CN108642546B - Preparation method and application of rare earth nanosheet fluorescent thin film sensor - Google Patents
Preparation method and application of rare earth nanosheet fluorescent thin film sensor Download PDFInfo
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- CN108642546B CN108642546B CN201810348891.8A CN201810348891A CN108642546B CN 108642546 B CN108642546 B CN 108642546B CN 201810348891 A CN201810348891 A CN 201810348891A CN 108642546 B CN108642546 B CN 108642546B
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D13/00—Electrophoretic coating characterised by the process
- C25D13/02—Electrophoretic coating characterised by the process with inorganic material
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D13/00—Electrophoretic coating characterised by the process
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6486—Measuring fluorescence of biological material, e.g. DNA, RNA, cells
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Abstract
The invention discloses a method for manufacturing a rare earth nanosheet fluorescent thin film sensorThe fluorescent film sensor prepared by the method is a rare earth nanosheet modified by an organic ligand plated with a PS film, and is prepared by (Y)0.95Eu0.05O)+The method comprises the steps of preparing a nanosheet film by using a single-layer nanosheet sol as a raw material through an electrophoretic deposition method, preparing the nanosheet film modified by an organic ligand through an immersion method, and plating a layer of hydrophobic polymer film by using an SYDC-200 type immersion lifting coating machine to obtain the fluorescent film sensor, wherein the sensor can detect the bilirubin content. The fluorescent film sensor prepared by the invention has the characteristics of convenient operation, high sensitivity and strong stability.
Description
Technical Field
The invention relates to a chemical synthesis material technology and application thereof, in particular to a preparation method and application of a rare earth nanosheet fluorescent thin film sensor.
Background
In recent years, it has been found that the nano-luminescent material can detect metal ions, inorganic molecules and small organic molecules, and can also measure and analyze biological macromolecules. The rare earth metal has abundant electronic energy levels, and part of the rare earth metal not only has excellent magnetic property, but also has excellent fluorescence property.
Bilirubin in human serum (plasma) is a metabolite of heme in the body, and has wide clinical application. The improved J-G method, the bilirubin oxidase method, the dimethyl sulfoxide method, the vanadate oxidation method and the like are used for measuring the bilirubin content, wherein the improved J-G method and the dimethyl sulfoxide method are not as good as the linear effects of the two methods, the enzyme method is not strong in practicability due to the high cost of enzyme reagents, the problems of enzyme sources, purity, stability and the like, and the vanadate oxidation method has good precision, but is relatively complex in operation, stable in preparation, good in effect and simple in operation, so that bilirubin detection by using a sensor becomes a key point of attention.
Disclosure of Invention
The invention aims to prepare a rare earth nanosheet fluorescent thin film sensor which can be used for detecting bilirubin content.
The specific technical scheme for realizing the purpose of the invention is as follows:
a preparation method of a rare earth nanosheet fluorescent thin film sensor comprises the following specific steps:
Step 1: placing the ITO conductive glass in a deposition electrophoresis apparatus, regulating the voltage to 60-90V, carrying out electrophoresis for 5-15 minutes, and obtaining (Y)0.95Eu0.05O)+Depositing the nanosheets on ITO glass to form a nanosheet film;
Step 2: dipping the ITO conductive glass plated with the nanosheet film in a 3-15% thenoyl trifluoroacetone (HTTA) solution for 3-10 minutes, taking out, drying at room temperature, dipping in the 3-15% solution again, and repeating the steps for three times to obtain the rare earth nanosheet film modified by the organic ligand;
And step 3: dissolving high molecular Polystyrene (PS) by using trichloromethane, and preparing 1-10% of high molecular Polystyrene (PS) solution; and (3) fixing the ITO glass coated with the rare earth nanosheet film modified by the organic ligand on a dipping and pulling coating machine, pulling for 5-15 minutes at the speed of 1000-2500ms/s by using the dipping and pulling coating machine, and drying at room temperature to obtain the rare earth nanosheet fluorescent film sensor.
The application of the rare earth nanosheet fluorescent film sensor in determination of bilirubin concentration is characterized in that bilirubin is dripped into the rare earth nanosheet fluorescent film sensor, the fluorescence of the sensor decreases along with the increase of bilirubin concentration, and the logarithm value of fluorescence attenuation proportion and the logarithm value of bilirubin concentration are in a linear relationship.
(Y) according to the invention0.95Eu0.05O)+Nanosheet sols, preparable in reference to Synthesis and chromatography of GdO + nanosheets with Tm, Advanced Materials Research,2014,1058:40-43。
The invention has the beneficial effects that:
(1) And preparing the rare earth nanosheet fluorescent thin film sensor.
(2) the sensor is combined with bilirubin with different concentrations to change fluorescence intensity, and the bilirubin concentration and the fluorescence intensity are in a linear relation, so that the sensor can be used as a fluorescence probe to detect the bilirubin content.
Drawings
FIG. 1 shows (Y) obtained in example 1 of the present invention0.95Eu0.05O)+TEM image spectrum of the nanosheet;
FIG. 2 is a graph showing the change of fluorescence intensity of the nanosheet fluorescent thin-film sensor prepared in example 1 of the present invention under the effect of different concentrations of bilirubin;
FIG. 3 is a linear relationship diagram between the fluorescence intensity of the nanosheet fluorescent thin film sensor prepared in example 1 of the present invention under the effect of different concentrations of bilirubin and bilirubin concentration.
