CN102676171A - Method for synthesizing amino functionalized rare earth-doped lanthanum fluoride nano fluorescent marker material - Google Patents
Method for synthesizing amino functionalized rare earth-doped lanthanum fluoride nano fluorescent marker material Download PDFInfo
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- CN102676171A CN102676171A CN2011102425267A CN201110242526A CN102676171A CN 102676171 A CN102676171 A CN 102676171A CN 2011102425267 A CN2011102425267 A CN 2011102425267A CN 201110242526 A CN201110242526 A CN 201110242526A CN 102676171 A CN102676171 A CN 102676171A
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Abstract
The invention relates to a method for synthesizing an amino functionalized rare earth-doped lanthanum fluoride nano fluorescent marker material, which comprises the steps of: with phosphorylethanolamine as a surface active agent, mixing sodium fluoride, lanthanum nitrate and rare earth nitrate in distilled water, carrying out heat preservation at the temperature of 30-90 DEG C, and stirring for a period of time, washing and drying to obtain the aminated rare earth-doped lanthanum fluoride nanocrystalline with the component of xLn<3+>-(1-x) LaF3, wherein Ln<3+>=Ce<3+>, Yb<3+>, Er<3+>, Tm<3+>, Ho<3+>, Eu<3+>, Gd<3+>, Tb<3+>, Dy<3+>, Sm<3+>, Nd<3+> and Pr<3+>, and x=0-50mol%. The rare earth-doped LaF3 nano fluorescent marker material prepared by the method has the advantages that the size of nanoparticles can be controlled to be about 5nm, water solubility is good and the surface amino can be used to realize the connection with biomolecule. Furthermore, different rare earth ions can be doped into the nanoparticles, so that the specific fluorescence emission can be realized so that the biological connection can be detected sensitively; and the nano fluorescent marker material prepared by the method has the potential in application in the biological marking field.
Description
Technical field
The present invention relates to a kind of method of inorganic nano fluorescence labeling material of synthesizing water-solubility, especially relate to a kind of preparation method with rear-earth-doped lanthanum fluoride nano fluorescent marker material of amino functional.
Background technology
Inorganic rare earth nanocrystalline in fields such as green illumination light source, nano photoelectronic devices, FPD existing wide purposes, but it is just to receive much concern in several years up to date as the biological marker material.The material that is widely used in the biological mark at present mainly is that organic dye, GFP, rare earth huge legendary turtle compound, the adulterated silica gel of organic chromophores/latex nano-beads, semiconductor-quantum-point and inorganic rare earth are nanocrystalline etc.Wherein, Than other marker material; Inorganic rare earth is nanocrystalline owing to have high photochemical stability, almost non-toxic property, narrow linewidth, comprehensive advantages such as long fluorescence lifetime, high-luminous-efficiency and tunable fluorescent emission wavelength, therefore is generally good at present biological marker material of new generation.In practical application, fluorescence labeling material is required the single dispersion of uniform particles, particle is more little good more under the situation that does not influence luminous efficiency, and has good water-solubility, and these all propose strict requirement to the preparation and the finishing of nano luminescent material.For solve the water-soluble of nano particle and and biomolecules between connectivity problem, need take two-step approach usually, promptly after nano particle is synthetic, carry out the finishing in second step again, this also is a gordian technique of said material practicability.
In recent years; Fluorochemical has than low phonon energy as one type; Stablize the luminous host of physicochemical property and receive people's favor; Wherein rear-earth-doped lanthanum fluoride fluorescent mark nano material is because its good optical property and in the potential application of aspects such as biomarker has caused the common concern of Chinese scholars.At present, it mainly is synthetic through hydrothermal method being used for fluorescently-labeled rear-earth-doped lanthanum fluoride nanocrystalline.Not only resulting nano particle big (being generally 30-50 nm) and have influence on follow-up biological detection analysis efficiency; And, need further to take finishing through methods such as surface silicon alkanisation or colloid electrostatic adhesion organic polymers in order to realize the water-soluble of nano particle.Obviously follow-up surface-functionalized processing has increased synthesis step, and also can have influence on nanocrystalline luminescent properties for the handling again of surface of nano particle, and these factors have all limited the practical application of nano material.To above problem, the present invention is a tensio-active agent with phosphorylethanolamine (AEP), adopts the water miscible rear-earth-doped lanthanum fluoride of low-temperature co-precipitation method one-step synthesis nanocrystalline.This method not only can be controlled the size of nano particle about 5 nm; And the surface amino groups functionalization that can realize nano particle simultaneously is beneficial to nano particle and can be connected with biomolecules; Luminous this connection is detected through doping with rare-earth ions in the nano particle is specific, promptly can be applicable to the fluorescent mark analysis.
