CN107952403A - A kind of fluorescent silicon dioxide method for preparing microsphere of Quantitative detection iron ion - Google Patents
A kind of fluorescent silicon dioxide method for preparing microsphere of Quantitative detection iron ion Download PDFInfo
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- CN107952403A CN107952403A CN201711258971.6A CN201711258971A CN107952403A CN 107952403 A CN107952403 A CN 107952403A CN 201711258971 A CN201711258971 A CN 201711258971A CN 107952403 A CN107952403 A CN 107952403A
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- silicon dioxide
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- fluorescent silicon
- quantitative detection
- iron ion
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- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/025—Applications of microcapsules not provided for in other subclasses
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/02—Use of particular materials as binders, particle coatings or suspension media therefor
- C09K11/025—Use of particular materials as binders, particle coatings or suspension media therefor non-luminescent particle coatings or suspension media
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/06—Luminescent, e.g. electroluminescent, chemiluminescent materials containing organic luminescent materials
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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Abstract
The invention discloses a kind of fluorescent silicon dioxide method for preparing microsphere of Quantitative detection iron ion, it is characterised in that includes the following steps：（1）With citric acid, thionyl chloride and aminoethylaminopropyl methyl dimethoxysilane（AEAPMS) citric amide fluorescent small molecule is prepared for reactant（CA‑AEAPMS）, which has fluorescence；（2）With ethyl orthosilicate（TEOS）It is raw material with CA AEAPMS, alcohols is medium, is hydrolyzed by ammonia-catalyzed, dry after filtering, prepares fluorescent silicon dioxide microballoon.Using fluorescent silicon dioxide microspherulite diameter made from method provided by the present invention in the range of 100 ~ 300 nm, its uniform particle diameter, size are controllable, have the advantages that property stabilization, fluorescence intensity height, good water solubility, hypotoxicity and be easy to functional modification.The fluorescent silicon dioxide microballoon is worth in ion identification field with applications well, to Fe3+With specific recognition ability and high sensitivity, detection is limited to 5.2 nM, and Quantitative detection can be achieved in 0 ~ 45 μM of concentration range.This method has the characteristics that easy to operate, quick, accuracy rate is high, test limit is low.
Description
Technical field
The present invention relates to a kind of fluorescent silicon dioxide method for preparing microsphere of Quantitative detection iron ion, belongs to fluorescence spy
Pin technical field.
Background technology
In recent years, fluorescent silicon dioxide microballoon is as a kind of new functional material, with its special morphosis and height
The luminous efficiency of effect, plays in the fields such as fluoroimmunoassay, biology sensor, high-flux medicaments sifting and ion detection
Important effect, is one of the hot subject of current research exploitation and application.
CN103484101A discloses a kind of core shell structure fluorescent silicon dioxide method for preparing microsphere, including is dispersed with glimmering
The macromolecule kernel of photoinitiator dye, and the homogeneous shell of thickness made of earth silicon material, used fluorescent dye are
Class and its derivative, pyrene class and its derivative, fluorenes class and its derivative, triaryl amino and derivative, pyrazolo quinoline and
One or more in its derivative, triaryl boron class and its derivative and the class dyestuff of structure containing DCM.CN101717644A is carried
For a kind of preparation method of silicon dioxide-coated quantum dots, the SiO of uniform particle sizes is obtained2The CdSe/CdS nucleocapsid structures of cladding
Fluorescent silicon dioxide microballoon.Although present fluorescent silicon dioxide microballoon species is various, general organic dyestuff fluorescence examination
Agent is mainly that fluorescein, rhodamine, BODIPY, cyanine class dyestuff etc. are all electron conjugated with traditional fluorophor, aromatic ring etc.
Structure and molecular rigidity structure produce fluorescence, and the fluorescent silicon dioxide microballoon of preparation is usually water-soluble poor, biocompatibility compared with
Low and toxicity is higher, seriously constrains its application.Another common fluorometric reagent is quantum dot, but its high toxicity is one
A problem for being very difficult to solve.Therefore the fluorescence of a kind of stable property, fluorescence intensity height, good water solubility and hypotoxicity is prepared
Silicon dioxide microsphere has great importance.
