A kind of mercury ion detection probe and its preparation method and application

A technology for detecting probes and mercury ions, which is applied in the field of chemical analysis and detection, can solve the problems of expensive instruments and troublesome sample processing, and achieve the effects of low detection limit, sensitive recognition and strong specificity

Active Publication Date: 2022-05-03
HUNAN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The traditional detection methods for mercury ions include atomic absorption spectrometry, atomic fluorescence spectrometry and inductively coupled plasma mass spectrometry. Although they have high detection sensitivity, their disadvantages such as expensive instruments and troublesome sample processing limit their application.

Method used

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  • A kind of mercury ion detection probe and its preparation method and application
  • A kind of mercury ion detection probe and its preparation method and application
  • A kind of mercury ion detection probe and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Synthesis of fluorescent probes of the present invention

[0043] The preparation route of fluorescent probe of the present invention is as follows:

[0044]

[0045] (1) Preparation of intermediate compound 2

[0046] Dissolve compound 1 and o-aminothiophenol in dimethyl sulfoxide (DMSO), the ratio of the amount of compound 1 and o-aminothiophenol is 1:1, heat reaction at 60 degrees for 6 hours, TLC monitoring Reaction process, after the reaction is complete, the reactant is cooled to room temperature, added with water, then separated and extracted, dried, and then subjected to column chromatography to obtain compound 2;

[0047] (2) Preparation of fluorescent probe I

[0048] Dissolve compound 2 and barbituric acid in DMSO, the ratio of the amount of compound 1 to barbituric acid is 1:1, heat and stir at 70 degrees for 10 hours, filter and separate the solid product in the reaction solution, and then use Washing with absolute ethanol for 3 times, the compound I ...

Embodiment 2

[0051] Ratiometric Fluorescent Probe Molecular Working Curve

[0052] Take 2 mL of the prepared aqueous dispersion solution of ratiometric fluorescent probe molecules, add 20 μL of different concentrations (0, 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 15, 20, 50 μmol / L) Mercury iodide aqueous solution, after standing for 60 min, the fluorescence spectrometer records the change of fluorescence intensity at 455nm. Taking the fluorescence intensity as the ordinate and the copper ion concentration as the abscissa, the working curve of the ratio fluorescent probe molecule is obtained by fitting. In the present embodiment, the ratiometric fluorescent probe is used for measuring the concentration of copper ions. Under the excitation of 375nm excitation light, the relationship between the fluorescence intensity and the concentration of copper ions is as follows: figure 1 As shown, the fluorescence intensity value decreases with the increase of mercury ion concentration.

Embodiment 3

[0054] Fluorescent Probe Molecular Cation Selectivity Determination

[0055] Take 2mL of the water-dispersed solution of the ratio fluorescent probe molecule prepared in Example 2, add 20 μL of Li with a concentration of 0.01M + 、K + 、Na + 、Sr 2+ 、Ba 2+ , Mg 2+ , Ca 2+ , Zn 2+ 、Ni 2+ 、Co 2+ , Hg 2+ , Pb 2+ , Pd 2+ , Fe 2+ , Mn 2+ 、Al 3+ 、Cr 3 + 、Cd 2+ , Fe 3+ After the aqueous solution was left for 60 minutes, the fluorescence spectrometer recorded the change of the fluorescence intensity at 445nm. Experimental results show that, except for mercury ions, other ions do not cause obvious changes in the fluorescence at 445 nm, indicating that the probe molecules of the present invention have good selectivity. In this embodiment, the molecular selectivity of the fluorescent probe is measured, and the relationship diagram of the fluorescence intensity changing with different ions under the excitation of 375nm excitation light is as follows figure 2 shown.

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Abstract

The invention discloses a mercury ion detection probe based on an intramolecular hydrogen bond structural unit, a preparation method and an application thereof. The structure of the fluorescent probe is shown in formula I, which uses 5-formyl salicylaldehyde as a raw material, first forms a benzothiazole derivative with o-aminothiophenol, and then condenses with barbituric acid. The probe of the invention has stable optical properties, high detection sensitivity to mercury ions, low detection limit and a response range of 2-20.0 μM. Good selectivity, no silver ions, barium ions, calcium ions, lithium ions, sodium ions, potassium ions, magnesium ions, aluminum ions, nickel ions, zinc ions, mercury ions, cobalt ions, lead ions, palladium ions, strontium ions response. The fluorescent molecular probe of the invention has practical application value in fields such as the detection of mercury ions in biochemistry and environmental chemistry. (I).

Description

technical field [0001] The invention relates to the technical field of chemical analysis and detection, in particular to a mercury ion detection probe based on an intramolecular hydrogen bond structural unit and its preparation method and application. Background technique [0002] Mercury is a highly toxic heavy metal element, as highly toxic as cadmium and lead. The main forms of mercury include metallic mercury, inorganic and organic mercury compounds. Metallic mercury and inorganic mercury are eventually oxidized into water-soluble divalent mercury ions in the body to exert toxic effects. The damage of mercury ions to the nervous system of primates is mainly in the central nervous system. Mercury ions have strong attack power on groups containing electron donors such as sulfur, oxygen, nitrogen, etc. in the body, and its neurotoxic effects include: (a ) damage the antioxidant properties of cells; (b) directly affect the ion exchange inside and outside neurons; (c) destro...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D417/10C09K11/06G01N21/64
Inventor 赵云辉刘立华周智华
Owner HUNAN UNIV OF SCI & TECH
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