CN112266789B - Synthesis method of whitlockite nano probe with red fluorescence - Google Patents
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Abstract
The invention discloses a whitlockite nano probe with red fluorescence and a synthetic method thereof. Firstly, synthesizing the whitlockite nanoparticles by using a solvothermal system, and secondly, doping europium ions by using the same solvent system on the basis of the synthesized whitlockite nanoparticles to synthesize the europium ion doped whitlockite nanoprobe with bright red fluorescence. The particle size of the europium ion doped whitlockite particles synthesized by the invention is about 5-40nm, and the europium ion doped whitlockite particles have good biocompatibility and can be applied to the fields of cell imaging, tissue engineering materials and the like.
Description
Technical Field
The invention relates to a synthesis method of a whitlockite nano probe with red fluorescence.
Background
Whitlockite (Ca)18Mg2(HPO4)2(PO4)12，Whitlockite, WH) is an important mineral in human bones, has excellent biocompatibility, and can be used for preparing biomedical materials with excellent performance. In recent years, many reports on whitlockite exist, the synthesis method mainly adopts a hydrothermal method, and the particle size of aqueous phase synthesis is micron-sized, so that the application performance of the whitlockite is limited. Recently, c. Wang et al used a solvothermal method to effectively control the size of the whitlockite in an alkaline environment, synthesizing nanocrystals of about 20nm for promoting cell growth. How to simply and effectively prepare the small-size whitlockite nanocrystal with uniform appearance and size is the key point for exerting the application potential of the small-size whitlockite nanocrystal.
Disclosure of Invention
The invention aims to provide a method for synthesizing a brushite nanoprobe with red fluorescence.
In order to achieve the purpose, the invention has the following implementation process:
a synthetic method of a whitlockite nanometer probe with red fluorescence comprises the following synthetic steps: sequentially adding a calcium nitrate solution, a magnesium nitrate solution and a soluble phosphate solution into a mixed solution of oleic acid and ethanol, stirring uniformly, transferring the mixed solution into a closed reaction kettle, fully reacting at the temperature of 120 plus of materials and 200 ℃, naturally cooling, collecting precipitate, washing with cyclohexane and ethanol, re-dispersing in a mixed system of the oleic acid and the ethanol, adding an europium nitrate aqueous solution under magnetic stirring, stirring uniformly, transferring into the closed reaction kettle again, fully reacting at the temperature of 120 plus of materials and 200 ℃, naturally cooling, centrifuging to obtain precipitate, and washing with cyclohexane and ethanol for 2-3 times to obtain the europium ion doped whitlockite nanoprobe.
In the above step, the volume ratio of the oleic acid, the ethanol and the salt solution is 1: (2-6): (2-6), wherein the salt solution is a calcium nitrate solution, a magnesium nitrate solution and a soluble phosphate solution.
In the above steps, the molar ratio of the calcium nitrate to the magnesium nitrate is 9:1, and the molar ratio of the sum of the calcium nitrate and the magnesium nitrate to the sodium phosphate is 1.43: 1.
In the above step, the soluble phosphate is selected from sodium phosphate, sodium hydrogen phosphate and sodium dihydrogen phosphate.
In the above step, the molar ratio of europium nitrate to the sum of calcium nitrate and magnesium nitrate is (0.05-0.2): 1.
in the above steps, the reaction temperature is 120-.
In the above step, the particle size of the europium ion doped whitlockite nanocrystal is 5-40 nm.
In the above steps, the prepared europium ion doped whitlockite nanoparticle has bright red fluorescence and can be used for cell fluorescence labeling.
According to the method, oleic acid and ethanol are used as solvents, soluble calcium salt, magnesium salt and phosphate aqueous solution are used as raw materials, the whitlockite nanocrystal is controllably synthesized, and the synthesized nanoparticles have the advantages of small size, uniform appearance and good dispersibility. Rare earth europium ions are doped in the whitlockite crystal, and the europium ions with bright red fluorescence are doped in the whitlockite nanocrystal and can be applied to biological cell imaging. The reaction solvent system of the invention does not relate to acid and alkali reagents, the reaction environment is friendly, the raw materials are low in price, the method for preparing the whitlockite nano particles is simple, the reproducibility is good, and the method can be used for cell imaging, preparation of biological scaffold materials and the like.
Drawings
FIG. 1 is a TEM image of the preparation of a brushite nanoparticle of example 1;
FIG. 2 is a fluorescent scan of the europium ion-doped brushite nanoprobe prepared in example 1;
FIG. 3 is an XRD pattern of the whitlockite nanoparticles and europium ion-doped whitlockite nanoprobes prepared in example 1;
FIG. 4 is a fluorescent labeling diagram of europium ion-doped brushite nanoprobes prepared in example 4.