Common qualitative and quantitative detection Fe3+Method have：Atomic absorption, colorimetric method, spectrophotometry, cyclic voltammetry,
Fluorescence probe method etc..CN102391150A provides a kind of iron-ion fluorescent probe compound p-phenylenediamine contracting ethyl diacetate base
Benzaldehyde and preparation method thereof, the compound show iron ion in buffer solution identity, minimum detectable iron from
Sub- concentration is 10-6 mol/L.Fe is detected currently with fluorescence probe method3+Patent have very much, but still have it is perhaps many not
Foot, such as fluorescence probe preparation process are relatively cumbersome, and test limit is higher, it is impossible to carries out Quantitative detection etc..Therefore, overcome with
Upper deficiency, prepare it is a kind of it is easy to use, test limit is low, strong antijamming capability can carry out the Fe of Quantitative detection at the same time3+Visit
Needle set has important practical significance.
The content of the invention
In view of the deficiencies of the prior art, one of present disclosure is to provide a kind of dioxy without Representative fluorescence group
The preparation method of SiClx fluorescent microsphere, the silica fluorescent microballoon have property stabilization, fluorescence intensity height, good water solubility, low
Toxicity and the advantages of being easy to functionalization.
The silica fluorescent microballoon that the two of present disclosure are to provide can be to Fe3+It can carry out specific recognition and fast
Fast quantitative detection, detection are limited to 5.2 nM, Quantitative detection can be carried out in 0 ~ 45 μM of concentration range.With existing Fe3+Concentration
Detection method is compared, and the fluorescent silicon dioxide microballoon is to Fe3+Test limit is far below other patents, and easy to operate, quick, accurate
True rate is high, strong antijamming capability.
The preparation method of fluorescent silicon dioxide microballoon provided by the present invention, comprises the following steps.
（1）Prepare citric amide fluorescent small molecule
Anhydrous citric acid and thionyl chloride are added in tetrahydrofuran, after the reaction was complete, pure lemon acyl is made in revolving purification
Chlorine, then the normal-temperature reaction in tetrahydrofuran by obtained lemon acyl chlorides and aminoethylaminopropyl methyl dimethoxysilane, revolves
After steaming purification, citric amide fluorescent small molecule is made.
（2）Prepare fluorescent silicon dioxide microballoon
By ethyl orthosilicate, citric amide fluorescent small molecule, deionized water, ammonium hydroxide by certain mass than being added to alcohols and water
In the mixed solvent is fully reacted, and is filtered, is washed, pulverizing after drying, fluorescent silicon dioxide microballoon is made.
As optimal technical scheme, during fluorescent silicon dioxide microballoon is synthesized, the alcohols solvent is methanol,
Ethanol or butanol, preferably absolute ethyl alcohol.
As optimal technical scheme, during fluorescent silicon dioxide microballoon is synthesized, the fluorescent silicon dioxide microballoon
Particle diameter be 100 ~ 300 nm, preferably 140 nm.
As optimal technical scheme, during fluorescent silicon dioxide microballoon is synthesized, the ethyl orthosilicate, lemon acyl
Amine fluorescent small molecule, deionized water, ammonium hydroxide are by certain mass than 1：(0.02~0.2)：(8~12)：(2 ~ 4), are preferably 1:
0.05:10:3。
As optimal technical scheme, during fluorescent silicon dioxide microballoon is synthesized, the volume of the alcohols and water
Than (8 ~ 12):1, it is preferably 10：1.
As optimal technical scheme, during fluorescent silicon dioxide microballoon is synthesized, the fluorescent silicon dioxide is micro-
Ball needs that 4 ~ 10 h of reaction, preferably 6 h is stirred at room temperature.
As optimal technical scheme, during fluorescent silicon dioxide microballoon is synthesized, the drying process temperature range
It is 0 ~ 150 DEG C, preferably 120 DEG C.
As optimal technical scheme, when configuring fluorescent silicon dioxide microspheres solution, using deionized water as solvent, concentration for 1 ~
10 μ g/ml, preferably 2 μ g/ml.