Detailed Description
the invention is described in detail below with reference to the figures and examples.
Example 1
a) 1g of 5% Eu doped yttrium oxide Y is taken2O3Eu (5%), adding 2.1617g NH4br; both were then ground thoroughly and homogeneously in a mortar.
b) And (b) transferring the mixture obtained in the step a into a crucible, compacting, putting into a muffle furnace, keeping the temperature for 2 hours at 450 ℃, then heating to 700 ℃, keeping the temperature for 2 hours, and cooling to room temperature to obtain a 5% Eu-doped YOBr sample.
c) placing 1g of 5% Eu-doped YOBr sample in 200ml of sodium benzoate solution, placing the mixture in a microwave oven under high fire (microwave output power is 700W) for 2 minutes, taking out ice water for cooling, cooling to room temperature, placing in the microwave oven under high fire for 2 minutes, cooling, circulating for 20 times, washing the obtained sample with water, washing with ethanol, and performing suction filtration to obtain Y after ion exchange between benzoate and bromide ions0.95Eu0.05OC6H5COO。
d) Taking 1g of Y from step c0.95Eu0.05OC6H5Placing COO sample in 200ml n-butanol, ball milling at 300r/min for 8 hr, centrifuging at 4000r/min for 15min to obtain (Y)0.95Eu0.05O)+Nanosheet sol, the nanosheet TEM spectrum of which is shown in figure 1.
e) taking 10ml of (Y)0.95Eu0.05and (3) electroplating the nanosheet sol for 10 minutes by using an electrophoretic deposition instrument to enrich the nanosheets on the ITO glass, and drying at room temperature to form the nanosheet film.
f) Dissolving 1g of HTTA in 20ml of alcohol to prepare a 5% HTTA solution, soaking the ITO glass plated with the nanosheet film in the 5% HTTA solution for 10 minutes, taking out the ITO glass, drying the ITO glass at room temperature, soaking the ITO glass in the 5% HTTA solution again, and repeating the steps for 3 times to obtain the HTTA coordinated nanosheet film.
g) And (3) dissolving 0.6g of Polystyrene (PS) in 20ml of chloroform to prepare a 3% PS solution, soaking the ITO glass obtained in the step f) for 10min at the speed of 2500ms/s by using an SYDC-200 type dipping and pulling film coating machine, and drying at room temperature to prepare the rare earth nanosheet fluorescent film sensor.
And (3) dripping bilirubin with different concentrations on the prepared rare earth nanosheet fluorescent film sensor, and measuring the fluorescence intensity of the fluorescent film sensor at the concentrations. The results are shown in FIG. 2 and FIG. 3, the fluorescence intensity decreases with the increase of bilirubin concentration, and the logarithm of the fluorescence attenuation ratio is in linear relation with the logarithm of bilirubin concentration.
Claims (3)
1. A preparation method of a rare earth nanosheet fluorescent thin film sensor is characterized by comprising the following specific steps:
Step 1: placing the ITO conductive glass in a deposition electrophoresis apparatus, regulating the voltage to 60-90V, carrying out electrophoresis for 5-15 minutes, and obtaining (Y)0.95Eu0.05O)+depositing the nanosheets on ITO glass to form a nanosheet film;
Step 2: dipping the ITO conductive glass plated with the nanosheet film in a 3-15% thenoyl trifluoroacetone (HTTA) solution for 3-10 minutes, taking out, drying at room temperature, dipping in the 3-15% solution again, and repeating the steps for three times to obtain the rare earth nanosheet film modified by the organic ligand;
And step 3: dissolving high molecular Polystyrene (PS) with chloroform to obtain 1-10% high molecular Polystyrene (PS) solution; fixing the ITO glass coated with the rare earth nanosheet film modified by the organic ligand on a dipping, pulling and coating machine, pulling for 5-15 minutes at the speed of 1000-2500ms/s, and drying at room temperature to obtain the rare earth nanosheet fluorescent film sensor.
2. Use of a rare earth nanosheet fluorescent thin film sensor of claim 1 in non-disease diagnosis and treatment for determination of bilirubin concentration.
3. The application of claim 2, wherein bilirubin is dripped into the rare earth nanosheet fluorescent thin film sensor, the fluorescence of bilirubin decreases with the increase of the bilirubin concentration, and the logarithm value of the fluorescence attenuation ratio is in a linear relationship with the logarithm value of the bilirubin concentration.
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| JP2011506967A (en) * | 2007-12-10 | 2011-03-03 | バイエル・ヘルスケア・エルエルシー | Method and system for producing a reagent with reduced background current |
| CN101302229A (en) * | 2008-06-27 | 2008-11-12 | 北京化工大学 | Tetraheteropoly rare earth organic complex and preparation thereof |
| CN101382491B (en) * | 2008-09-25 | 2011-09-14 | 湖南大学 | Long life luminous nanometer bio probe for detecting pathogenic microorganism and preparing and detecting method thereof |
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