Summary of the invention
The objective of the invention is to propose the preparation method of the rear-earth-doped lanthanum fluoride nano fluorescent of a kind of synthetic particle amination little, good water solubility marker material.
The present invention adopts following technical scheme:
1. the method for the rear-earth-doped lanthanum fluoride nano fluorescent marker material of a synthesizing amino functionalization; It is characterized in that: be dissolved in phosphorylethanolamine in the zero(ppm) water and with the pH value of ammoniacal liquor regulator solution; Then, stir and obtain colourless transparent solution to wherein adding Sodium Fluoride; Be added drop-wise in the above-mentioned solution after in addition rare earth nitrate being dissolved in zero(ppm) water; 30-90 ℃ of insulation and stir for some time, adding acetone makes nanocrystalline deposition in this solution then, and carries out spinning; Washing, it is nanocrystalline to obtain amidized rear-earth-doped lanthanum fluoride after the drying.
2. one kind as 1 a described rear-earth-doped lanthanum fluoride preparation of nano crystal, it is characterized in that: selecting phosphorylethanolamine for use is tensio-active agent, and both the nanocrystalline size of may command can realize the amino functional that it is surperficial again.
3. one kind as 1 and 2 described lanthanum fluoride preparation of nano crystal is characterized in that the adding molar weight ratio of reactant:
Lanthanum trinitrate: 1 part;
Sodium Fluoride: 3 ~ 6 parts;
Phosphorylethanolamine: 0.1 ~ 5 part.
4. like a described method of 1-3, resulting rear-earth-doped lanthanum fluoride is nanocrystalline, and its component is: xLn
3+-(1-x) LaF
3, Ln wherein
3+=Ce
3+, Yb
3+, Er
3+, Tm
3+, Ho
3+, Eu
3+, Gd
3+, Tb
3+, Dy
3+, Sm
3+, Nd
3+, Pr
3+, x=0-50 mol%.
5. like a purposes of the resultant amidized rear-earth-doped lanthanum fluoride nano fluorescent marker material of the described preparation method of 1-4, it is characterized in that: be applied to biomarker and detection.Nanocrystalline its surperficial amino that utilizes of rear-earth-doped lanthanum fluoride of preparation gained is connected with biomolecules; Can realize simultaneously specific luminous through the different rare earth ion that mixes in nanocrystalline; Come this biological connection is detected, be applied to fields such as biological mark.
Preparation flow: take by weighing phosphorylethanolamine and be dissolved in the zero(ppm) water; Regulate the pH value with ammoniacal liquor then, then it is dissolved fully toward wherein adding Sodium Fluoride, stirring; Be added drop-wise in the above-mentioned solution after in addition rare earth nitrate being dissolved in zero(ppm) water, under heating condition, continue to stir and insulation for some time.Add acetone precipitation then in this solution and go out nanocrystallinely, spinning with the deposition that obtains water and washing with alcohol several respectively, can obtain rear-earth-doped lanthanum fluoride manocrystalline powders after the drying.
The nanocrystalline sign of amidized rear-earth-doped lanthanum fluoride: detect through X-ray powder diffraction (XRD) experiment and to show that the lanthanum fluoride of preparing is nanocrystalline and be pure six side's phase structures.What transmission electron microscope (TEM) test demonstration obtained is the homodisperse nano particle about 5 nanometers; High-resolution-ration transmission electric-lens (HRTEM) photo can clearly be observed even successive lattice fringe, shows that the nano particle crystallization is better.Show that through FFIR (FTIR) detection nanocrystal surface has the infrared vibration absorption peak corresponding to phosphorylethanolamine clearly: 1085 cm
-1It is stretching vibration absorption peak corresponding to P-O; 2853 cm
-1With 2924 cm
-1Be corresponding to-CH
2-the stretching vibration absorption peak; And 1635 cm
-1Then be corresponding to-NH
2The stretching vibration absorption peak, show that nanocrystal surface has successfully been modified to have gone up amino, so particle also has better water solubility.In addition, in nanocrystalline, can realize needed specific fluorescent emission through the different rare earth ion that mixes.