Compared with prior art, the present invention is for the first time using the citric amide fluorescent small molecule for not containing Representative fluorescence group
As fluorescence source, by preparing silica fluorescent microballoon with ethyl orthosilicate cohydrolysis, which has
The advantages of fluorescence intensity height, good biocompatibility, low high water solubility and toxic side effect, prepare environmental-friendly luminescent material,
Therapeutic treatment, biological fluorescent labelling and ion detection etc. have a wide range of applications potentiality.
Brief description of the drawings
Fig. 1 is fluorescent silicon dioxide microballoon scanning electron microscopic picture prepared by embodiment one.
Fig. 2 is fluorescence spectra of the fluorescent silicon dioxide microballoon of the preparation of embodiment one under different excitation wavelengths.
Fig. 3 is fluorescence spectra of the fluorescent silicon dioxide microballoon to each ion identification of the preparation of embodiment one.
Fig. 4 is the fluorescent silicon dioxide microballoon of the preparation of embodiment one to Fe3+The fluorescence spectra of identification.
Fig. 5 is the fluorescent silicon dioxide microballoon of the preparation of embodiment one to Fe3+The linear relationship chart of identification.
Embodiment
Such scheme is described further below in conjunction with specific embodiment.These embodiments be used for illustrate the present invention without
It is limited to limit the scope of the invention.The implementation condition used in embodiment can do further adjustment according to actual conditions.Below
Illustrate the specific implementation process of the present invention by embodiment.
Embodiment one
（1）Prepare citric amide fluorescent small molecule
1 g anhydrous citric acids and 1.2 ml thionyl chlorides are placed in the flask full of nitrogen, 12h is stirred at -5 DEG C.So
Gained lemon acyl chlorides, revolving purification three times, are removed excessive thionyl chloride, obtain pure lemon acyl chlorides afterwards.Again by lemon
Acyl chlorides is dissolved in 40 ml tetrahydrofurans, is added dropwise 3.8 ml AEAPMS under stirring condition the reaction was continued 3 h, obtain citric amide fluorescence
Small molecule crude product.By gained citric amide small molecule crude product with the purification of petroleum ether revolving three times, it is glimmering to obtain pure citric amide
Light small molecule.
（2）Prepare fluorescent silicon dioxide microballoon
80 ml absolute ethyl alcohols, 10ml water and 3 ml ammonium hydroxide are sequentially added in 250 ml round-bottomed flasks first, use magnetic force at room temperature
Blender stirs 30 min.Then it is dissolved in 0.08 small point of g citric amide fluorescence being uniformly mixed in 20 ml absolute ethyl alcohols
Son and 1 ml ethyl orthosilicates (TEOS) are slowly dropped in above-mentioned mixed solution.After stirring 6 h, centrifugation, washing, and in 120
DEG C obtain fluorescent silicon dioxide microballoon within dry two hours.
（3）Fluorescent silicon dioxide microspheres solution is prepared by solvent of deionized water, concentration is 2 μ g/ml, is detected
Fe3+0 ~ 80 μM of concentration range.A length of 360 nm of optimum excitation wave is set, the fluorescence intensity of recording solution is with Fe3+Concentration variation diagram
Spectrum.Its detection is limited to 5.2 nM, 0 ~ 45 μM of the range of linearity.
Embodiment two
（1）Prepare citric amide fluorescent small molecule
1 g anhydrous citric acids and 1.2 ml thionyl chlorides are placed in the flask full of nitrogen, 14h is stirred at -0 DEG C.So
Afterwards by gained lemon acyl chlorides, revolving purification three times, removes excessive thionyl chloride, obtains pure lemon acyl chlorides.Again by lemon
Acyl chlorides is dissolved in 40 ml tetrahydrofurans, is added dropwise 3.8 ml AEAPMS under stirring condition the reaction was continued 5 h, obtain citric amide fluorescence
Small molecule crude product.By gained citric amide small molecule crude product with the purification of petroleum ether revolving three times, it is glimmering to obtain pure citric amide
Light small molecule.
