Fluorescent probe for identifying mercury ions and preparation and identification method thereof

A fluorescent probe and identification method technology, applied in chemical instruments and methods, fluorescence/phosphorescence, luminescent materials, etc., can solve the problems of high detection cost, time-consuming, complex sample processing, etc., and achieve the effect of simple operation and low detection cost

Active Publication Date: 2019-06-25
GUIZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the sensitivity of these methods is relatively high, they all have the disadvantages of high detection cost, complicated sample processing, time-consuming, and are not suitable for real-time and on-site detection.

Method used

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  • Fluorescent probe for identifying mercury ions and preparation and identification method thereof
  • Fluorescent probe for identifying mercury ions and preparation and identification method thereof
  • Fluorescent probe for identifying mercury ions and preparation and identification method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Embodiment 1: A kind of fluorescent probe that recognizes mercury ion, the molecular formula of probe is: C 34 h 31 BrN 4 o 2 , the structural formula of the probe is attached figure 1 Shown; NMR spectrum as attached figure 2 shown.

Embodiment 2

[0042] Embodiment 2: a kind of preparation method of the probe described in embodiment 1, the steps are as follows:

[0043] (1) Add 1g of 4-bromobenzaldehyde in 15mL of ethanol to obtain A;

[0044] (2) Add 1.21g of 2-acetylpyridine, 0.9g of potassium hydroxide and 15mL of ammonia water to 20mL of ethanol to obtain the B substance;

[0045] (3) Mix substance A and substance B, stir at 2°C for 1 hour, and reflux at 80°C for 20 hours, then cool to room temperature and stir for 45 minutes, filter the precipitate, and recrystallize in acetic acid to obtain substance C;

[0046] (4) Mix 300mg 4-pyridineethylene, 60mg palladium acetate, 200mg triphenylphosphine and 20cm 3 Triethylamine, seal the mixture under N 2 In a high-pressure reaction flask under atmosphere, react at 110°C for 70 h, dissolve the product in chloroform, wash the organic phase with distilled water for 3 times, then wash the organic phase with saturated saline for 3 times, dry with anhydrous magnesium sulfate f...

Embodiment 3

[0048] Embodiment 3: a kind of preparation method of the probe described in embodiment 1, the steps are as follows:

[0049] (1) Add 0.5g of 4-bromobenzaldehyde in 15mL of ethanol to obtain A;

[0050] (2) Add 1g of 2-acetylpyridine, 0.5g of potassium hydroxide and 10mL of ammonia water to 20mL of ethanol to obtain material B;

[0051] (3) Mix substance A and substance B, stir at 0°C for 3 hours, and reflux at 70°C for 30 hours, then cool to room temperature and stir for 30 minutes, filter the precipitate, and recrystallize in acetic acid to obtain substance C;

[0052] (4) Mix 250mg 4-pyridineethylene, 50mg palladium acetate, 150mg triphenylphosphine and 15cm 3 Triethylamine, seal the mixture under N 2 In a high-pressure reaction flask under atmosphere, react at 100°C for 65 h, dissolve the product in chloroform, wash the organic phase twice with distilled water, then wash the organic phase twice with saturated brine, dry over anhydrous magnesium sulfate for 0.5 h, and spin...

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Abstract

The invention discloses a fluorescent probe for identifying mercury ions and a preparation method and an identification method thereof. The preparation method comprises the following steps: firstly dissolving 4-bromobenzaldehyde in ethanol so as to obtain a; dissolving 2-acetylpyridine, potassium hydroxide and ammonia water in ethanol to obtain b; mixing the a and the b, carrying out reacting to obtain a precipitate, filtering the precipitate, and recrystallizing the precipitate in acetic acid to obtain c; mixing the c , 4-pyridine ethylene, palladium acetate and triphenylphosphine into triethylamine to obtain a mixture, and sealing the mixture in a high-pressure reaction flask under N2 atmosphere for reaction, dissolving a product in chloroform, performing spin-drying, and recrystallizingwith ethanol to obtain d; and dissolving the d into N, N-dimethylformamide, then adding 6-bromohexanoic acid to react, adding diethyl ether into the reaction solution until the reaction solution is completely precipitated, carrying out suction filtration, washing twice with diethyl ether, and drying to obtain the fluorescent probe for identifying the mercury ions. The fluorescent probe can realize qualitative and quantitative analysis of the mercury ions, and has the characteristics of low identification cost, simplicity in operation, visual result, high sensitivity, good selectivity and thelike.

Description

technical field [0001] The invention relates to a fluorescent probe and its preparation method and identification method, in particular to a fluorescent probe for identifying mercury ions and its preparation method and identification method. Background technique [0002] Mercury is one of the most dangerous metal pollutants. It is a typical heavy metal ion with strong toxicity and can cause permanent damage to the biological nervous system. Mercury in the environment is oxidized into water-soluble divalent mercury ions in the air. Once mercury ions enter the water environment, they will be converted into organic methylmercury by bacterial microorganisms, and quickly accumulate in organisms such as fish to enter food chain. Methylmercury damages the human nervous system, causing brain damage, cognitive and motor disorders, etc. The "Minamata disease" that shocked the world is a type of organic mercury poisoning. Therefore, the development of highly selective, highly sensiti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/04C09K11/06G01N21/64
Inventor 周桂林粟绍媛王攀张晓东倪新龙
Owner GUIZHOU UNIV
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