CN101214382A - Method for preparing europium-labeled hydroxyapatite nano particle - Google Patents
Method for preparing europium-labeled hydroxyapatite nano particle Download PDFInfo
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- CN101214382A CN101214382A CNA2008100036826A CN200810003682A CN101214382A CN 101214382 A CN101214382 A CN 101214382A CN A2008100036826 A CNA2008100036826 A CN A2008100036826A CN 200810003682 A CN200810003682 A CN 200810003682A CN 101214382 A CN101214382 A CN 101214382A
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- hydroxyapatite
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Abstract
The invention discloses a method of preparing an Eu-labelled nano-HAP, which is characterized in that calcium nitrate and monoammonium sulfate are taken according to the stoichiometric ratio of the hydroxyapatite produced in stoichiometry; the calcium nitrate is dissolved in the water solution of ethyl alcohol, and solution A is obtained by adding europium nitrate by quantity; solution B is obtained by dissolving monoammonium sulfate into the water solution of ethyl alcohol; solution A is dripped into solution B, the pH value of the mixed solution is regulated, and dispersant is added; a filter cake is obtained through sucking filtration, and the impurities are washed with a cleaner; the filter cake is dried through a freeze-drying method, for obtaining hydroxyapatite powder; the diameter of the powder is between 20mm to 150mm. The method of preparing an Eu-labelled nano-HAP provided by the invention has simple process which is easy to be controlled and raw materials which are easy to be collected; fluorescent light can be excited from the prepared hydroxyapatite for tracing. The invention is widely applicable in tracing and positioning in cells in cell culturing and other vitro experiments as well as tracing and positioning in animal bodies in vivo experiments.
Description
Technical field
The present invention relates to a kind of preparation method of synthesizing hydroxylapatite, be specifically related to a kind of preparation method of europium-labeled hydroxyapatite nano particle.
Background technology
(hydroxyapatite is the main inorganic composition of human bone HA) to hydroxyapatite, and the good tissue compatibility and adsorptivity are arranged, and its powder has been widely used in clinical as the material for repairing and the pharmaceutical carrier of bone defect.Studies show that in recent years, the numerous characteristics of HA and its size are closely related.When size during between 1～100nm HA be not only a kind of inorganic ceramic powder of function admirable, and it is active to have unique biological, existingly discovers that the hydroxyapatite superfine powder has the obvious suppression effect to people's hepatocarcinoma, gastric cancer, colon cancer.The type that hydroxyapatite is used mainly contains block ceramic, granule, coating, composite.Preparation method mainly contains solid phase method, coprecipitation, hydro-thermal method, mechanochemical reaction, sonochemistry method, sol-gal process etc. at present, though can prepare the hydroxyapatite of corresponding particle diameter, also not have spike in use and localized hydroxyapatite at present.
Summary of the invention
The objective of the invention is to provide a kind of preparation method that can be inspired fluorescence and the hydroxyapatite by fluorescent tracing at the deficiencies in the prior art, it is to adopt coprecipitation to prepare hydroxy apatite powder, and employing ultra-sonic dispersion, the particle diameter of steps such as lyophilization control powder body is used to adapt to widely.
The preparation method of the europium-labeled hydroxyapatite nano particle that the present invention is designed, concrete steps are:
1). the stoichiometric proportion that generates hydroxyapatite by stoichiometry is got lime nitrate, ammonium hydrogen phosphate, the ratio calcium (Ca) of amount of substance/phosphorus (P) is 1.67;
2). lime nitrate is dissolved in the alcoholic acid aqueous solution, and alcoholic solution concentration is not more than 55%, is that 1% amount is added europium nitrate by ratio europium (the Eu)/calcium (Ca) of amount of substance;
3). ammonium hydrogen phosphate is dissolved in the alcoholic acid aqueous solution, and alcoholic solution concentration is not more than 55%;
4). with join in the step 2 drips of solution add join in the step 3 solution in, utilize ammonia to regulate between mixed liquor pH value to 9～10, add dispersant simultaneously, vigorous stirring is after question response is finished; Described dispersant is a polysaccharide;
5). sucking filtration obtains filter cake, with abluent flush away impurity; Described abluent is a kind of or the two mixing in water or the ethanol;
6). place cryogenic refrigerator freezing the gained filter cake, wait to freeze real after, under vacuum condition, carry out lyophilization, obtain hydroxy apatite powder;
7). detect through observing, the particle diameter of hydroxy apatite powder is between 20nm～150nm.
The preparation method technical process of europium-labeled hydroxyapatite nano particle provided by the present invention is simple and easy to control, raw material is easy to get, the hydroxyapatite for preparing can be inspired fluorescence and by fluorescent tracing, can be widely used in the cell in the experiment in vitro such as cell culture interior spike of animal body and the location in the experiment in the spike and location and body.
Description of drawings
Fig. 1 does the fluorescence photo of laser confocal microscope gained for the hydroxyapatite of gained of the present invention.
Fig. 2 makees the photo of transmission electron microscope gained for the needle-like hydroxyapatite of gained of the present invention.
The specific embodiment
The invention will be further described with indefiniteness embodiment below.
Embodiment 1
Get lime nitrate 1.8892g (0.008mol) and be dissolved in the 33ml water, add 14ml ethanol again, add europium nitrate 0.0357g (8 * 10 in proportion
-5Mol), promptly in the step 2). gained; Get ammonium hydrogen phosphate 0.6339g (0.0048mol), be dissolved in the 33ml water, add 14ml ethanol again, be in the step 3). gained, with 3). in join drips of solution add 2). in join solution in, regulating pH value by ammonia is 10, add dispersant simultaneously, vigorous stirring.Handle with ultra-sonic dispersion then, vacuum filtration is got filter cake and is placed refrigerator, after waiting to be frozen into ice, carries out lyophilization, obtains hydroxy apatite powder.Obtain product cut size, greatly about 90～110nm.