Can the rear-earth-doped LaF of the water miscible amination of one-step synthesis through the present invention
3Fluorescence labeling material, preparation equipment is simple, synthesis condition is easy to control, good reproducibility, can produce in enormous quantities.The present invention compares with the lanthanum fluoride for preparing both at home and abroad is nanocrystalline, has the particle homogeneous, and size is less; Owing to when synthesizing nanocrystalline, just added phosphorylethanolamine, nano particle has better water solubility simultaneously, and the amino that the surface has can be used for being connected with biomolecules; Can realize specific advantages such as fluorescent emission through the doping different rare earth ions in addition, therefore promise to be a kind of novel nano fluorescent marker material, be applied to fluoroimmunoassay and bio-imaging.
Description of drawings
Accompanying drawing 1: nanocrystalline X-ray powder diffraction figure.
Accompanying drawing 2: (a) nanocrystalline transmission electron microscope picture; (b) nanocrystalline high-resolution-ration transmission electric-lens figure; (c) the nanocrystalline aqueous solution.
Accompanying drawing 3: nanocrystalline FFIR figure.
Accompanying drawing 4: the structure iron that surface amination is nanocrystalline.
Accompanying drawing 5: (a) LaF
3: 2%Eu reaches (b) LaF
3: 15%Ce, nanocrystalline fluorescence spectrum and the solution luminous photo that is scattered in the zero(ppm) water of 5%Tb, excitation wavelength is respectively 394 nanometers and 253 nanometers.
Accompanying drawing 6: the avidin after the nanocrystalline and resorcinolphthalein behind the biotin modification is modified is connected, and carries out the time resolved fluorescence resonance energy and transmits the principle that (TR-FRET) detects.
Embodiment
The preparation method of the rear-earth-doped lanthanum fluoride nano fluorescent of water miscible amination provided by the present invention marker material, its substantive features and Preliminary Applications can further embody through following examples.
Instance 1: take by weighing 0.07 g AEP, be dissolved in the 30 mL zero(ppm) water and obtain clear solution, regulate pH value to 6 with ammoniacal liquor then, then it is dissolved fully, obtain solution A, it is incubated at 30 ℃ toward wherein adding 0.126 g NaF, stirring; In addition with 0.424 g La (NO
3)
36H
2O and 0.009 g Eu (NO
3)
36H
2O is dissolved in fully in the 5 mL zero(ppm) water and obtains clear solution B; Under whipped state, solution B is dropwise joined solution A, continue to stir 20 hours, will obtain clear solution.Add 50 mL acetone precipitations then in this solution and go out nanocrystallinely, spinning with the deposition that obtains water and washing with alcohol several respectively, is drying to obtain LaF under 60 ℃ of vacuum conditions then
3: the 2%Eu manocrystalline powders.The manocrystalline powders that obtains is dissolved in the water, can obtains the water white aqueous solution.Detect with spectrograph, excite down at 394 nm, it is luminous to obtain strong red europium ion.
Instance 2: take by weighing 0.14 g AEP, be dissolved in the 30 mL zero(ppm) water and obtain clear solution, regulate pH value to 7 with ammoniacal liquor then, then it is dissolved fully, obtain solution C, it is incubated at 60 ℃ toward wherein adding 0.168 g NaF, stirring; In addition with 0.346 g La (NO
3)
36H
2O, 0.065 g Ce (NO
3)
36H
2O and 0.023 g Tb (NO
3)
36H
2O is dissolved in fully in the 5 mL zero(ppm) water and obtains clear solution D; Under whipped state, solution D is dropwise joined solution C, continue to stir 20 hours, will obtain clear solution.Add in this solution then 50 mL acetone precipitations go out nanocrystalline, spinning, with the deposition that obtains water and washing with alcohol several respectively, drying obtains LaF under 60 ℃ of vacuum conditions then
3: 15%Ce, 5%Tb manocrystalline powders.The manocrystalline powders that obtains is dissolved in the water, can obtains the water white aqueous solution.Detect with spectrograph, 253 nm excite down, and it is luminous to obtain strong green terbium ion.
