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Gold ion fluorescent probe based on o-aminopyridine nitrile compound and preparation method thereof

A technology of o-aminopyridine nitrile and fluorescent probe, which is applied in the field of symmetrical o-aminopyridine nitrile compound fluorescent probe and preparation thereof, can solve the problems of complicated steps and high cost, and achieve the effect of high detection sensitivity

Inactive Publication Date: 2015-07-15
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In summary, gold plays an important role in human production and life, but the existing gold exploration methods generally have the disadvantages of high cost and cumbersome steps.

Method used

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  • Gold ion fluorescent probe based on o-aminopyridine nitrile compound and preparation method thereof
  • Gold ion fluorescent probe based on o-aminopyridine nitrile compound and preparation method thereof
  • Gold ion fluorescent probe based on o-aminopyridine nitrile compound and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0022] The preparation of example example 1 gold ion fluorescent probe

[0023] Add 20ml of ethanol and 10ml of water into a 100ml round bottom flask, add 10mmol of naphthalene formaldehyde, 20mmol of malononitrile, and 15mmol of concentrated ammonia water under stirring. The mixture is heated and stirred at 50°C for 5 hours with magnetic stirring at room temperature. After the reaction was completed, it was directly filtered to obtain a solid crude product. Recrystallized from THF and acetone,

[0024] White crystals (I) were obtained, and the single crystal structure of compound I was as follows figure 1 , the yield is about 75% (mother liquor recovery), m.p.>300°C. The synthetic route of naphthyl formaldehyde and malononitrile, ammoniacal liquor is:

[0025]

[0026] The spectral characterization data of product (I) is: 1 H NMR (400MHz, DMSO-d 6 )δ:8.05-8.10(3H,m,Ar-H),7.59-7.67(4H,m,Ar-H),7.33(4H,s,NH 2 ); 13 C NMR (100MHz, DMSO-d 6 ),(ppm):160.8(2C),158.9,133,1...

Embodiment 3

[0029] Example 3 Fluorescent probes for quantitative fluorescence detection of gold ions

[0030] Add 10uL of fluorescent probe stock solution and 0-100uL of gold ion aqueous solution to different 10mL colorimetric tubes (the concentration of gold ion stock solution is 1*10 -2mol / L) and make up to 10 mL with deionized water. The concentration of fluorescent probe after constant volume is 1*10 -5 mol / L, gold ion concentration is 2*10 -7 mol / L*10 -4 mol / L. Transfer 3 mL of the working solution to a 1 cm fluorescence cuvette to record the fluorescence spectrum and record the fluorescence intensity at 446 nm. Drawing the relationship between the change of fluorescence intensity and the concentration of gold ions, the concentration of gold ions can be quantitatively detected according to the change trend of fluorescence intensity, and the detection limit of gold ions is 39.4ug / ml. The fluorescence spectrum as a function of gold ion concentration is as follows Figure 4 shown....

Embodiment 4

[0031] Example 4 Interference experiment of other metal ions on the detection of gold ions by fluorescent probes

[0032] Add 10uL of fluorescent probe stock solution to different 10mL colorimetric tubes, the concentration of 100uL is 1*10 -2 mol / L of other interfering metal ions Au 3+ , Cu 2+ , Al 3+ , Zn 2+ , Pb 2+ , Ag + , Cu + , Hg 2+ , Ni 2+ , Ca 2+ , Cd 2+ , Co 2+ , Fe 2+ , Mn 2+ , Mg 2+ , Na + , K + Aqueous solution, then add 100ul respectively to the concentration of 1*10 -2 mol / L gold ion aqueous solution, and make up to 10 mL with deionized water. The concentration of fluorescent probe after constant volume is 1*10 -5 mol / L, the concentration of gold ions and other metal ions is 1*10 -4 mol / L. Transfer 3 mL of the working solution to a 1 cm fluorescence cuvette to record the fluorescence spectrum. The excitation and emission wavelengths are 334 nm and 446 nm, respectively. The recorded fluorescence intensity is plotted against different metal ion...

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Abstract

The invention relates to a symmetrical o-aminopyridine nitrile compound fluorescent probe for detecting gold ions and a preparation method thereof. The structural formula of the o-aminopyridine nitrile compound is shown as a formula I which is as shown in the specification. The preparation method comprises the following steps: stirring and synthesizing naphthaldehyde, malononitrile and ammonium water by a one-pot method at 50 DEG C in the presence of a methanol-water mixed solution; after reaction for 3-5 hours, filtering and recrystallizing to obtain the o-aminopyridine nitrile compound fluorescent probe. The fluorescent probe provided by the invention is simple in preparation process, good in stability, high in selectivity to gold ions, strong in interference resistance by other metal ions, quick to respond and good in sensitivity. The detection limit is 39.4 milligram / ml which meets the national detection standard, so that the fluorescent probe is an ideal fluorescent probe for field detection of gold ions in gold ores.

Description

(1) Technical field [0001] The invention belongs to the field of fluorescent probes and preparation thereof, in particular to a fluorescent probe of a symmetrical o-aminopyridinenitrile compound used for detecting gold ion content and a preparation method thereof. (2) Background technology [0002] Gold is a popular precious metal that has been used as money for centuries and thousands of years. In recent years, gold has gradually shown more and more important applications in food additives, medical treatment, electronics industry, etc. . Due to the excellent electrical conductivity and oxidation resistance of gold, it also has important applications in the electronics industry: in communication equipment, spacecraft, jet engines, etc., gold is used as a connector for electronic measuring instruments Gold plating to prevent oxidation; at the same time, gold or gold alloys are also used in scanning electron microscopes to increase the measurement accuracy of the sample posi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D213/85C09K11/06G01N21/64
Inventor 李加荣杨俊娟史大昕张奇
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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