（2）Prepare fluorescent silicon dioxide microballoon
80 ml absolute ethyl alcohols, 10ml water and 3 ml ammonium hydroxide are sequentially added in 250 ml round-bottomed flasks first, use magnetic force at room temperature
Blender stirs 30 min.Then it is dissolved in 0.06 small point of g citric amide fluorescence being uniformly mixed in 20 ml absolute ethyl alcohols
Son and 0.8 ml ethyl orthosilicates (TEOS) are slowly dropped in above-mentioned mixed solution.After stirring 6 h, centrifugation, washing, and in
100 DEG C of dryings obtain fluorescent silicon dioxide microballoon in two hours.
（3）Fluorescent silicon dioxide microspheres solution is prepared by solvent of deionized water, concentration is 3 μ g/ml, is detected
Fe3+0 ~ 80 μM of concentration range.A length of 360 nm of optimum excitation wave is set, the fluorescence intensity of recording solution is with Fe3+Concentration variation diagram
Spectrum.Its detection is limited to 11.3 nM, 0 ~ 45 μM of the range of linearity.
Embodiment three
（1）Prepare citric amide fluorescent small molecule
1 g anhydrous citric acids and 1.2 ml thionyl chlorides are placed in the flask full of nitrogen, 10h is stirred at 10 DEG C.So
Afterwards by gained lemon acyl chlorides, revolving purification three times, removes excessive thionyl chloride, obtains pure lemon acyl chlorides.Again by lemon
Acyl chlorides is dissolved in 40 ml tetrahydrofurans, is added dropwise 3.2 ml AEAPMS under stirring condition the reaction was continued 4 h, obtain citric amide fluorescence
Small molecule crude product.By gained citric amide small molecule crude product with the purification of petroleum ether revolving three times, it is glimmering to obtain pure citric amide
Light small molecule.
（2）Prepare fluorescent silicon dioxide microballoon
100 ml absolute ethyl alcohols, 10ml water and 5 ml ammonium hydroxide are sequentially added in 250 ml round-bottomed flasks first, use magnetic at room temperature
Power blender stirs 30 min.Then it is small to be dissolved in 0.08 g citric amide fluorescence being uniformly mixed in 20 ml absolute ethyl alcohols
Molecule and 1 ml ethyl orthosilicates (TEOS) are slowly dropped in above-mentioned mixed solution.After stirring 8 h, centrifugation, washing, and in
130 DEG C of dryings obtain fluorescent silicon dioxide microballoon in two hours.
（3）Fluorescent silicon dioxide microspheres solution is prepared by solvent of deionized water, concentration is 4 μ g/ml, is detected
Fe3+0 ~ 80 μM of concentration range.A length of 360 nm of optimum excitation wave is set, the fluorescence intensity of recording solution is with Fe3+Concentration variation diagram
Spectrum.Its detection is limited to 20 nM, 0 ~ 25 μM of the range of linearity.
Example IV
（1）Prepare citric amide fluorescent small molecule
1 g anhydrous citric acids and 1.5 ml thionyl chlorides are placed in the flask full of nitrogen, 14 h are stirred at -20 DEG C.
Then by gained lemon acyl chlorides, revolving purification three times, removes excessive thionyl chloride, obtains pure lemon acyl chlorides.Again by lemon
Lemon acyl chlorides is dissolved in 40 ml tetrahydrofurans, is added dropwise 3.8 ml AEAPMS under stirring condition the reaction was continued 6 h, it is glimmering to obtain citric amide
Light small molecule crude product.By gained citric amide small molecule crude product with the purification of petroleum ether revolving three times, pure citric amide is obtained
Fluorescent small molecule.
（2）Prepare fluorescent silicon dioxide microballoon
60 ml absolute ethyl alcohols, 5 ml water and 4 ml ammonium hydroxide are sequentially added in 250 ml round-bottomed flasks first, use magnetic force at room temperature
Blender stirs 30 min.Then it is dissolved in 0.10 small point of g citric amide fluorescence being uniformly mixed in 20 ml absolute ethyl alcohols
Son and 1.5 ml ethyl orthosilicates (TEOS) are slowly dropped in above-mentioned mixed solution.After stirring 7 h, centrifugation, washing, and in
150 DEG C of dryings obtain fluorescent silicon dioxide microballoon in two hours.
（3）Fluorescent silicon dioxide microspheres solution is prepared by solvent of deionized water, concentration is 3 μ g/ml, is detected
Fe3+0 ~ 80 μM of concentration range.A length of 360 nm of optimum excitation wave is set, the fluorescence intensity of recording solution is with Fe3+Concentration variation diagram
Spectrum.Its detection is limited to 42.7 nM, 0 ~ 40 μM of the range of linearity.