Detailed description of the preferred embodiment
The experimental methods used in the following examples are conventional methods unless otherwise specified; the material reagents used, unless otherwise specified, are commercially available.
Example 1
Step 1, synthesizing the brushite nano-particles.
Adding 5ml of oleic acid, 16ml of absolute ethyl alcohol, 4.5ml of 0.25M calcium nitrate solution, 0.5ml of 0.25M magnesium nitrate solution and 5ml of 0.15M sodium phosphate solution into a 50ml reaction kettle in sequence, uniformly stirring, sealing the reaction kettle, transferring the reaction kettle into a 150 ℃ oven for reaction for 15 hours, cooling to room temperature after the reaction is finished, centrifuging, collecting precipitate, washing the precipitate for 3 times by using cyclohexane and ethanol to obtain a sample.
The samples were examined and the associated TEM (figure 1) and XRD (figure 2) data showed that the product was a brushite nanoparticle with a particle size of about 20nm, with XRD diffraction peaks consistent with the standard card of brushite with no miscellaneous peaks, indicating that pure phase brushite nanocrystals were prepared.
And 2, synthesizing the europium ion doped whitlockite nano probe.
Adding 5ml of oleic acid and 16ml of absolute ethanol into a 50ml reaction kettle in sequence, uniformly stirring the whitlockite nanoparticles synthesized in the step 1, 250 mu l of 0.25M europium nitrate solution and 10ml of deionized water, sealing the reaction kettle, placing the reaction kettle in a 150 ℃ oven for reaction for 15 hours, naturally cooling the reaction kettle to room temperature after the reaction is finished, centrifuging and collecting precipitates, and washing the precipitates for 3 times by using cyclohexane and ethanol to obtain a target final product.
XRD diffraction analysis (figure 2) of the target final product shows that the europium ion doped whitlockite nanoparticles are consistent with the standard card of whitlockite and are pure-phase whitlockite nanocrystals; by observing that the europium ion-doped brushite nanoparticles have bright red fluorescence under an ultraviolet lamp, a fluorescence scanning image is shown in figure 3 (wherein an inset is a fluorescent photograph image).
Example 2
Step 1, synthesizing the brushite nano particles.
5ml of oleic acid, 10ml of absolute ethanol, 4.5ml of 0.25M calcium nitrate solution, 0.5ml of 0.25M magnesium nitrate solution and 5ml of 0.15M sodium hydrogen phosphate solution are sequentially added into a 50ml reaction kettle, the reaction kettle is sealed after uniform stirring, the reaction kettle is transferred into a 120 ℃ oven for reaction for 20 hours, after the reaction is finished, the reaction kettle is cooled to room temperature, precipitates are collected by centrifugation, and the precipitates are washed 3 times by cyclohexane and ethanol to obtain a sample similar to step 1 in example 1.
And 2, synthesizing the europium ion doped whitlockite nanoprobe.
Adding 5ml of oleic acid and 10ml of absolute ethanol into a 50ml reaction kettle in sequence, adding 500 mu l of 0.25M europium nitrate solution and 10ml of deionized water into the white apatite nanoparticles synthesized in the step 1, uniformly stirring, sealing the reaction kettle, placing the reaction kettle in a 120 ℃ oven for reaction for 20 hours, naturally cooling the reaction kettle to room temperature after the reaction is finished, centrifugally collecting precipitate, and washing the precipitate with cyclohexane and ethanol for 3 times to obtain a target final product. The target product has a similar appearance to the nanocrystalline obtained in step 2 of example 1, and also has bright red fluorescence.
Example 3
Step 1, synthesizing the brushite nano particles.
50ml of oleic acid, 100ml of absolute ethanol, 45ml of 0.25M calcium nitrate solution, 5ml of 0.25M magnesium nitrate solution and 50ml of 0.15M sodium dihydrogen phosphate solution are sequentially added into a 500ml reaction kettle, the mixture is uniformly stirred, then the reaction kettle is sealed and transferred into a 180 ℃ oven for reaction for 12 hours, after the reaction is finished, the reaction kettle is cooled to room temperature, precipitate is collected by centrifugation and washed 3 times by cyclohexane and ethanol, and a sample similar to the sample obtained in the step 1 in the example 1 is obtained.
And 2, synthesizing the europium ion doped whitlockite nano probe.
