Preparation and visual detection method of a core-shell magnetic multicolor fluorescent probe

A fluorescent probe, core-shell technology, applied in the field of nanocomposite material preparation, can solve the problems of low yield and poor specificity, achieve the effect of fast response time, moderate price, and eliminate data errors

Active Publication Date: 2019-08-16
HENAN POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The problem in the prior art that the present invention solves is that the detection of a single rare earth ion to DPA is easily interfered by other molecules and ions, resulting in poor specificity, low yield, and limited application; it is hoped to study a method that uses cheap and easy The natural mineral halloysite with excellent performance is used as a probe for the matrix. By synthesizing magnetic kaolin, a magnetic matrix is ​​obtained, which can effectively improve the separation efficiency of the material and the recycling rate of the material; because halloysite has a tubular structure, and the tube The inside has a positive charge, which is easy to adsorb anionic dyes, and the magnetic ferric iron tetroxide is attached to the outside of the tube. The natural barrier of halloysite can effectively avoid the influence of magnetic substances on fluorescence, and effectively introduce fluorescent internal standard molecule fluorescein. ;Using the magnetic halloysite adsorbed with fluorescein molecules as the fluorescent internal standard, the detection of DPA is realized by the fluorescence ratiometric method, and the data distortion caused by photobleaching, probe loading and retention and equipment factors is solved and eliminated; Realize the high sensitivity and specific recognition of DPA, effectively prevent the interference of other molecules and ions; realize the visual detection of DPA, through the change of fluorescent color, the concentration of DPA can be determined initially, laying the foundation for the realization of practical application

Method used

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  • Preparation and visual detection method of a core-shell magnetic multicolor fluorescent probe
  • Preparation and visual detection method of a core-shell magnetic multicolor fluorescent probe
  • Preparation and visual detection method of a core-shell magnetic multicolor fluorescent probe

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Effect test

Embodiment 1

[0036] A preparation method of a rare earth-doped core-shell magnetic multicolor fluorescent probe, comprising the following steps:

[0037] The first step, magnetic halloysite to adsorb fluorescein: weigh 0.8g magnetic halloysite (Fe 3 o 4 -Hal) 0.08g, polyvinylpyrrolidone (PVP) and 0.01g of luminescent dye fluorescein (FL), after uniform mixing, grind, then add 15mL of deionized water, and stir for 4 hours; then put into the reaction vessel , placed in an oven, and reacted at a temperature of 160°C for 10 hours; then cooled to room temperature, and the product was taken out for centrifugation, washed with absolute ethanol for 3 times during the centrifugation process, and vacuum-dried at 60°C to obtain the first step Product Fe 3 o 4 -Hal-fluorescein;

[0038] The second step is to absorb amino groups to make a protective film: take 0.2g of the product in the first step and dissolve it in 60mL of absolute ethanol; add 100uL of a mixture of APTES and TEOS in a ratio of 1:...

Embodiment 2

[0041] A preparation method of a rare earth-doped core-shell magnetic multicolor fluorescent probe, comprising the following steps:

[0042] The first step, magnetic halloysite to adsorb fluorescein: weigh 1g of magnetic halloysite (Fe 3 o 4 -Hal), 0.1g polyvinylpyrrolidone (PVP) and 0.05g luminescent dye fluorescein (FL), after uniform mixing, grind, then add 15mL of deionized water, and stir for 5 hours; then put into the reaction vessel, Put it into an oven and react at a temperature of 180°C for 8 hours; then cool to room temperature, take out the product for centrifugation, wash it with absolute ethanol three times during the centrifugation process, and dry it in vacuum at 60°C to obtain the product of the first step;

[0043] The second step is to absorb amino groups to make a protective film: take 0.2g of the product in the first step and dissolve it in 60mL of absolute ethanol; while the product is stirring, add 100uL of a mixture of APTES and TEOS in a ratio of 1:2, ...

Embodiment 3

[0046] A preparation method of a rare earth-doped core-shell magnetic multicolor fluorescent probe, comprising the following steps:

[0047] The first step, magnetic halloysite to adsorb fluorescein: weigh 1.5g magnetic halloysite (Fe 3 o 4 -Hal), 0.15g polyvinylpyrrolidone (PVP) and 0.08g luminescent dye fluorescein (FL), after uniform mixing, grinding treatment, then add 25mL of deionized water, and stir for 6 hours; then put into the reaction vessel , placed in an oven, and reacted at a temperature of 200°C for 7 hours; then cooled to room temperature, and the product was taken out for centrifugation, washed with absolute ethanol three times during the centrifugation process, and vacuum-dried at 60°C to obtain the product of the first step Fe 3 o 4 -Hal-fluorescein;

[0048] The second step is to absorb amino groups to make a protective film: take 0.25g of the product in the first step and dissolve it in 60mL of absolute ethanol; add 200uL of a mixture of APTES and TEOS...

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Abstract

The invention belongs to the technical field of nano composite material preparation, and particularly relates to preparation of a core-shell type magnetic multi-color fluorescent probe and a visible detection method. The preparation of the rare-earth doped core-shell type magnetic multi-color fluorescent probe comprises the following steps: (1) loading fluorescein to magnetic halloysite by using a hydrothermal method, wherein the magnetic halloysite can show green fluorescence under a three-purpose ultraviolet analyzer; (2) to prevent the fluorescein from leaking out from the magnetic halloysite, dropping ammonium hydroxide into a mixed liquid of APTES+TEOS, and performing a reaction to substance hydroxyl of the product by amino so as to form a layer of a protection membrane; (3) grafting an ethylenediamine tetraacetic acid derivative, performing coordination with rare-earth ions to form a chelate compound, thereby obtaining the fluorescent probe. The invention further relates to a visible detection method. Fluorescent testing on DPA of detected substances of different concentrations is carried out after the fluorescent probe is mixed with a Tris-HCl buffer solution, and multi-color fluorescent variations show the recognition performance of the fluorescent probe.

Description

technical field [0001] The invention belongs to the technical field of preparation of nanocomposite materials, and in particular relates to a preparation and visual detection method of a rare earth-doped core-shell magnetic nanometer multicolor fluorescent probe. Background technique [0002] Anthrax is an acute infectious disease that spreads between humans and animals and is mainly caused by Bacillus anthracis. The bacteria enter the human body through the respiratory tract and damaged skin, first multiply locally, and then produce toxins that cause hemorrhagic infiltration, necrosis, and high edema in tissues and organs, forming primary cutaneous anthrax, intestinal anthrax, and pulmonary anthrax. The exploration of Bacillus anthracis is a hotspot in the scientific community, and the current research method is the detection of DPA (2,6-pyridine dicarboxylic acid), because DPA is the core component of spores. Commonly used methods include high performance liquid chromatog...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/06C09K11/02G01N21/64
CPCC09K11/02C09K11/06C09K2211/1088C09K2211/182G01N21/6428G01N21/6486
Inventor 孙俊岭徐君吴信科白万备张琳琳胡文亮郭凯沈晓科
Owner HENAN POLYTECHNIC UNIV
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