Colorimetric fluorescence probes used for analyzing mercury ions, and preparation method and application of colorimetric fluorescence probe

A technology of fluorescent probes and mercury ions, which is applied in the analysis of materials, fluorescence/phosphorescence, material excitation analysis, etc., can solve the problems of insufficient response speed, complex synthesis, and insufficient selectivity, etc., and achieves sensitive and synthetic mercury ions. Simple, water-soluble effect

Inactive Publication Date: 2017-10-27
UNIV OF JINAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are still some problems with the fluorescent probes reported so far, including insufficient selectivity, insufficient response speed, and complex synthesis.

Method used

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  • Colorimetric fluorescence probes used for analyzing mercury ions, and preparation method and application of colorimetric fluorescence probe
  • Colorimetric fluorescence probes used for analyzing mercury ions, and preparation method and application of colorimetric fluorescence probe
  • Colorimetric fluorescence probes used for analyzing mercury ions, and preparation method and application of colorimetric fluorescence probe

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Embodiment 1: preparation formula 3 and formula 4 compound

[0044] Get 244 mg of p-Hydroxybenzaldehyde shown in Formula 6 and dissolve it in 15 mL of methylene chloride, then add 519 mg of phenyl thiochloroformate shown in Formula 5, the molar ratio of the two is 1:1.5, at 120 mg N, Under the catalysis of N-diisopropylethylamine (DIPEA), stir at room temperature for 10 h, and then perform suction filtration to obtain the pure product of formula 3.

[0045]

[0046] Formula 5 Formula 6 Formula 3

[0047]Get 306 mg of 3-OH-3-CH3-2 butanone shown in formula 7 and dissolve it in pyridine, add 2-3 drops of acetic acid, then add 396 mg of malononitrile shown in formula 8, the molar ratio of the two is 1 : 2, react 24h in 25 ℃ of oil baths, carry out suction filtration then, obtain pure product formula 4

[0048]

[0049] Formula 7 Formula 8 Formula 4

Embodiment 2

[0051]

[0052] Formula 3 Formula 4 Formula 2

[0053] (Scheme 1) Dissolve 199 mg (1 mmol) of the carbonate compound represented by formula 3 in 15 mL of absolute ethanol, add a tablet of piperazine (86 g / mol), and then add 258 mg (1 mmol) of the compound represented by formula 4 The nitrile shown was stirred at room temperature for 10 h, and then subjected to suction filtration to obtain 364.8 mg of pure product with a yield of 83%.

[0054] (Scheme 2) Dissolve 198 mg (1 mmol) of the carbonate compound represented by formula 3 in 15 mL of absolute ethanol, add a tablet of piperazine (86 g / mol), and then add 337 mg (1.3 mmol) of the compound represented by formula 4 The nitrile shown was stirred at room temperature for 10 h, and then subjected to suction filtration to obtain 400.0 mg of pure product with a yield of 91%.

[0055] (Scheme 3) Dissolve 198 mg (1 mmol) of the carbonate compound represented by formula 3 in 15 mL of absolute ethanol, add a tablet of piperazin...

Embodiment 3

[0063] The detection method of absorption spectrum is: add 1mL of absolute ethanol to the colorimetric tube, pipette 50 µL of the probe stock solution (1mM) into the colorimetric tube, add 4-6mL of distilled water, and then add 0.5 mL of phosphate buffer Saline solution PBS, then distilled water to 10mL, pipette 200 µL of mercury ion solution (1 mM) into the colorimetric tube. Shake well, and after 40min, measure the absorption spectrum with an ultraviolet-visible spectrophotometer (UV-3101PC).

[0064] Test results such as figure 1 with figure 2 shown.

[0065] figure 1 It is the fluorescence spectrum of the probe (5µM) before and after adding Hg2+ (20µM). We can see that the fluorescence change is very obvious through the illustration.

[0066] figure 2 It is the absorption spectrum of the probe (5 µM) before and after adding Hg2+ (20 µM). Through the illustration, we can clearly see the change of the absorption spectrum, and through the color change, it can be ob...

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Abstract

The invention relates to high-selectivity mercury ion colorimetric fluorescence probes. Specifically, the probes provided by the invention are thiocarbonate compounds, and the compounds can be used as the mercury ion colorimetric fluorescence probes for detecting mercury ions. The structure formula of the compounds is described in the description. The probes can realize at least one of the technical effects of realizing high selective identification of the mercury ions, more rapidly responding to the mercury ions, being good in water solubility, being stable in properties and being stored for a long time, and having higher anti-interference ability.

Description

technical field [0001] The invention relates to a thiocarbonate compound as a fluorescent probe of mercury ions, which can identify mercury ions with high selectivity and sensitivity, or it can measure the concentration of mercury ions in a sample. Background technique [0002] Mercury is the only liquid metal at normal temperature and pressure. It is a relatively rare element in the earth's crust. A very small amount of mercury exists in the state of simple metal in the natural state. Mercury has many uses, not only can be used to make measuring instruments, such as thermometers, sphygmomanometers, etc.; it can also be used to make pesticides; it can also be used to extract other precious metals (gold) from mineral deposits, etc. [0003] However, mercury is a heavy metal element, and its harm to the environment and human body cannot be ignored. The main sources of mercury pollution include the combustion of solid waste, wastewater from instrument factories, smelting preci...

Claims

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Application Information

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IPC IPC(8): C07D307/68C09K11/06G01N21/64
CPCC07D307/68C09K11/06C09K2211/1007C09K2211/1088G01N21/643
Inventor 徐征和徐晶朱宝存徐立荣桑国庆于潇
Owner UNIV OF JINAN
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