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Preparation method of fast-respondability Hg2+developing fluorescence probe based on rhodamine B-thiophene derivative

A technology of thiophene derivatives and fluorescent probes, applied in fluorescence/phosphorescence, material analysis by optical means, measurement devices, etc. The binding effect of fluorescent probes is not ideal enough to achieve the effects of low detection limit, strong anti-interference ability and high sensitivity

Inactive Publication Date: 2016-04-13
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0011] However, most of the chromogenic-fluorescent probes of mercury ions that have been studied currently use the principle of complexing metal ions with organic groups, so most of the chromogenic-fluorescent probes are molecules containing organic heterocycles, and their solubility in aqueous solution is not ideal.
In addition, the combination effect of micro / trace mercury ions and chromogenic-fluorescent probes is still not ideal, so the detection sensitivity and scope of application are subject to many restrictions. For mercury ions, finding more sensitive and efficient detection agents is still an issue the problem before us

Method used

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  • Preparation method of fast-respondability Hg2+developing fluorescence probe based on rhodamine B-thiophene derivative
  • Preparation method of fast-respondability Hg2+developing fluorescence probe based on rhodamine B-thiophene derivative
  • Preparation method of fast-respondability Hg2+developing fluorescence probe based on rhodamine B-thiophene derivative

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Experimental program
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Effect test

Embodiment 1

[0037] Weigh 3g of rhodamine B and 60mL of ethanol into a 250mL three-neck flask, stir well to completely dissolve rhodamine B, add 3.00mL of diethylenetriamine drop by drop, after the dropwise addition, reflux at 80°C for 10 hours, and pass nitrogen gas during the reaction process After the reaction, the reaction bottle was cooled to room temperature, suction filtered, and the ethanol was removed by rotary evaporation, and the obtained light brown solid was extracted 3 times with 100mL dichloromethane, the organic phases were combined, washed 4 times with water, and dried with anhydrous sodium sulfate for 2 hours. Filtrate, collect the filtrate, and rotary evaporate to obtain an orange solid, which is then separated by column chromatography (developing solvent: methanol: dichloromethane = 1:5, v / v) to obtain rhodamine B-diethylenetriamine derivatives. The rate is 93.2%.

[0038] Weigh 2.0g of the above-mentioned rhodamine B-diethylenetriamine derivative and 50mL of absolute e...

Embodiment 2

[0041] Embodiment 2: same as embodiment 1, but the volume ratio of water and ethanol becomes 4:1 in the step (3).

Embodiment 3

[0042] Embodiment 3: same as embodiment 1, but the volume ratio of water and ethanol becomes 6:1 in the step (3).

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Abstract

The invention relates to a preparation method of a fast-respondability Hg2+developing fluorescence probe based on a rhodamine B-thiophene derivative. The preparation method comprises the steps of performing a condensation acylation reaction by using rhodamine B and DETA (diethylenetriamine), so as to obtain the rhodamine B-DETA derivative, then reacting the rhodamine B-DETA derivative with 2-thiophenecarboxaldehyde, so as to obtain the rhodamine B-thiophene derivative, and a water-ethyl alcohol mixing solution based on the rhodamine B-thiophene derivative can be used for the fast-respondability Hg2+developing fluorescence probe. The preparation method provided by the invention can be used for the fast-respondability developing fluorescence probe for rapidly analyzing the content of Hg2+ in a water sample, and the fast-respondability developing fluorescence probe has strong anti-interference to other metal ions (Na+, K+, Mg2+, Fe3+, Cu2+, Cr3+), the applicable pH value range is from acid to neutral, and the fast-respondability developing fluorescence probe is an ideal Hg2+developing fluorescence probe; the respond time of an Hg2+ color indicator to the Hg2+ is less than 2 minutes, the lowest detectable limit is 2.0 times 10<-7> mol / L; the preparation method provided by the invention has the advantages of being simple in synthetic process, low in cost, easy and simple to operate, high in sensitivity, quick in respond speed, low in detectable limit, wide in application prospect and the like.

Description

technical field [0001] The present invention relates to a mercury ion (Hg 2+ ) detection agent, specifically related to a rapid response Hg based on rhodamine B-thiophene derivatives 2+ Chromogenic-fluorescent probe preparation method. Background technique [0002] In the process of global industrialization, the content of heavy metal ions in the environment is increasing day by day due to human activities, and the scope of pollution is also expanding day by day. The problem of heavy metal pollution in my country's water is very prominent, and the pollution rate of the bottom of rivers, lakes and reservoirs is as high as 80.1% [Zhou Huaidong, Peng Wenqi, etc. Water Environment and Water Environment Restoration. Beijing: Chemical Industry Press, 2005]. As early as the investigation in the early 1980s, it was found that many water bodies such as the Jinsha River, Xiangjiang River, Jiyun River, and Jinzhou Bay had heavy metal pollution to varying degrees. The concentration r...

Claims

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Application Information

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IPC IPC(8): G01N21/64
CPCG01N21/6404
Inventor 杨正龙
Owner TONGJI UNIV
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