Adding 50ml of oleic acid and 100ml of absolute ethanol into a 500ml reaction kettle in sequence, adding 5.0ml of 0.25M europium nitrate solution and 100ml of deionized water into the white apatite nanoparticles synthesized in the step 1, uniformly stirring, sealing the reaction kettle, placing the reaction kettle in a 180 ℃ oven for reaction for 12 hours, naturally cooling the reaction kettle to room temperature after the reaction is finished, centrifugally collecting precipitate, and washing the precipitate with cyclohexane and ethanol for 3 times to obtain a target final product. The appearance of the target product is similar to that of the nanocrystalline obtained in the step 2 of the embodiment 1, and the target product also has bright red fluorescence.
Example 4 cellular fluorescence labeling of europium ion-doped brushite nanoprobes
Carrying out hydrophilic modification on the synthesized europium ion doped nanocrystalline, and carrying out fluorescent labeling on cells, wherein the method comprises the following steps:
step 1, hydrophilic modification of europium ion doped whitlockite nanoprobe
Adding a proper amount of cyclohexane into a 50ml beaker, adding a proper amount of europium ion-doped whitlockite nanocrystals prepared in the step 2 in the example 1, uniformly dispersing, then adding a glucan aqueous solution, violently stirring for 2-4h, centrifuging to obtain a precipitate, washing the precipitate with ethanol and water for 3 times, and finally obtaining the hydrophilic europium ion-doped whitlockite nanoparticles.
Step 2, carrying out cell fluorescence labeling on europium ion doped whitlockite nanoprobe
(1) Preparation of related reagents
DMEM cell complete medium: adding 10% fetal calf serum, 100 mug/ml streptomycin and 100U/ml penicillin into a DMEM basic culture medium, mixing uniformly, and placing into a refrigerator at 4 ℃ for later use.
Preparation of PBS solution: weighing potassium chloride 0.01g, sodium chloride 0.40g, dipotassium hydrogen phosphate 0.01g and disodium hydrogen phosphate 0.17g respectively, adding 1000ml double distilled water, ultrasonic dissolving, adjusting pH to 7.40, sterilizing at 121 ℃ for 30min, and storing in a refrigerator at 4 ℃ for later use.
Preparation of 0.25% pancreatin: 100mg of pancreatin was weighed, 40ml of PBS was added, and the mixture was filtered through a 0.22 μm filter and stored in a refrigerator at 4 ℃ for further use.
Preparing a europium ion doped whitlockite nanoparticle solution with the concentration of 160 mu g/ml: after the nanoparticles were irradiated with cobalt 60, 1.6mg of the nanoparticles were weighed and dispersed in 10ml of DMEM culture solution, mixed well, and stored in a 4 ℃ refrigerator for later use.
(2) Fluorescent labeling of cells
Recovery of cells
Taking out frozen MCF-7 cells in a liquid nitrogen tank, putting the cells into water at 37 ℃ until ice cubes are melted, adding the cells into a centrifuge tube, adding 2ml of culture solution, uniformly blowing, centrifuging for 5min at the rotation speed of 1000 revolutions, sucking out supernatant after the centrifugation is finished, adding 2ml of culture solution, uniformly blowing the cells precipitated at the bottom of the centrifuge tube, adding about 10ml of culture solution into a culture dish, adding the cells in the centrifuge tube into the culture dish, uniformly mixing, and finally putting the cells into a culture dish at 37 ℃ and 5% CO2And (5) recovering the cells in the incubator.
② passage of cells
After the recovered MCF-7 cells grow to 90% adherent, sucking out culture solution, adding 2ml of PBS to clean the cells for 2 times, adding 2ml of pancreatin into a culture dish, placing the culture dish into an incubator to digest for 2 min, and observing the digestion condition under a microscope; after digestion is finished, adding 3 ml of culture solution, blowing and beating cells for a plurality of times, transferring the cells into a 15 ml centrifuge tube, centrifuging for 5min at the rotating speed of 1000 revolutions, removing supernatant, adding 2ml of culture solution into the supernatant, and uniformly blowing; adding 10ml culture solution into a new culture dish, and addingDividing the cells in the centrifuge tube into two parts, adding into a culture dish, mixing, and adding 5% CO at 37 deg.C2Culturing in an incubator.