Embodiment five
（1）Prepare citric amide fluorescent small molecule
1 g anhydrous citric acids and 1.2 ml thionyl chlorides are placed in the flask full of nitrogen, 10 h are stirred at 20 DEG C.So
Afterwards by gained lemon acyl chlorides, revolving purification three times, removes excessive thionyl chloride, obtains pure lemon acyl chlorides.Again by lemon
Acyl chlorides is dissolved in 40 ml tetrahydrofurans, is added dropwise 3.5 ml AEAPMS under stirring condition the reaction was continued 4 h, obtain citric amide fluorescence
Small molecule crude product.By gained citric amide small molecule crude product with the purification of petroleum ether revolving three times, it is glimmering to obtain pure citric amide
Light small molecule.
（2）Prepare fluorescent silicon dioxide microballoon
65 ml absolute ethyl alcohols, 7 ml water and 4 ml ammonium hydroxide are sequentially added in 250 ml round-bottomed flasks first, use magnetic force at room temperature
Blender stirs 30 min.Then it is dissolved in 0.08 small point of g citric amide fluorescence being uniformly mixed in 20 ml absolute ethyl alcohols
Son and 1.7 ml ethyl orthosilicates (TEOS) are slowly dropped in above-mentioned mixed solution.After stirring 6 h, centrifugation, washing, and in
140 DEG C of dryings obtain fluorescent silicon dioxide microballoon in two hours.
（3）Fluorescent silicon dioxide microspheres solution is prepared by solvent of deionized water, concentration is 5 μ g/ml, is detected
Fe3+0 ~ 80 μM of concentration range.A length of 360 nm of optimum excitation wave is set, the fluorescence intensity of recording solution is with Fe3+Concentration variation diagram
Spectrum.Its detection is limited to 32.4 nM, 0 ~ 35 μM of the range of linearity.
Embodiment six
（1）Prepare citric amide fluorescent small molecule
1 g anhydrous citric acids and 1.4 ml thionyl chlorides are placed in the flask full of nitrogen, 11h is stirred at 30 DEG C.So
Afterwards by gained lemon acyl chlorides, revolving purification three times, removes excessive thionyl chloride, obtains pure lemon acyl chlorides.Again by lemon
Acyl chlorides is dissolved in 40 ml tetrahydrofurans, is added dropwise 3.8 ml AEAPMS under stirring condition the reaction was continued 6 h, obtain citric amide fluorescence
Small molecule crude product.By gained citric amide small molecule crude product with the purification of petroleum ether revolving three times, it is glimmering to obtain pure citric amide
Light small molecule.
（2）Prepare fluorescent silicon dioxide microballoon
110 ml absolute ethyl alcohols, 15ml water and 3 ml ammonium hydroxide are sequentially added in 250 ml round-bottomed flasks first, use magnetic at room temperature
Power blender stirs 30 min.Then it is dissolved in small point of 0.15g citric amide fluorescence being uniformly mixed in 20 ml absolute ethyl alcohols
Son and 0.8 ml ethyl orthosilicates (TEOS) are slowly dropped in above-mentioned mixed solution.After stirring 8 h, centrifugation, washing, and in
115 DEG C of dryings obtain fluorescent silicon dioxide microballoon in two hours.
（3）Fluorescent silicon dioxide microspheres solution is prepared by solvent of deionized water, concentration is 8 μ g/ml, is detected
Fe3+0 ~ 80 μM of concentration range.A length of 360 nm of optimum excitation wave is set, the fluorescence intensity of recording solution is with Fe3+Concentration variation diagram
Spectrum.Its detection is limited to 0.12 μM, 0 ~ 50 μM of the range of linearity.