Instance 3: take by weighing 0.28 g AEP, be dissolved in the 30 mL zero(ppm) water and obtain clear solution, regulate pH value to 8 with ammoniacal liquor then, then it is dissolved fully, obtain solution E, it is incubated at 90 ℃ toward wherein adding 0.21 g NaF, stirring; In addition with 0.216 g La (NO
3)
36H
2O and 0.228 g Dy (NO
3)
36H
2O is dissolved in fully in the 5 mL zero(ppm) water and obtains clear solution F; Under whipped state, solution F is dropwise joined solution E, continue to stir 20 hours, will obtain clear solution.Add in this solution then 50 mL acetone precipitations go out nanocrystalline, spinning, with the deposition that obtains water and washing with alcohol several respectively, drying obtains LaF under 60 ℃ of vacuum conditions then
3: the 50%Dy manocrystalline powders.
Instance 4:LaF
3: 15%Ce, the preparation of the nanocrystalline connection vitamin H of 5%Tb.Take by weighing 0.2 mmol vitamin H (biotin) and 0.2 mmol 1-ethyl-3-(3-dimethyl aminopropyl)-carbodiimide (EDC) and 0.5 mmol N-hydroxy-succinamide (NHS); Be dissolved in 20 mL phosphate buffered saline buffers (pH=7.2); Stirred 15 minutes, then to wherein adding 20 mg LaF
3: 15%Ce, the 5%Tb nano particle stirred 1 day, and is with zero(ppm) water and washing with alcohol repeatedly dry in vacuum drying oven then with precipitation and centrifugal separation, can obtain the LaF of finishing vitamin H
3: 15%Ce, 5%Tb inorganic nano-crystal.
Instance 5: the LaF that will connect vitamin H
3: 15%Ce; The nanocrystalline phosphate buffered saline buffer (pH=7.2) that is dissolved in of 5%Tb; Be divided into several parts of equal volume, after cultivating with the avidin that is marked with fluorescein isothiocyanate (FITC-avidin) of different concns then, on the fluorescence plate reading machine, take time resolved spectroscopy to detect; Excitation wavelength is 253 nm, and be 100 time of lag
μS, the gate time is 1 ms.Because Doped Rare Earth ion Tb in the nano particle
3+With the fluorescence resonance energy transmission (FRET) that resorcinolphthalein FITC exists, the result shows along with the increase of the FITC-avidin concentration that adds, detects Tb
3+Luminous intensity corresponding to 489 nm wave bands reduces; Resorcinolphthalein FITC increases corresponding to the luminous intensity of 520 nm wave bands simultaneously; In 3.7-200 nM scope; Exist the better linearity relation between avidin concentration and fluorescence intensity change, explain that the fluorescence that utilizes nano particle can be applied to detect avidin.
Claims (5)
1. the method for the rear-earth-doped lanthanum fluoride nano fluorescent marker material of a synthesizing amino functionalization; It is characterized in that: be dissolved in phosphorylethanolamine in the zero(ppm) water and with the pH value of ammoniacal liquor regulator solution; Then, stir and obtain colourless transparent solution to wherein adding Sodium Fluoride; Be added drop-wise in the above-mentioned solution after in addition rare earth nitrate being dissolved in zero(ppm) water; 30-90 ℃ of insulation and stir for some time, adding acetone makes nanocrystalline deposition in this solution then, and carries out spinning; Washing, it is nanocrystalline to obtain amidized rear-earth-doped lanthanum fluoride after the drying.
2. rear-earth-doped lanthanum fluoride preparation of nano crystal as claimed in claim 1, it is characterized in that: selecting phosphorylethanolamine for use is tensio-active agent, and both the nanocrystalline size of may command can realize the amino functional that it is surperficial again.
