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Rapid high-selectivity fluorine ion colorimetric probe and preparation method therefor

A technology of colorimetric probes and fluoride ions, which is applied in chemical instruments and methods, color-changing fluorescent materials, color/spectral characteristic measurement, etc., can solve the problems of limited application and development, poor reproducibility of fluoride-ion selective electrodes, and sensitivity of capillary electrophoresis Low-level problems, to achieve the effect of simple synthesis

Inactive Publication Date: 2015-12-09
杭州百裕生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although there are many methods for detecting fluoride ions, unfortunately, the low sensitivity of capillary electrophoresis, the poor reproducibility of fluoride ion selective electrodes, and the high cost of fluoride ion NMR severely limit its application and development.

Method used

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  • Rapid high-selectivity fluorine ion colorimetric probe and preparation method therefor
  • Rapid high-selectivity fluorine ion colorimetric probe and preparation method therefor
  • Rapid high-selectivity fluorine ion colorimetric probe and preparation method therefor

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Experimental program
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Effect test

Embodiment 1

[0024]

[0025] (Scheme 1) Dissolve 174mg (1.0mmol) 2-cyanobenzothiazole, 361mg (1.0mmol) 4-tert-butyldiphenylsilyloxybenzaldehyde and 50μL triethylamine in 20mL ethanol, at 25°C After stirring and reacting for 8 hours, the crude product was obtained by filtration under reduced pressure, and then separated by column chromatography using a mixed system of dichloromethane and petroleum ether (v / v, 1:1) to obtain 310 mg of a light yellow pure product with a yield of 60%.

[0026] (Scheme 2) Dissolve 174mg (1.0mmol) 2-cyanobenzothiazole, 542mg (1.5mmol) 4-tert-butyldiphenylsilyloxybenzaldehyde and 50μL triethylamine in 20mL ethanol, at 25°C After stirring and reacting for 8 hours, the crude product was obtained by filtration under reduced pressure, and then separated by column chromatography using a mixed system of dichloromethane and petroleum ether (v / v, 1:1) to obtain 372 mg of a light yellow pure product with a yield of 72%.

[0027] 1 H-NMR (400MHz, CDCl 3 )δ(*10 -6 ):1...

Embodiment 2

[0029] The inventor of the present invention has carried out following test: (a) the impact of different concentration NaF (0~200 μ M) on probe (10 μ M) absorption spectrum; 2,4,6,8,10,15,20,30,40,60μM). The above measurements were performed in acetonitrile, and all spectral measurements were made at 25°C after NaF addition for 20 min. See results figure 1 .

[0030] From figure 1 It can be seen that with the increase of NaF concentration in the probe solution, the absorption spectrum gradually increases, and has a good linear relationship with the absorption value in the range of 0-60 μM NaF concentration. Therefore, the probe of the present invention can more accurately determine the content of fluoride ions in the blood sample to be tested or in the environment.

Embodiment 3

[0032] Effect of different analytes (100 μM) on the absorption spectra of probes (10 μM). Analytes include: Chloride Cl - , bromide ion Br - , iodide ion I - , Sulfate ion SO 4 2- , nitrate ion NO 3 - , nitrite ion NO 2 - , Thiocyanate ion SCN - and fluoride ion F - , and their concentration is 100 μM. All test conditions were performed in acetonitrile and all spectra were measured at 25°C after 20 min of analyte addition. Pipette 50 μL of the probe stock solution (1 mM) into a 5 mL colorimetric tube, then add 3 mL of acetonitrile, then pipette 50 μL of the above analyte stock solution (10 mM) into the colorimetric tube, and then dilute to 5 mL with acetonitrile. Shake well, let it stand for 20min, then measure. The result is as figure 2 shown.

[0033] From figure 2 It can be seen that the probe has high selectivity to fluoride ions and can specifically react with fluoride ions. In acetonitrile solution, compared with other analytes, the absorption spectrum ...

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Abstract

The invention relates to a rapid high-selectivity fluorine ion colorimetric probe and a preparation method therefor. The probe not only can highly selectively recognize fluorine ions, but also can quantitatively and qualitatively analyze the fluorine ions by way of observation in naked eyes. The probe can be used for quickly responding to the fluorine ions, so that the fluorine ions can be immediately detected. The probe is stable in property, and can be stored and used for a long time. In addition, the probe further can be used for quantitatively analyzing the fluorine ions by virtue of absorption spectroscopy and has relatively strong anti-interference capacity. The probe is synthesized by a room temperature method, requires only one step reaction, and is simple to synthesize.

Description

technical field [0001] The invention relates to a colorimetric probe for fluoride ions, its preparation method and its application for rapid and high-selectivity recognition of fluoride ions. Background technique [0002] In the environment and organisms, anions are ubiquitous. They exist in the air, water and soil in the environment, and in the organs, cells, and even the cell fluid of the human body. They play an extremely important role in the environment and ecosystem. important role. As the smallest anion, fluoride ion is an essential element for biological life activities, and plays an important role in dental health care and osteoporosis treatment. In order to contain sufficient fluoride ions in the human body, people use it as an important additive, often used in toothpaste, medicine and drinking water. However, excessive fluorine not only has toxic effects on aquatic organisms and plants, but also causes serious human health problems. For example, higher concentr...

Claims

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Application Information

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IPC IPC(8): C09K9/02C07F7/18G01N21/78G01N21/31
Inventor 叶龙武郭艳
Owner 杭州百裕生物科技有限公司
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