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Preparation method of metal complex fluorescence probe for detecting hydrogen sulfide and application thereof

A metal complex and fluorescent probe technology, applied in the field of analytical chemistry, to achieve the effects of good selectivity, good sensitivity analysis, and good photostability

Active Publication Date: 2018-11-16
WEST ANHUI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

And through the fluorescent switch mechanism, solve the problem of the relationship between the fluorescent signal output and the concentration of hydrogen sulfide in the reaction process

Method used

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  • Preparation method of metal complex fluorescence probe for detecting hydrogen sulfide and application thereof
  • Preparation method of metal complex fluorescence probe for detecting hydrogen sulfide and application thereof
  • Preparation method of metal complex fluorescence probe for detecting hydrogen sulfide and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0028] A method for preparing a metal complex fluorescent probe, the method steps are as follows:

[0029] S1: Add 0.1g dansyl chloride and 80μL triethylamine into a round bottom flask containing 8mL of dichloromethane, then add 0.0043g chloroethylamine hydrochloride, under the protection of nitrogen, stir at room temperature for 0.5h , remove the methylene chloride solvent with a rotary evaporator to obtain a yellow oil;

[0030] S2: Then the obtained substance was separated in petroleum ether with silica gel column: ethyl acetate=4:1, R f =0.42 under the conditions of separation and purification to obtain the product Ds-1;

[0031] S3: Weigh 0.06g of the Ds-1 product and place it in 2mL of DMF to dissolve, then add 0.03g of furan-2-ylmethyl-pyridin-2-ylmethyl-amine and 0.02g of anhydrous potassium carbonate, and stir at room temperature for 22h Finally, 12mL of ice water was added to the reaction mixture, a large amount of precipitate was formed, and the precipitate solid ...

Embodiment 2

[0034] S1: Add 0.1500g of dansyl chloride and 117μL of triethylamine into a round bottom flask containing 10mL of dichloromethane, then add 0.0065g of chloroethylamine hydrochloride, under the protection of nitrogen, stir at room temperature for 1h, The dichloromethane solvent was removed with a rotary evaporator to obtain a yellow oil;

[0035] S2: Then the obtained substance was separated in petroleum ether with silica gel column: ethyl acetate=4:1, R f =0.42 under the conditions of separation and purification to obtain the product Ds-1;

[0036] S3: Weigh 0.0625g of the Ds-1 product and place it in 3mL of DMF to dissolve, then add 0.0376g of furan-2-ylmethyl-pyridin-2-ylmethyl-amine and 0.0276g of anhydrous potassium carbonate, and stir at room temperature for 24h Finally, 15 mL of ice water was added to the reaction mixture, a large amount of precipitate was formed, and the precipitate solid was obtained by filtration, and then the resulting substance was separated and pu...

Embodiment 3

[0039] S1: Add 0.2g dansyl chloride and 160μL triethylamine into a round bottom flask containing 12mL of dichloromethane, then add 0.0086g chloroethylamine hydrochloride, under the protection of nitrogen, stir at room temperature for 1.5h , remove the methylene chloride solvent with a rotary evaporator to obtain a yellow oil;

[0040] S2: Then the obtained substance was separated in petroleum ether with silica gel column: ethyl acetate=4:1, R f =0.42 under the conditions of separation and purification to obtain the product Ds-1;

[0041] S3: Weigh 0.07g of the Ds-1 product and place it in 4mL of DMF to dissolve, then add 0.04g of furan-2-ylmethyl-pyridin-2-ylmethyl-amine and 0.04g of anhydrous potassium carbonate, and stir at room temperature for 26h Finally, 18mL of ice water was added to the reaction mixture, a large amount of precipitate was formed, and the precipitate solid was obtained by filtration, and then the resulting substance was separated and purified with a sili...

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Abstract

The invention discloses a preparation method of a metal complex fluorescence probe for detecting hydrogen sulfide. A dansyl chloride derivative has large stokes shift and relative high quantum yield,a synthetic route is simple, and the probe has good light stability; the probe contains a polydentate ligand, and by coordinating with copper ions, the stable dansyl chloride copper metal complex probe is generated. The copper complex probe has good sensitivity analysis on hydrogen sulfide, and has good selectivity on hydrogen sulfide.

Description

technical field [0001] The invention relates to the technical field of analytical chemistry, in particular to a method for preparing a fluorescent probe of a metal complex. Background technique [0002] Since the reform and opening up, with the rapid development of economy, the rapid development of industrial level, and the remarkable improvement of human living standards, it has also brought a series of environmental problems. Among them, the problem of air pollution is particularly serious, including sulfur oxides, nitrogen oxides, and hydrocarbons. Compounds, carbon monoxide and other gas pollution. For example, hydrogen sulfide H 2 S--a poisonous polluting gas, colorless, foul-smelling, highly toxic and flammable. It mainly comes from the manufacturing process of sulfur, sulfuric acid, dyes and cosmetics, as well as the decomposition process of microorganisms. A small amount of hydrogen sulfide can irritate the respiratory tract and cause dizziness, headache, throat d...

Claims

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Application Information

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IPC IPC(8): C07F1/08C09K11/06G01N21/64
CPCC07F1/005C09K11/06C09K2211/1029C09K2211/1088C09K2211/188G01N21/6428
Inventor 闫叶寒陈丽娟傅绪成戴娃子王慧慧郑玉王素华
Owner WEST ANHUI UNIV
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