Embodiment 2
Get lime nitrate 5.9038g (0.025mol) and be dissolved in the 50ml water, add europium nitrate 0.1115g (2.5 * 10 in proportion
-4Mol), promptly in the step 2). gained; Get ammonium hydrogen phosphate 1.9809g (0.015mol), be dissolved in the 30ml water, promptly in the step 3). gained, with 3). in join drips of solution add 2). in join solution in, regulating pH value by ammonia is 9.5, adds dispersant simultaneously, vigorous stirring.Handle with ultra-sonic dispersion then, vacuum filtration is got filter cake and is placed refrigerator, after waiting to be frozen into ice, carries out lyophilization, obtains hydroxy apatite powder.Obtain product cut size, greatly about 60～70nm.
Embodiment 3
Get lime nitrate 5.9038g (0.025mol) and be dissolved in the 25ml water, add 25ml ethanol again, add europium nitrate 0.1115g (2.5 * 10 in proportion
-4Mol), promptly in the step 2). gained; Get ammonium hydrogen phosphate 1.9809g (0.015mol), be dissolved in the 25ml water, add 5ml ethanol again, promptly in the step 3). gained, with 3). in join drips of solution add 2). in join solution in, regulating pH value by ammonia is 9, adds dispersant simultaneously, vigorous stirring.Handle with ultra-sonic dispersion then, vacuum filtration is got filter cake and is placed refrigerator, after waiting to be frozen into ice, carries out lyophilization, obtains hydroxy apatite powder.Obtain product cut size, greatly about 80～100nm.
Claims (2)
1. the preparation method of an europium-labeled hydroxyapatite nano particle, it is characterized in that: concrete steps are:
1). the stoichiometric proportion that generates hydroxyapatite by stoichiometry is got lime nitrate, ammonium hydrogen phosphate, the ratio calcium (Ca) of amount of substance/phosphorus (P) is 1.67;
2). lime nitrate is dissolved in the alcoholic acid aqueous solution, and alcoholic solution concentration is not more than 55%, is that 1% amount is added europium nitrate by ratio europium (the Eu)/calcium (Ca) of amount of substance;
3). ammonium hydrogen phosphate is dissolved in the alcoholic acid aqueous solution, and alcoholic solution concentration is not more than 55%;
4). with join in the step 2 drips of solution add join in the step 3 solution in, utilize ammonia to regulate between mixed liquor pH value to 9～10, add dispersant simultaneously, vigorous stirring is after question response is finished; Described dispersant is a polysaccharide;
5). sucking filtration obtains filter cake, with abluent flush away impurity; Described abluent is a kind of or the two mixing in water or the ethanol;
6). place cryogenic refrigerator freezing the gained filter cake, wait to freeze real after, under vacuum condition, carry out lyophilization, obtain hydroxy apatite powder.
2. the preparation method of europium-labeled hydroxyapatite nano particle according to claim 1, it is characterized in that: the particle diameter of described hydroxy apatite powder is between 20nm～150nm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CNA2008100036826A CN101214382A (en) | 2008-01-11 | 2008-01-11 | Method for preparing europium-labeled hydroxyapatite nano particle |
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| Application Number | Priority Date | Filing Date | Title |
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| CNA2008100036826A CN101214382A (en) | 2008-01-11 | 2008-01-11 | Method for preparing europium-labeled hydroxyapatite nano particle |
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| CN101214382A true CN101214382A (en) | 2008-07-09 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102020258A (en) * | 2010-10-26 | 2011-04-20 | 青岛科技大学 | Method for preparing magnetic fluorescence hydroxyapatite nanocomposite structure |
| CN102250615A (en) * | 2011-05-06 | 2011-11-23 | 清华大学 | Fluorine-containing hydroxylapatite single crystal nano shuttle with fluorescence labeling and preparation method thereof |
| CN103822906A (en) * | 2014-02-19 | 2014-05-28 | 武汉理工大学 | Quantitative detection tracing method of intracellular HPA (hydroxyapatite) nano particles |
| RU2628610C1 (en) * | 2016-06-17 | 2017-08-21 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Санкт-Петербургский государственный университет" (СПбГУ) | Method for production of nano-dimensional high-luminescent apatite with europium (eu) impurity |
-
2008
- 2008-01-11 CN CNA2008100036826A patent/CN101214382A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102020258A (en) * | 2010-10-26 | 2011-04-20 | 青岛科技大学 | Method for preparing magnetic fluorescence hydroxyapatite nanocomposite structure |
| CN102020258B (en) * | 2010-10-26 | 2013-01-09 | 青岛科技大学 | Method for preparing magnetic fluorescence hydroxyapatite nanocomposite structure |
| CN102250615A (en) * | 2011-05-06 | 2011-11-23 | 清华大学 | Fluorine-containing hydroxylapatite single crystal nano shuttle with fluorescence labeling and preparation method thereof |
| CN103822906A (en) * | 2014-02-19 | 2014-05-28 | 武汉理工大学 | Quantitative detection tracing method of intracellular HPA (hydroxyapatite) nano particles |
| CN103822906B (en) * | 2014-02-19 | 2016-03-09 | 武汉理工大学 | A kind ofly quantitatively detect the method for spike for HAP nano particle in cell |
| RU2628610C1 (en) * | 2016-06-17 | 2017-08-21 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Санкт-Петербургский государственный университет" (СПбГУ) | Method for production of nano-dimensional high-luminescent apatite with europium (eu) impurity |
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Open date: 20080709 |