-3h, obtain having concurrently the difunctional SPIOY of fluorescence and magnetic this moment at last
2O
3: the Nano capsule of Eu egg yolk-eggshell structure.
2. by the egg yolk that has fluorescence and the magnetic concurrently-eggshell Nano capsule of the described preparation method of claim 1 preparation.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103211767A (en) * | 2013-04-01 | 2013-07-24 | 长春理工大学 | Preparation method of multifunctional eccentric mesoporous silicon dioxide core-shell nano particles |
| CN103589417A (en) * | 2012-08-13 | 2014-02-19 | 展晶科技(深圳)有限公司 | Phosphor, preparation method thereof, and light emitting diode using phosphor |
| CN111228487A (en) * | 2020-01-14 | 2020-06-05 | 同济大学 | Magnetic particle containing graphitized fluorescent carbon dots and having yolk-shell structure, and preparation method and application thereof |
-
2011
- 2011-08-22 CN CN2011102410346A patent/CN102294039A/en active Pending
Non-Patent Citations (4)
| Title |
|---|
| FAN ZHANG ETAL: "Fabrication of Ag@SiO2@Y2O3:Er nanostructures for Bioimaging: Tuning of the Upconversion Fluorescence with Silver Nanoparticles", 《J.AM.CHEM.SOC》 * |
| IVAN GORELIKOV ETAL: "Single-Step Coating of Mesoporous Silica on Cetyltrimethyl Ammonium Bromide-Capped Nanoparticles", 《NANO LETTERS》 * |
| QUNLING FANG ETAL: "Yolk-like Micro/Nanoparticles with superparamagnetic Iron Oxide Cores and Hierarchical Nickel Silicate Shells", 《ADVANCED FUNCTIONAL MATERIALS》 * |
| ZHI YA MA ETAL: "Synthesis and bio-functionalization of multifunctional magnetic Fe3O4@Y2O3:Eu nanocomposites", 《JOURNAL OF MATERIALS CHEMISTRY》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103589417A (en) * | 2012-08-13 | 2014-02-19 | 展晶科技(深圳)有限公司 | Phosphor, preparation method thereof, and light emitting diode using phosphor |
| CN103589417B (en) * | 2012-08-13 | 2015-03-25 | 展晶科技(深圳)有限公司 | Phosphor, preparation method thereof, and light emitting diode using phosphor |
| CN103211767A (en) * | 2013-04-01 | 2013-07-24 | 长春理工大学 | Preparation method of multifunctional eccentric mesoporous silicon dioxide core-shell nano particles |
| CN103211767B (en) * | 2013-04-01 | 2014-10-01 | 长春理工大学 | Preparation method of multifunctional eccentric mesoporous silicon dioxide core-shell nano particles |
| CN111228487A (en) * | 2020-01-14 | 2020-06-05 | 同济大学 | Magnetic particle containing graphitized fluorescent carbon dots and having yolk-shell structure, and preparation method and application thereof |
| CN111228487B (en) * | 2020-01-14 | 2021-09-24 | 同济大学 | Magnetic particle containing graphitized fluorescent carbon dots and having yolk-shell structure, and preparation method and application thereof |
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Application publication date: 20111228 |