Preparation method of mercury ion rate probe based on rhodamine derivative and quantum dot fluorescent microsphere

A technology of fluorescent microspheres and derivatives, which is applied in chemical instruments and methods, fluorescence/phosphorescence, luminescent materials, etc., can solve the problems of uneconomical, complicated operation process, inconvenient detection of heavy metal ions, etc.

Inactive Publication Date: 2015-11-04
TIANJIN POLYTECHNIC UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Traditional methods for the detection of heavy metal ions, including chemical titration, atomic fluorescence, atomic absorption, atomic emission and ICP-MS, have many problems, such as complex operation process, not economical, etc., which bring a lot of inconvenience to the detection of heavy metal ions

Method used

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  • Preparation method of mercury ion rate probe based on rhodamine derivative and quantum dot fluorescent microsphere
  • Preparation method of mercury ion rate probe based on rhodamine derivative and quantum dot fluorescent microsphere
  • Preparation method of mercury ion rate probe based on rhodamine derivative and quantum dot fluorescent microsphere

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Experimental program
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Effect test

Embodiment 1

[0028] (1) Preparation of rhodamine derivatives: Dissolve 1.5g of rhodamine B in 30ml of anhydrous methanol, add 4.8ml of tris(2-aminoethyl)amine, heat and stir at reflux at 80°C, add 50ml after rotary evaporation of the solvent Dichloromethane and 100ml of secondary water were washed, filtered and spin-dried, and RHB-NH was obtained by silica gel column chromatography 2 (Eluant: CH 2 Cl 2 / MeOH / Et 3 N=40:2:1); the RHB-NH 2 Dissolve in toluene, add 0.2ml isocyanate propyltriethoxysilane and 0.4ml triethylamine, stir and reflux at 80°C, evaporate the solvent by rotary evaporation, and obtain rhodamine derivatives by silica gel column chromatography.

[0029] (2) Preparation of CdTe:Zn quantum dots: Add 0.285g of sodium borohydride and 0.32g of tellurium powder into 10ml of secondary water, react under nitrogen protection at 4°C for 8 hours to obtain sodium tellurium hydride; mix 0.114g of cadmium chloride, 0.682 Add zinc chloride and 0.105ml mercaptopropionic acid into 100m...

Embodiment 2

[0033] Mercury ion ratio probe for fluorescence detection of different concentrations of mercury ions in aqueous solution:

[0034] Weigh 2.383g of HEPES and dissolve it in 800ml of secondary water. After dissolving, adjust the pH with sodium hydroxide and adjust the volume to 1L to obtain a 10mmol / L HEPES buffer solution. Dilute the prepared mercury ion ratio probe dispersion with HEPES buffer solution (PH=7) in a certain ratio, and then use HEPES buffer solution (PH=7) to prepare a certain concentration of mercury ion solution and add it to the above probe dispersion. Make up to 2ml to measure the fluorescence intensity (excitation wavelength 400nm).

[0035] The fluorescence spectra of the mercury ion ratioprobe in response to different concentrations of mercury ions in aqueous solution are shown in Figure 4 ; Fluorescence intensity ratio (I 577 / I 521 ) changes with the concentration of mercury ions in the aqueous solution as shown in Figure 5 .

Embodiment 3

[0037] Selectivity of ratiometric probes for mercury ion detection:

[0038] Configure 1×10 respectively-2 mol / L Na + 、K + , Ca 2+ , Mg 2+ , Fe 2+ 、Co 2+ 、Ni 2+ 、Cu 2+ , Zn 2+ , pb 2+ 、Cd 2+ , Hg 2+ 、Al 3+ and other aqueous solutions, and dilute the above solutions to 1×10 -3 mol / L, 1×10 -4 mol / L, 1×10 -5 mol / L. The solvent is the 10mmol / L HEPES buffer solution configured above. Add the ratio probe dispersion to constant volume to measure the fluorescence intensity.

[0039] The selectivity of ratiometric probes for the detection of mercury ions in aqueous solutions is as follows: Figure 6 .

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Abstract

The invention relates to a preparation method of a mercury ion rate probe based on a rhodamine derivative and a quantum dot fluorescent microsphere. The preparation method comprises the steps of firstly, preparing a water-soluble quantum dot (CdTe:Zn) by using a water-phase synthesis method, and synthesizing a silicon dioxide nanoparticle by using a reverse-phase microemulsion method, wherein Zn<2+> is doped into the water-soluble quantum dot, the surface of the water-soluble quantum dot is provided with mercaptopropionic acid (MPA), and the quantum dot is doped into the silicon dioxide nanoparticle; then, preparing a lactamized rhodamine derivative with specific recognition capability for Hg<2+>, and modifying siloxy through aminopropyltriethoxysilane (APS) on the basis, so that the lactamized rhodamine derivative is connected with the silicon dioxide nanoparticle; and finally, grafting the rhodamine derivative onto the surface of the silicon dioxide nanoparticle to construct the mercury ion rate probe based on FRET. By using the probe, not only is the interference of the external environment to the optical property of the quantum dot reduced, but also the distance from an energy donor (the quantum dot) to an energy acceptor (the rhodamine derivative) is shortened, the energy transfer efficiency of FRET is increased, and furthermore the mercury ion detection sensitivity is enhanced.

Description

Technical field [0001] The invention is a fluorescent probe and its preparation field, which specializes in a preparation method based on the mercury ratio probe based on Rodin Ming derivatives and quantum dot fluorescent microspheres. Background technique [0002] The applications of fluorescent nano -sensors in biological testing, environmental monitoring, cell imaging, drug transmission, disease diagnosis and treatment have attracted widespread attention.The fluorescent resonance energy transfer mechanism provides us with a new method of building biology, chemical and physical sensors. Its unique spatial effects and spectral effects give these sensors prominent performance.For example, energy transfer can be used to design fluorescence ratio probes.Compared with single -signal fluorescence probes, the ratio probe effectively avoids the interference of probe concentration, probe environment, and stimulation intensity, and greatly improves the sensitivity and accuracy of the det...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/06C09K11/88C09K11/02G01N21/64
Inventor 张纪梅韩鑫田力张坤王瞳尧耿海康
Owner TIANJIN POLYTECHNIC UNIV
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