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Thioester in rhodamine B as well as preparation method and application thereof

A thioester and preparation process technology, applied in the field of mercury ion optical probes, can solve problems such as poor selectivity and influence, and achieve the effects of fast reaction speed, good solubility, and huge application prospects

Inactive Publication Date: 2009-06-17
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the mercury ion detection reagents in my country mainly choose dithizone as the complexing agent for mercury ions, but its selectivity is relatively poor and it is easily affected by many other metal ions

Method used

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  • Thioester in rhodamine B as well as preparation method and application thereof
  • Thioester in rhodamine B as well as preparation method and application thereof
  • Thioester in rhodamine B as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Embodiment 1: the preparation of rhodamine B lactone

[0018] The synthetic route of rhodamine B internal thioester is as follows:

[0019]

[0020] The specific synthesis process is as follows:

[0021] Step a): Dissolve 239mg of rhodamine B in about 5ml of 1,2-dichloroethane, slowly add about 0.3ml of phosphorus oxychloride, and react at reflux at 83°C for 4h. After cooling, the reaction system was vacuum-dried to obtain rhodamine B acid chloride.

[0022] Step b): Dissolve the obtained rhodamine B acid chloride in 6ml of tetrahydrofuran, then add the solution dropwise to 6ml of tetrahydrofuran solution containing 152mg of thiourea and 1.2ml of triethylamine, and stir overnight. The reaction system was evaporated to dryness under reduced pressure to obtain a purple-red oily liquid, and 5 ml of water was added thereto to produce a purple-red precipitate, which was washed with a large amount of water. The obtained crude product was separated by column chromatograp...

Embodiment 2

[0023] Embodiment 2, the spectroscopic properties of rhodamine B lactone and its reaction product with mercury ions

[0024] Weigh 4.6 mg of rhodamine B lactone to prepare 10 ml of 1,4-dioxane solution as mother solution (1 mM).

[0025] Add 50 μl of the above mother solution dropwise to a certain amount of 0.02M phosphate buffer solution, then add different equivalents of mercury ion solutions, and then use 0.02M phosphate buffer solution to make the volume to 10ml. After reacting at room temperature for 5 minutes, measure its UV-visible absorption spectrum and fluorescence emission spectrum. When the fluorescence emission spectrum is measured, it is de-excited at 530nm; the slit width for excitation and emission is 10nm; the voltage is 400V.

[0026] figure 1 It is the ultraviolet-visible absorption spectrum and fluorescence emission spectrum of 5 μM rhodamine B endothioate in the range of 0-100 μM final concentration of mercury ions.

[0027] figure 2 It is the working...

Embodiment 3

[0029] Example 3: Research on the interference of other metal ions on the determination of mercury by rhodamine B lactone.

[0030] Various metal ions (Ag + , Ca 2+ , Cd 2+ ,Co 2+ , Cu 2+ , Fe 3+ , K + , Mg 2+ , Mn 2+ , Pb 2+ , Zn 2+ or Hg 2+ ) to a final concentration of 50 μM. After reacting at room temperature for 5 minutes, measure its UV-visible absorption spectrum and fluorescence emission spectrum. When the fluorescence emission spectrum is measured, it is de-excited at 530nm; the slit width for excitation and emission is 10nm; the voltage is 400V.

[0031] Various metal ions (Ag + , Ca 2+ , Cd 2+ ,Co 2+ , Cu 2+ , Fe 3+ , K + , Mg 2+ , Mn 2+ , Pb 2+ , Zn 2+ ) solution, add 50 μl of rhodamine B lactone mother solution, and then add mercury ions to make the final concentration 50 μM.

[0032] image 3 Rhodamine B lactone (5μM) and various metal ions (Ag + , Ca 2+ , Cd 2+ ,Co 2+ , Cu 2+ , Fe 3+ , K + , Mg 2+ , Mn 2+ , Pb 2+ , Zn 2+ or Hg...

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Abstract

The invention discloses rhodamine B intra-thioester, a preparation method and application thereof. The rhodamine B thioester has a structural formula as formula I. The method prepares intra-thioester compounds of a first rhodamine dye, an intra-thioester ring of the compounds can be selectively cut off by mercury ions, and the method improves the selectivity and sensitivity of the reaction compared with the prior reagent. Through introducing an active intra-thioester ring group on the rhodamine B, the method realizes optical response to the mercury ions, can realize quantitative detection for trace mercury ions with high sensitivity and high selectivity, and has huge application prospect in the fields such as quality, environment and biology.

Description

technical field [0001] The invention relates to a novel mercury ion optical probe-rhodamine B lacthione, its preparation method and the application of the compound in mercury ion content analysis. Background technique [0002] Mercury is a common heavy metal pollutant that poses serious hazards to the natural environment and human health. Various human activities (such as mining, chemical industry, electronics and other industries) release a large amount of mercury to nature every year. This mercury is converted by organisms in nature to neurotoxic methylmercury and its concentration accumulates along the food chain. Long-term intake of water or food containing excessive mercury by the human body will cause chronic mercury poisoning. Due to the strong toxicity of mercury, the poisoning dose is small. Therefore, the mercury content in drinking water and farmland irrigation in my country must not exceed 0.001 mg / L. The mercury content in fishery water should not exceed 0.005...

Claims

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Application Information

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IPC IPC(8): C07D495/10G01N33/52
Inventor 马会民史文
Owner INST OF CHEM CHINESE ACAD OF SCI
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