Mercury ion detection probe, and preparation method and application thereof

A technology for detecting probes and mercury ions, applied in chemical instruments and methods, fluorescence/phosphorescence, organic chemistry, etc., can solve the problems of expensive instruments and troublesome sample processing, and achieve low detection limit, sensitive recognition, and strong specificity Effect

Active Publication Date: 2019-05-03
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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  • Mercury ion detection probe, and preparation method and application thereof
  • Mercury ion detection probe, and preparation method and application thereof
  • Mercury ion detection probe, and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Synthesis of fluorescent probe of the present invention

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

[0044]

[0045] (1) Preparation of intermediate compound 2

[0046] Take compound 1 and o-aminothiophenol dissolved in dimethyl sulfoxide (DMSO), the ratio of the amount of the compound 1 and o-aminothiophenol is 1:1, heated at 60 degrees for 6 hours, TLC monitoring During the reaction process, when the reaction is complete, the reactants are cooled to room temperature, water is added, and 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°C for 10 hours. The solid product in the reaction solution is filtered and separated. Washed with anhydrous ethanol three times to obtain a yellow sol...

Embodiment 2

[0051] Ratio Fluorescence Probe Molecular Working Curve

[0052] Take 2 mL of the prepared aqueous dispersion solution of fluorescent probe molecules and 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 60 min, the fluorescence spectrometer records the change of fluorescence intensity at 455nm. Take the fluorescence intensity as the ordinate and the copper ion concentration as the abscissa to plot, and fit the working curve of the ratio fluorescent probe molecule. In this example, the ratio fluorescent probe is used to determine 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 value of fluorescence intensity decreases with increasing mercury ion concentration.

Embodiment 3

[0054] Fluorescent probe molecular cation selective determination

[0055] Take 2 mL of the aqueous dispersion solution of the ratio fluorescent probe molecules prepared in Example 2, and add 20 μL of 0.01M Li + , 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 is left for 60 minutes, the fluorescence spectrometer records the change in fluorescence intensity at 445 nm. Experimental results show that, except for mercury ions, other ions did not cause a significant change in fluorescence at 445 nm, indicating that the probe molecule of the present invention has good selectivity. In this example, the fluorescent probe molecules are selectively determined. Under the excitation of 375nm excitation light, the relationship between the fluorescence intensity and the changes of different ions is shown in figure 2 Shown.

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Abstract

The invention discloses a mercury ion detection probe based on intramolecular hydrogen bond structural units, and a preparation method and an application thereof, wherein the fluorescent probe has thestructure as the formula (I). With 5-formylsalicylaldehyde being a raw material, firstly a benzothiazole derivative is generated with o-aminobenzenethiol; and then condensation is carried out with barbituric acid. The probe has stable optical performance and is high in detection sensitivity and low in detection limit on the mercury ion, wherein response range is 2-20.0 [mu]M. The probe has greatselectivity and has no response on silver ion, barium ion, calcium ion, lithium ion, sodium ion, potassium ion, magnesium ion, aluminum ion, nickel ion, zinc ion, mercury ion, cobalt ion, lead ion, palladium ion and strontium ion. The fluorescence molecular probe has practical application value in the fields of detection on the mercury ion in biochemistry and environmental chemistry.

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 a preparation method and application thereof. Background technique [0002] Mercury, a highly toxic heavy metal element, is 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 finally 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 a strong attack on the groups containing sulfur, oxygen, nitrogen and other electron donors in the body. Its neurotoxic effects include: (a ) Damage to the antioxidant properties of cells; (b) directly affect the ion exchange inside and outside neurons; (c) destroy the...

Claims

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Application Information

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Patent Type & Authority Applications(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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