Cloth board
Taking the cell culture dish out of the culture box in the step II, observing under a microscope, removing the culture solution after the adherent growth of the cells reaches 90 percent, then adding 2ml of PBS to clean the cells for 2 times, adding 2ml of pancreatin into the culture dish, putting the culture dish into the culture box to digest for 2 min, observing the digestion condition under the microscope, adding 5-8 ml of culture solution after the digestion is finished, blowing and beating the cells for a plurality of times, then pumping the cells into a cell counting plate with the volume of 50 mu l, diluting the cells according to a certain proportion after counting, then distributing the cells into a laser confocal dish, wherein the cell density is about 5 multiplied by 104One/hole, put into 37 ℃ and 5% CO2Culturing in an incubator for 24 h.
Laser confocal measurement
After the cells adhere to the wall in the step III, adding a culture solution containing europium ion-doped whitlockite nanoparticles into a laser confocal dish, co-culturing for 24 hours, sucking out the culture solution, cleaning the nanoparticles which are not phagocytized by the cells by PBS, then adding a certain amount of 4% paraformaldehyde fixing solution, fixing for 15 minutes, sucking out the fixing solution, cleaning the surfaces of the cells by PBS, and observing under a Nikon A1 type laser confocal microscope, wherein the result is shown in figure 4, the cells phagocytose nanocrystalline to form bright red images, the middle parts of the cells have oval dark shadows, and the parts are the cell nuclei, which indicates that the nanoparticles cannot enter the cell nuclei due to large size and only exist in cytoplasm.
Claims (5)
1. A synthetic method of a whitlockite nanoprobe with red fluorescence is characterized in that: sequentially adding a calcium nitrate solution, a magnesium nitrate solution and a soluble phosphate solution into a mixed solution of oleic acid and ethanol, stirring uniformly, transferring the mixed solution into a closed reaction kettle, fully reacting at the temperature of 120-plus-200 ℃, naturally cooling, collecting precipitate, washing with cyclohexane and ethanol, re-dispersing in a mixed system of oleic acid and ethanol, adding an europium nitrate aqueous solution under magnetic stirring, stirring uniformly, transferring into the closed reaction kettle again, fully reacting at the temperature of 120-plus-200 ℃, naturally cooling, centrifuging to obtain precipitate, and washing with cyclohexane and ethanol to obtain a europium ion-doped whitlockite nanoprobe;
the volume ratio of the oleic acid to the ethanol to the salt solution is 1: (2-6): (2-6), wherein the salt solution is a calcium nitrate solution, a magnesium nitrate solution and a soluble phosphate solution; the molar ratio of the calcium nitrate to the magnesium nitrate is 9:1, and the molar ratio of the sum of the calcium nitrate and the magnesium nitrate to the sodium phosphate is 1.43: 1.
2. The method for synthesizing the brushite nanoprobe with red fluorescence according to claim 1, wherein: the soluble phosphate is selected from sodium phosphate, sodium hydrogen phosphate and sodium dihydrogen phosphate.
3. The method for synthesizing the brushite nanoprobe with red fluorescence according to claim 1, wherein: the molar ratio of europium nitrate to the sum of calcium nitrate and magnesium nitrate is (0.05-0.2): 1.
4. the method for synthesizing the nanoprobe of whitlockite with red fluorescence according to claim 1, wherein: the reaction temperature is 120 ℃ and 200 ℃, and the reaction time is 12-20 h.
5. The method for synthesizing the nanoprobe of whitlockite with red fluorescence according to claim 1, wherein: the grain diameter of the europium ion doped whitlockite nanocrystal is 5-40 nm.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103569985A (en) * | 2012-08-10 | 2014-02-12 | Seoul大学校产学协力团 | Whitlockite and method for manufacturing the same |
| CN105219391A (en) * | 2015-09-22 | 2016-01-06 | 西北大学 | A kind of preparation method of fluoro-europium-doped column hydroxide radical phosphorite nanocrystalline |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103569985A (en) * | 2012-08-10 | 2014-02-12 | Seoul大学校产学协力团 | Whitlockite and method for manufacturing the same |
| CN105219391A (en) * | 2015-09-22 | 2016-01-06 | 西北大学 | A kind of preparation method of fluoro-europium-doped column hydroxide radical phosphorite nanocrystalline |
Non-Patent Citations (2)
| Title |
|---|
| Simultaneously tuning emission color and realizing optical thermometry via efficient Tb3+/Eu3+ energy transfer in whitlockite-type phosphate multifunctional phosphors;Li Li et al.;《Journal of Alloys and Compounds》;20181129;第780卷;第266-275页 * |
| Synthesis and formation mechanism of bone mineral, whitlockite nanocrystals in tri-solvent system;Caifeng Wang et al.;《Journal of Colloid and Interface Science》;20200217;第569卷;第1-11页 * |
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