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Method for preparing highly selective colorimetric probe for detecting mercury ions in sample

A high-selectivity, sample-detecting technology, applied in chemical instruments and methods, measuring devices, compounds of Group 5/15 elements of the periodic table, etc., can solve the problems of high cost and complicated operation of detection methods

Active Publication Date: 2017-04-26
LESHAN NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, in practical applications, these detection methods are expensive and complicated to operate

Method used

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  • Method for preparing highly selective colorimetric probe for detecting mercury ions in sample
  • Method for preparing highly selective colorimetric probe for detecting mercury ions in sample
  • Method for preparing highly selective colorimetric probe for detecting mercury ions in sample

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Embodiment 1: the synthesis of fluorescent probe

[0023] The synthetic route and the method of mercury ion fluorescent probe of the present invention are as follows:

[0024]

[0025] Specifically, 7-hydroxycoumarin (0.49g, 3mmol) was dissolved in THF (2mL), and the solution of selenium powder (0.19g, 24mmol) in THF (5mL) was slowly added dropwise under nitrogen protection, and stirred at room temperature 10min, add diphenylphosphine chloride (0.53g, 24mmol) dissolved in a mixed solution of triethylamine (2mL) and THF (20mL), stir and react for 24h under nitrogen protection, spin to dry the solvent, add 25mL toluene with a water separator Backwash for 4 hours to remove the solid, spin the organic phase to dryness, and separate and purify the target product by column chromatography (dichloromethane: petroleum ether = 1:1) to obtain 1.01 g of red powder fluorescent probe with a yield of 52%. 1 H NMR (400MHz,D 2 O)δ7.77-7.68(m,6H),7.62(dd,J=10.9,4.0Hz,1H),7.55-7.43(m...

Embodiment 2

[0026] Embodiment 2: the preparation of reaction reagent

[0027] Probe stock solution and probe test solution: Accurately weigh 4.26 mg of the probe synthesized in Example 1, dissolve it with a small amount of dichloromethane, then transfer it into a 10mL volumetric flask, dilute to the mark with ethanol, and mix At this time, a probe stock solution with a concentration of 1 mmol / L was obtained. And take 1mL of the stock solution and add it to 100mL of ethanol, first add some deionized water, then add 5mL of PBS buffer solution (pH=7.4), continue to add deionized water to make the volume to 200mL, and obtain a probe of 5 μmol / L test fluid.

[0028] Mercury ion stock solution: Accurately weigh 32.46mg mercury nitrate (Hg(NO 3 ) 2 ), add deionized water to dissolve, and after the sample is completely dissolved, transfer it into a 10mL volumetric flask, set the volume to the mark, and mix well. The concentration of this solution is 10mmol / L. Take 1mL of the above solution an...

Embodiment 3

[0029] Embodiment 3: the mensuration of probe fluorescence spectrum

[0030] Take 15 10mL colorimetric tubes, and then number them, add 5μmol / L probe test solution 5mL, and then add 1mmol / L mercury ions in order of 0μL, 2.5μL, 5μL, 10μL, 12.5μL, 15μL , 17.5 μL, 20 μL, 22.5 μL, 25 μL, 30 μL, 35 μL, 40 μL, 45 μL, 50 μL, shake well. Take 4mL of the solutions in the above-mentioned 15 colorimetric tubes in a cuvette, and measure the fluorescence spectrum at 456nm.

[0031] In the probe synthesized in embodiment 1, add the change of fluorescence intensity of different concentrations of mercury ions, such as figure 1 shown. Along with the increase of mercury ion concentration, its fluorescence intensity is also increasing, when the concentration of mercury ion is greater than 4 μ mol / L, the fluorescence intensity of the synthesized probe in embodiment 1 is basically stable, and it can be seen that the concentration of mercury ion is in When the concentration of mercury ions is 0-4 ...

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Abstract

The invention relates to a method for preparing a highly selective colorimetric probe for detecting mercury ions in a sample. The method specifically comprises the following steps: dissolving 7-hydroxycoumarin in THF; dropwise adding a THF solution of selenium powder slowly under protection of nitrogen; stirring at room temperature; adding chlorodiphenylphosphine dissolved in a mixed solution of triethylamine and THF; stirring under protection of nitrogen for reaction; spin-drying the solvent; adding toluene and backwashing with a water separator; removing solids; spin-drying an organic phase; separating and purifying a target product through column chromatography. The probe synthesized in the invention specifically responds to mercury ions, is not affected by coexisting ions K<+>, Na<+>, Mg<2+>, Zn<2+>, Ni<2+>, Cr<3+>, Cd<2+>, Pb<2+> and Cu<+>, and has good selectivity to Hg<2+>.

Description

technical field [0001] The invention relates to a method for preparing a colorimetric probe, which can be used to detect the concentration or content of mercury ions in a sample. [0002] technical background [0003] Mercury is a volatile and highly toxic element. Once mercury enters the water body, mercury ions in the environment will be converted into organic mercury (such as methylmercury, etc.) by bacteria, and will always accumulate in the organism. Enrichment, and finally absorbed by humans and other animals such as birds to cause harm. Mercury and its derivatives can destroy the molecular structure of organisms, because mercury ions can combine with sulfur-containing groups in proteins and enzymes. Methylmercury, in particular, can seriously poison the nerves of animals, cause behavioral perception disorders of animals, poison nerves and kidneys, and pose a great threat to humans and other animals such as birds. [0004] Bird feathers and eggs have a high concentrat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/655C09K11/06G01N21/64
CPCC07F9/65522C09K11/06C09K2211/1088G01N21/643
Inventor 文陇英刘方庆杨佐忠邓加林赵文海
Owner LESHAN NORMAL UNIV
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