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Preparation method of rare earth metal organic framework fluorescent probe and application of rare earth metal organic framework fluorescent probe in detection of trivalent arsenic

A fluorescent probe and organic framework technology, applied in the field of fluorescence sensing, to achieve the effect of ultra-sensitive and selective fluorescence detection

Active Publication Date: 2018-06-22
NANCHANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although Ln-MOFs fluorescent sensing materials have been used in the detection of inorganic metal ions, anions, organic small molecule pollutants, and explosives, there is no report on the construction of fluorescent probes using Ln-MOFs for the detection of As(III).

Method used

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  • Preparation method of rare earth metal organic framework fluorescent probe and application of rare earth metal organic framework fluorescent probe in detection of trivalent arsenic
  • Preparation method of rare earth metal organic framework fluorescent probe and application of rare earth metal organic framework fluorescent probe in detection of trivalent arsenic
  • Preparation method of rare earth metal organic framework fluorescent probe and application of rare earth metal organic framework fluorescent probe in detection of trivalent arsenic

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Experimental program
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Effect test

Embodiment 1

[0018] Preparation of Rare Earth Metal Organic Framework Fluorescent Probes

[0019] (1) Preparation of 2,5-dimethylmercaptoterephthalic acid: add 2.99g potassium permanganate, 1.0g 2,5-dibromo-p-xylene and 1.5g diatomaceous earth to 50mL water and 50mL tert-butanol In the mixed solution, stir mechanically at 100°C for 36 hours, after cooling to 70°C, slowly add ethanol dropwise until the solution turns from red to brown, collect the filtrate by filtration, concentrate to 20mL at 60°C, add 10mL concentrated hydrochloric acid to acidify, filter , washed with ethanol, the white solid was collected and dried in vacuo; 0.25 g of the dried white solid was dissolved in N,N-dimethylformamide (DMF), 0.14 g of sodium methyl mercaptide was added, and stirred at room temperature for 10 minutes. Then extract with chloroform, wash with water, dry over anhydrous magnesium sulfate, and finally dry under vacuum at 60°C to obtain a yellow powder, which is made into 2,5-dimethylmercaptoterephth...

Embodiment 2

[0024] Interaction mechanism between Ce-MOFs and As(III)

[0025] The interaction mechanism between Ce-MOFs and As(III) was characterized by means of TEM, scattering spectroscopy, fluorescence spectroscopy, UV-visible absorption spectroscopy and infrared spectroscopy. Depend on image 3 A shows that when As(III) is added to Ce-MOFs, the Ce-MOFs nanoparticles originally dispersed in the solution aggregate, which may be due to the interaction between Ce-MOFs and As(III) that brings Ce-MOFs closer. Distance between MOFs. The interaction between Ce-MOFs and As(III) was characterized by dynamic light scattering spectroscopy and fluorescence spectroscopy ( image 3 B), the dynamic light scattering intensity of Ce-MOFs is small (curve b), and when As(III) is added to Ce-MOFs, the dynamic light scattering intensity is enhanced (curve a), indicating that Ce-MOFs and As(III) Coordination aggregation occurs and the particle size increases. In addition, Ce-MOFs have a strong emission ...

Embodiment 3

[0028] Application of Ce-MOFs to As(III) Detection

[0029] Add 20 μL of As(III) solutions of different concentrations to 10 μL of 4 mg / mL rare earth metal organic framework fluorescent probe solution, dilute the total volume of the solution to 200 μL with ultrapure water, incubate at room temperature for 40 minutes, and measure the solution when the excitation wavelength is 280 nm. of fluorescence. Depend on Figure 4 It can be seen that as the concentration of As(III) increases, the fluorescence intensity of Ce-MOFs decreases gradually, and the concentration of As(III) is related to the fluorescence intensity of the fluorescent probe (1-F / F 0 , F is the fluorescence intensity of Ce-MOFs in the presence of As(III), F 0 is the fluorescence intensity of Ce-MOFs) shows good linearity in the range of 1ppb-80ppb, and the detection limit is 0.65ppb, which can be used for ultrasensitive detection of As(III) in water samples.

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Abstract

The invention discloses a preparation method of a rare earth metal organic framework fluorescent probe and application of the rare earth metal organic framework fluorescent probe in detection of trivalent arsenic, belonging to the technical field of fluorescent sensing. The rare earth cerium metal organic framework fluorescent probe is prepared by adopting a simple solvothermal method taking 2,5-dimethylmercaptophthalic acid as a ligand and using lanthanide-series luminous ion cerium as central ions. When the trivalent arsenic exists, the carboxyl group and methyl mercapto group in the fluorescent probe are effectively coordinated with the trivalent arsenic under the action of arsenic-oxygen and arsenic-sulfur, so that the dispersed fluorescent probes in the solution are aggregated, the effective intersystem crossing between the ligand in the fluorescent probe and the central ion, cerium ion, is weakened by means of pi-pi stacking action induced by the aggregation, and the fluorescenceof the fluorescent probe is further weakened. With the increase of the concentration of the trivalent arsenic, the fluorescence emission peak intensity of the fluorescent probe gradually decreases, so that the sensitive fluorescence detection of the trivalent arsenic is realized.

Description

technical field [0001] The invention relates to a preparation method of a rare earth metal organic framework fluorescent probe and its application in the detection of trivalent arsenic, belonging to the technical field of fluorescent sensing. Background technique [0002] Arsenic is widely distributed on the earth, is a carcinogenic toxic substance, and even has a great poisonous effect on human health at trace levels. Arsenic exists mainly in the form of inorganic arsenic in drinking water, among which trivalent arsenic (As(III)) is the most toxic. Therefore, many new methods for detecting As(III) have emerged at the historic moment. However, the low sensitivity of common colorimetric methods and the strong acidity of the detection bottom solution of most electrochemical methods often limit the practical application of the above methods. Fluorescence methods are characterized by high sensitivity, rapidity, and simple operation. However, most fluorescence methods are based ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G83/00C09K11/06G01N21/64
CPCC08G83/008C09K11/06C09K2211/182G01N21/643
Inventor 邱建丁杨佳乐梁汝萍
Owner NANCHANG UNIV
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