Mercury ion analysis fluorescent probe and preparation method and application thereof

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, and achieve good stability and simple synthesis , the effect of reducing the impact

Inactive Publication Date: 2017-11-10
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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  • Mercury ion analysis fluorescent probe and preparation method and application thereof
  • Mercury ion analysis fluorescent probe and preparation method and application thereof
  • Mercury ion analysis fluorescent probe and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Embodiment 1: preparation formula 5 and formula 8 compounds

[0037] Dissolve 11.2 g of hexamethylenetetramine shown in formula 4 in 20 mL of trifluoroacetic acid, then add 2.16 g of p-cresol shown in formula 3, the molar ratio of the two is 4:1, 100 °C Heating to reflux for 6 hours, and shading treatment, after the reaction, the product was added to ice water, and after the solid was precipitated, suction filtration was performed to obtain the pure product Formula 5.

[0038]

[0039] Formula 3 Formula 4 Formula 5

[0040] Take 656 mg shown in Formula 5 and dissolve in 20 mL of absolute ethanol, then add 500 mg of aminobenzenethiol shown in Formula 6, the molar ratio of the two is 1:1, stir at room temperature, and add dropwise during the stirring process 1184 mg of 37% hydrochloric acid and 2720 mg of 30% hydrogen peroxide were reacted for 30 min, and then filtered by suction to obtain the pure product Formula 8.

[0041]

[0042] Formula 6 Formula 5 Formula...

Embodiment 2

[0044]

[0045] Formula 8 Formula 9 Formula 2

[0046] (Scheme 1) Dissolve 374 mg (1 mmol) of the compound of formula 8 prepared in Example 1 in 10 mL of dichloromethane, add 129 mg (1 mmol) of DIPEA, and then add 173 mg (1 mmol) of benzene thiochloroformate The ester was refluxed at 50° C. for 10 h, and then subjected to suspension evaporation using a rotary evaporator to obtain a solid, which was the crude product of the compound represented by Formula 2. If you want to get a purer product, you can use a mixed system of dichloromethane and petroleum ether (for example, v / v, 1:1) to obtain 423.3 mg of an orange pure product by silica gel column chromatography. The rate is 83%.

[0047](Scheme 2) Dissolve 374 mg (1 mmol) of the compound of formula 8 prepared in Example 1 in 10 mL of dichloromethane, add 387 mg (3 mmol) of DIPEA, and then add 519 mg (3 mmol) of benzene thiochloroformate The ester was refluxed at 50° C. for 10 h, and then subjected to suspension evaporati...

Embodiment 3

[0054] Using the compounds of Scheme 5, probes were prepared. Weigh 5 mg of the compound represented by formula 2 into a colorimetric tube, add 1 mL of dichloromethane, shake well to dissolve the probe, and then dilute to 10 mL with absolute ethanol to prepare a 1 mM probe. Needle stock solution.

[0055] The prepared probe was used for detection, and the fluorescence detection method was as follows: add 5 mL of absolute ethanol to the colorimetric tube, pipette 50 µL of the probe stock solution (1 mM) into the colorimetric tube, add 2- Add 3mL of distilled water, then add 0.5mL of 4-hydroxyethylpiperazineethanesulfonic acid (HEPES), then dilute to 10mL with distilled water, pipette 200 µL of mercury ion solution (1 mM) into the colorimetric tube. Shake well, and after 20 min, measure the fluorescence spectrum with a fluorescence spectrophotometer (Horiba FluoroMax-4).

[0056] Test results such as figure 1 shown.

[0057] figure 1 It is the fluorescence spectrum of the ...

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Abstract

The present invention relates to a fast and highly selective mercury ion fluorescent probe. The mercury ion fluorescent probe is a sulfocarbonate compound, and the structural formula is as shown in the specification. The mercury ion fluorescent probe can achieve at least one of the following technical effects: highly selective identification of mercury ions; rapid response to the mercury ions; large Stokes shift; stable nature, long term preservation and use; and strong anti-interference ability.

Description

technical field [0001] The invention relates to a thiocarbonate compound used as a fluorescent probe for analyzing mercury ions and a preparation method, which can rapidly and sensitively identify mercury ions with high selectivity, or can measure the concentration of mercury ions in a sample. Background technique [0002] Mercury is a silvery white shiny heavy liquid, chemically stable, insoluble in acid and alkali. Mercury can evaporate at room temperature, and mercury vapor and mercury compounds are highly toxic (chronic). Mercury is widely used in the manufacture of scientific measuring instruments (such as thermometers, etc.), medicines, electrodes, catalysts, etc. Mercury is ubiquitous in nature. Generally, animals and plants contain trace amounts of mercury. Therefore, there are trace amounts of mercury in our food, which can be metabolized through excretion and hair without affecting health. [0003] Mercury is a heavy metal pollutant with strong biological toxicit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D277/66C09K11/06G01N21/64
CPCC07D277/66C09K11/06C09K2211/1037G01N21/6428
Inventor 徐征和徐晶朱宝存孔珂丛鑫温家华
Owner UNIV OF JINAN
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