3. one kind like claim 1 and 2 described lanthanum fluoride preparation of nano crystal, it is characterized in that the adding molar weight ratio of reactant:
Lanthanum trinitrate: 1 part;
Sodium Fluoride: 3 ~ 6 parts;
Phosphorylethanolamine: 0.1 ~ 5 part.
4. like the described method of claim 1-3, resulting rear-earth-doped lanthanum fluoride is nanocrystalline, and its component is: xLn
3+-(1-x) LaF
3, Ln wherein
3+=Ce
3+, Yb
3+, Er
3+, Tm
3+, Ho
3+, Eu
3+, Gd
3+, Tb
3+, Dy
3+, Sm
3+, Nd
3+, Pr
3+, x=0-50 mol%.
5. like the purposes of the resultant amidized rear-earth-doped lanthanum fluoride nano fluorescent marker material of the described preparation method of claim 1-4; It is characterized in that: be applied to biomarker and detection; Nanocrystalline its surperficial amino that utilizes of rear-earth-doped lanthanum fluoride of preparation gained is connected with biomolecules; Can realize simultaneously specific luminously through the different rare earth ion that mixes in nanocrystalline, come this biological connection is detected, be applied to fields such as biological mark.
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| CN106010539A (en) * | 2016-06-07 | 2016-10-12 | 中国科学院合肥物质科学研究院 | Blue light excited praseodymium doped lanthanum fluoride red-light phosphor and preparation method thereof |
| CN106085432A (en) * | 2016-06-07 | 2016-11-09 | 中国科学院合肥物质科学研究院 | Organic-inorganic hybrid nanometer powder body of praseodymium doped lanthanum fluoride and its production and use |
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-
2011
- 2011-08-22 CN CN2011102425267A patent/CN102676171A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| LOIC J. CHARBONNIE` RE等: "Highly luminescent water-soluble lanthanide nanoparticles through surface coating sensitization", 《NEW JOURNAL OF CHEMISTRY》 * |
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| CN105623664A (en) * | 2016-02-17 | 2016-06-01 | 周口师范学院 | Rare earth ion doped trifluoride nanocrystalline in shape of stick of sugar coated fruits and preparation method of rare earth ion doped trifluoride nanocrystalline |
| CN105623664B (en) * | 2016-02-17 | 2018-02-27 | 周口师范学院 | A kind of rare earth ion doped trifluoride of sugarcoated haws shape is nanocrystalline and preparation method thereof |
| CN105623665A (en) * | 2016-02-23 | 2016-06-01 | 华中科技大学 | Oil soluble nanometer scintillation crystal and preparation method thereof |
| CN106010539A (en) * | 2016-06-07 | 2016-10-12 | 中国科学院合肥物质科学研究院 | Blue light excited praseodymium doped lanthanum fluoride red-light phosphor and preparation method thereof |
| CN106085432A (en) * | 2016-06-07 | 2016-11-09 | 中国科学院合肥物质科学研究院 | Organic-inorganic hybrid nanometer powder body of praseodymium doped lanthanum fluoride and its production and use |
| CN106085432B (en) * | 2016-06-07 | 2018-04-20 | 中国科学院合肥物质科学研究院 | Organic-inorganic hybrid nanometer powder of praseodymium doped lanthanum fluoride and its preparation method and application |
| CN110487763A (en) * | 2019-08-29 | 2019-11-22 | 临沂大学 | A kind of rapid sensitive detection method of hydrogen sulfide |
| CN112683985A (en) * | 2020-12-28 | 2021-04-20 | 中国科学院苏州生物医学工程技术研究所 | Metal label based on rare earth doped nano metal organic framework material |
| CN112683985B (en) * | 2020-12-28 | 2023-03-14 | 中国科学院苏州生物医学工程技术研究所 | Metal label based on rare earth doped nano metal organic framework material |
| CN113956881A (en) * | 2021-11-02 | 2022-01-21 | 西安文理学院 | Terbium-doped lanthanum fluoride nano particle, sol-gel hybrid material and preparation method |
| CN113956881B (en) * | 2021-11-02 | 2023-05-26 | 西安文理学院 | Terbium-doped lanthanum fluoride nano particle, sol-gel hybrid material and preparation method |
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Application publication date: 20120919 |