Applicant states that the present invention illustrates the detailed process equipment of the present invention and technological process by above-described embodiment,
But the invention is not limited in above-mentioned detailed process equipment and technological process, that is, it is above-mentioned detailed not mean that the present invention has to rely on
Process equipment and technological process could be implemented.Person of ordinary skill in the field it will be clearly understood that any improvement in the present invention,
The addition of equivalence replacement and auxiliary element to each raw material of product of the present invention, selection of concrete mode etc., all fall within the present invention's
Within protection domain and the open scope.
Claims (7)
1. a kind of fluorescent silicon dioxide method for preparing microsphere of Quantitative detection iron ion, it is characterised in that including following step
Suddenly：
（1）Prepare citric amide fluorescent small molecule
Anhydrous citric acid and thionyl chloride are added in tetrahydrofuran, after the reaction was complete, pure lemon acyl is made in revolving purification
Chlorine, then the normal-temperature reaction in tetrahydrofuran by obtained lemon acyl chlorides and aminoethylaminopropyl methyl dimethoxysilane, revolves
After steaming purification, citric amide fluorescent small molecule is made；
（2）Prepare fluorescent silicon dioxide microballoon
By ethyl orthosilicate, citric amide fluorescent small molecule, deionized water, ammonium hydroxide by certain mass than being added to alcohols and water
In the mixed solvent is fully reacted, and is filtered, is washed, pulverizing after drying, fluorescent silicon dioxide microballoon is made.
2. a kind of fluorescent silicon dioxide method for preparing microsphere of Quantitative detection iron ion as claimed in claim 1, it is special
Sign is step（2）The particle diameter of the fluorescent silicon dioxide microballoon is 100 ~ 300 nm.
3. a kind of fluorescent silicon dioxide method for preparing microsphere of Quantitative detection iron ion as claimed in claim 1, it is special
Sign is step（2）The ethyl orthosilicate, citric amide fluorescent small molecule, deionized water, ammonium hydroxide are by certain mass than 1：
(0.02~0.2)：(8~12)：(2~4).
4. a kind of fluorescent silicon dioxide method for preparing microsphere of Quantitative detection iron ion as claimed in claim 1, it is special
Sign is step（2）The alcohols is ethanol, methanol, isopropanol etc.；The volume ratio of alcohols and water (8 ~ 12):1.
5. a kind of fluorescent silicon dioxide method for preparing microsphere of Quantitative detection iron ion as claimed in claim 1, it is special
Sign is step（2）The fluorescent silicon dioxide microballoon needs that 4 ~ 10 h of reaction is stirred at room temperature.
6. a kind of fluorescent silicon dioxide method for preparing microsphere of Quantitative detection iron ion as claimed in claim 1, it is special
Sign is step（2）The fluorescent silicon dioxide microballoon needs dry at 0 ~ 150 DEG C.
7. a kind of fluorescent silicon dioxide method for preparing microsphere of Quantitative detection iron ion as claimed in claim 1, it is special
Sign is that the microspheres solution detection of configuration fluorescent silicon dioxide is used for Fe3+When, using deionized water as solvent, concentration is 1 ~ 10 μ g/ml.
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|---|---|---|---|---|
| US4983369A (en) * | 1989-11-22 | 1991-01-08 | Allied-Signal Inc. | Process for forming highly uniform silica spheres |
| US5480582A (en) * | 1993-06-30 | 1996-01-02 | Pope; Edward J. A. | Process for synthesizing amorphous silica microspheres with fluorescence behavior |
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| CN105400510A (en) * | 2015-12-15 | 2016-03-16 | 辽宁师范大学 | Self-fluorescent silica microsphere material and preparation method and application thereof |
| CN105693532A (en) * | 2016-01-21 | 2016-06-22 | 济南大学 | Preparation method of fluorescent ammonia carboxylate |
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2017
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| US4983369A (en) * | 1989-11-22 | 1991-01-08 | Allied-Signal Inc. | Process for forming highly uniform silica spheres |
| US5480582A (en) * | 1993-06-30 | 1996-01-02 | Pope; Edward J. A. | Process for synthesizing amorphous silica microspheres with fluorescence behavior |
| CN103992789A (en) * | 2014-05-26 | 2014-08-20 | 江苏大学 | Preparation method of inorganic-organic composite fluorescent microsphere |
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Application publication date: 20180424 |