A fluorescent probe for detecting silver ions and its preparation method and application

A technology of fluorescent probes and silver ions, which is applied in the field of fluorescent probes for detecting silver ions, can solve problems such as fewer silver ion fluorescent probes, low sensitivity, and environmental hazards, and achieve easy scale production, high sensitivity, and low environmental impact Harmful effect

Active Publication Date: 2019-12-31
浙江工业大学上虞研究院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] At present, there are few effective silver-ion fluorescent probes, and there are generally disadvantages such as low selectivity, low sensitivity, interference by other metal ions, and slow response, and most silver-ion fluorescent probes are mainly composed of rhodamines and pyrenes. and the application process have greater environmental hazards

Method used

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  • A fluorescent probe for detecting silver ions and its preparation method and application
  • A fluorescent probe for detecting silver ions and its preparation method and application
  • A fluorescent probe for detecting silver ions and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment I-1

[0043] The preparation method of embodiment I-1 fluorescent probe I of the present invention, its steps comprise:

[0044] (1) Synthesis of indazole

[0045] Add 21.4g (200mmol) of o-methylaniline, 50mL (600mmol) of concentrated hydrochloric acid and 100mL of water into the reaction flask, stir at 0°C, add dropwise 13.8g (200mmol) of an aqueous solution of sodium nitrite, after the addition is complete Keep stirring at 0°C for 30 minutes; add sodium fluoroborate solution (24.2g (200mmol) dissolved in 100mL water), keep at 0°C for 2 hours, a large amount of white diazonium salt precipitates in the reaction bottle; pump the reaction solution at low temperature The diazonium salt was obtained by filtration, washed with 300 mL of ice-cold ethanol, and dried to obtain 28.5 g of the diazonium salt, with a yield of 46.1%.

[0046] Dissolve the diazonium salt in 50mL chloroform and add it to the reaction flask, stir at 0°C, add 19.8g (200mmol) potassium acetate solid in batches, retu...

Embodiment I-2

[0057] Spectral properties of embodiment 1-2 silver ion fluorescent probe 1 and various metal ions

[0058] The structure of fluorescent probe I is characterized in that it has a structural formula as shown in formula 9:

[0059]

[0060] Fluorescent probe I was prepared in tetrahydrofuran to 1.0 × 10 -5 mol / L mother liquor, packed in ten 5mL glass bottles. Ten metals (Ag(I), Li(I), Cu(II), Zn(II), Hg(II), Ni(II), Al(III), Fe(III), Cr(III)) The salt is dissolved in water, respectively dubbed 5.0×10 -3 mol / L metal salt solution. Add 10 μL of these 10 metal salt solutions to these 10 glass bottles, so that the final concentration of metal ions in each bottle is 1.0×10 -4 mol / L test sample. After ultrasonic vibration for 30 minutes, take the test sample and test its fluorescence emission spectrum under the excitation light wavelength of 450nm, the obtained results are as follows: figure 1 shown.

[0061] This experiment shows that the fluorescent probe 1 has high select...

Embodiment I

[0062] Embodiment I-3 Spectral properties of the reaction product of fluorescent probe I and silver ions.

[0063] The mother solution of fluorescent probe I in Example I-1 was filled into 10 5mL glass bottles respectively. Mix silver nitrate into 0.5×10 -3 mol / L, 1.0×10 -3 mol / L, 1.5×10 -3 mol / L, 2.0×10 -3 mol / L, 2.5×10 -3 mol / L, 3.0×10 - 3 mol / L, 3.5×10 -3 mol / L, 1.5×10 -3 mol / L, 4.0×10 -3 mol / L, 4.5×10 -3 mol / L and 5.0×10 -3 mol / L solution. Add 10 μL of these 10 concentrations of silver nitrate solutions to these 10 glass bottles, and these 10 bottles contain test samples with a molar ratio (metal ion: fluorescent probe) of 1:10 to 1:1. After ultrasonic vibration for 30 minutes, take the solution in the bottle and test its fluorescence emission spectrum under the excitation light wavelength of 450nm, the obtained results are as follows: figure 2 shown.

[0064] The experimental results showed that the fluorescence emission peak of fluorescent probe 1 reacted ...

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Abstract

The invention discloses a fluorescence probe for detecting a silver ion, and provides a preparation method and application thereof at the same time. The fluorescence probe can quickly respond and high-selectively detect the silver ion. The fluorescence probe for detecting the silver ion provided by the invention has a structure as shown in a formula 1. The probe provided by the invention can selectively react with the silver ion so as to produce fluorescence-emission red shift. The reaction is not interfered by other metal ions, a fluorescence-emission peak change can be produced within a short time, and the wave length of the fluorescence-emission peak red shift is in linear correlation with the concentration of the silver ion. The fluorescence probe provided by the invention only carriesout fluorescence reaction with the silver ion instead of other metal ions, so that the fluorescence probe has better selectivity and specificity.

Description

technical field [0001] The invention belongs to the technical field of fluorescent probe sensing in analytical chemistry, and relates to a fluorescent probe for detecting silver ions, a preparation method and an application thereof. Background technique [0002] Too high or too low metal ion content will cause serious consequences to organisms and the environment, especially heavy metals can cause cell pathology in animals, and the damage is particularly serious. Heavy metals are also very harmful to plants. Wastewater containing heavy metal ions is used to irrigate and fertilize farmland, which not only pollutes the soil, but also further pollutes the water body. Fluorescent probes are widely used in the detection of metal ions due to their high selectivity to specific metal ions. [0003] Fluorescent probes refer to molecules that can change the fluorescence signal (intensity or wavelength) when a certain physical or chemical property of a substance or system changes in a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D403/14C09K11/06G01N21/64
CPCC07D403/14C09K11/06C09K2211/1029C09K2211/1044G01N21/6402
Inventor 叶青许萌贾平胡圆圆朱博也刘效奇高建荣
Owner 浙江工业大学上虞研究院有限公司
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