Thioureas ultraviolet probe and preparation and application thereof

A technology of thioureas and probes, which is applied in the fields of thioureas ultraviolet probes and their preparation and application, can solve problems such as difficult application of metal ions in real-time on-line monitoring, and achieve low cost, good selectivity and high yield Effect

Inactive Publication Date: 2017-06-23
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These regulatory agency-approved assays have a major limitation: they are difficult to apply to real-time on-line monitoring of metal ions

Method used

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  • Thioureas ultraviolet probe and preparation and application thereof
  • Thioureas ultraviolet probe and preparation and application thereof
  • Thioureas ultraviolet probe and preparation and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Synthesis of UV probe PHT: 1.2 mL (19.8 mmol) of 80% hydrazine hydrate was added to 20 mL of acetonitrile, stirred at room temperature and 0.85 mL (19.8 mmol) of phenyl isothiocyanate was slowly added dropwise. Under a nitrogen atmosphere, heat to reflux at 82° C. for 5 h, and cool to room temperature after the reaction is completed; a solid precipitate is obtained by suction filtration and washed with acetonitrile. The crude product was purified by recrystallization with acetone, and dried in a vacuum oven at 25°C to obtain the product with a yield of 47%.

[0041] FTIR (KBr): v=3221cm -1 ,3116cm -1 (NH2):1192cm -1 (C=S):1541cm -1 (-NH-):2061cm -1 (-N=C=S); HNMR (400MHz, DMSO, 298K, δ / ppm): 3.33 (S, 2H), 7.16-7.55 (m, ArH) 9.64-9.87 (d, -NH)

Embodiment 2

[0043] The concrete method that thiourea ultraviolet probe detects lead ion:

[0044] Configuration 1×10 -5 The lead ion test liquid of M, the method for the lead ion detection wherein of the thiourea ultraviolet probe synthesized in the application embodiment 1, concrete steps are:

[0045] Step 1: Dissolve the thiourea UV probe synthesized in Example 1 in the solvent DMF, and use the solvent DMF to set the volume in a 100mL volumetric flask to obtain a concentration of 1.0×10 -3 Probe stock solution of M;

[0046] Step 2: Dissolve lead nitrate in solvent deionized water, use solvent deionized water to set the volume in a 100mL volumetric flask, and obtain a concentration of 1.0×10 -2 M lead ion stock solution; the pipetting concentration is 1.0×10 -2 The lead ion stock solution of M is placed in a 100mL volumetric flask, and the solvent deionized water is used to constant volume to obtain a concentration of 1.0×10 -3 M lead ion stock solution; the pipetting concentration...

Embodiment 3

[0050] Selectivity of PHT UV-Vis absorption spectrum to metal ions:

[0051] DMF / H at volume ratio 9:1 2 In the O system, the determination of the ultraviolet probe (PHT) in the addition of metal ions Pb 2+ , Fe 3+ 、Cd 2 + , Zn 2+ , Mg 2+ 、Cr 3+ , Ca 2+ 、Ba 2+ , Sn 2+ 、Na + , Mn 2+ , Hg 2+ UV-Vis absorption spectra before and after.

[0052] Step 1: Dissolve the reactive dye fluorescent probe synthesized in Example 1 in the solvent DMF, and use the solvent DMF to constant volume in a 100mL volumetric flask to obtain a concentration of 1.0×10 -3 Probe stock solution of M;

[0053] Step 2: Dissolve lead salts, iron salts, cadmium salts, zinc salts, magnesium salts, chromium salts, calcium salts, barium salts, sodium salts, manganese salts, and mercury salts in deionized water as a solvent, and use deionized water as a solvent in 100mL Constant volume in the volumetric flask to obtain a concentration of 1.0×10 -2 Each metal ion stock solution of M;

[0054] Step ...

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PUM

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Abstract

The invention relates to a thioureas ultraviolet probe and preparation and application thereof. A structural formula of the probe is as follows. The probe is obtained by reaction between phenyl isothiocyanate and hydrazine hydrate. The thioureas ultraviolet probe is used for detecting lead ions: preparing a probe solution, adding the probe solution into a lead ion solution to be detected, making the volume constant by utilizing a solvent, standing, detecting absorbance under the wavelength of 382nm by means of an ultraviolet-visible spectrometry, and determining the content of the lead ions in the lead ion solution to be detected according to a relationship between relative ultraviolet strength and lead ion concentration. The thioureas ultraviolet probe in the invention is solid powder which is convenient to use and store, and is obtained by direct reaction between the phenyl isothiocyanate and the hydrazine hydrate. A synthesis method is simple, the yield is high, the cost is low, and the application prospect is good.

Description

technical field [0001] The invention belongs to the field of probes and their preparation and application, in particular to a thiourea ultraviolet probe and its preparation and application. Background technique [0002] Among the heavy metals, lead has the highest content, so it is also the most serious hazard to human health. Lead enters the environment through gasoline, paint, etc. Lead has a strong toxic effect on the environment and human health. For example, lead can inhibit heme synthase, hinder heme synthesis, and reduce hemoglobin levels; in addition, lead poisoning can also increase the fragility of red blood cell membranes. And it is easy to hemolysis, which shortens its life span and causes anemia. Lead poisoning can also cause damage to various systems such as the nervous system, digestive system, cardiovascular system, and kidney system, seriously endangering human health. The harm of lead to children is more serious and can lead to mental retardation in childr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C337/06G01N21/33
CPCC07C337/06G01N21/33
Inventor 光善仪任霞赵爽赵岗徐洪耀
Owner DONGHUA UNIV
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