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Method for detecting concentration of hydrazine

A technology for concentration and detection of samples, applied in chemical instruments and methods, fluorescence/phosphorescence, luminescent materials, etc., to achieve good stability and simple synthesis

Inactive Publication Date: 2016-03-16
晋江尚京富本环保科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although fluorescent probes for the detection of hydrazine have been reported, most of them are based on the change of fluorescence intensity at a single wavelength to achieve qualitative and quantitative analysis. Such detection methods are easily affected by the distribution of probes and the detection environment. And the influence of factors such as the stability of the instrument

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  • Method for detecting concentration of hydrazine
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  • Method for detecting concentration of hydrazine

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Experimental program
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Embodiment 1

[0023]

[0024] (Scheme 1) 4-hydroxy-1,8-naphthalimide (269mg, 1.0mmol), 4-bromobutyric acid (166mg, 1.0mmol), 4-dimethylaminopyridine (122mg, 1.0mmol) and di Cyclohexylcarbodiimide (412mg, 2.0mmol) was dissolved in 20mL of dry dichloromethane, reacted at room temperature for 6h, evaporated under reduced pressure to obtain a crude product, and then separated by column chromatography using dichloromethane to obtain 179mg of a light yellow pure product , and the yield was 43%.

[0025] (Scheme 2) 4-hydroxy-1,8-naphthalimide (269mg, 1.0mmol), 4-bromobutyric acid (332mg, 2.0mmol), 4-dimethylaminopyridine (244mg, 2.0mmol) and di Cyclohexylcarbodiimide (618 mg, 3.0 mmol) was dissolved in 20 mL of dry dichloromethane, reacted at room temperature for 6 hours, evaporated under reduced pressure to obtain a crude product, and then separated by column chromatography using dichloromethane to obtain 283 mg of a light yellow pure product , and the yield was 68%.

[0026] (Scheme 3) 4-hy...

Embodiment 2

[0030] The inventor of the present invention has carried out following test: (a) the impact of different concentrations of hydrazine (0~100 μ M) on the probe (5 μ M) fluorescence spectrum; Insert figure is the ratio of fluorescence intensity at 547nm place and fluorescence intensity at 452nm place and added hydrazine The linear relationship between concentrations. The above determinations were made in a system containing ethanol and water (3:7, V / V) containing 5mM phosphate buffered saline (PBS), pH 7.4, and all spectral tests were measured at 25°C after adding hydrazine for 15 minutes of. See results figure 1 .

[0031] From figure 1 It can be seen that with the increase of the concentration of hydrazine in the probe solution, the fluorescence emission peak at 452nm gradually decreases, and at the same time, a new emission peak at 547nm occurs and gradually increases. The ratio of the intensity to the fluorescence intensity at 452nm has a good linear relationship. Theref...

Embodiment 3

[0033] Effect of different analytes (50 μM) on the fluorescence spectra of probes (5 μM). Analytes include: ethylenediamine EDA, dimethylamine DMA, triethylamine TEA, n-butylamine nBA, ammonium acetate AA, sulfide ion S 2- , Chloride ion Cl - , bromide ion Br - , iodide ion I - , Sulfate ion SO 4 2- , Thiocyanate ion SCN -, glutathione GSH and hydrazine, and their concentrations are all 50 μM. All test conditions were completed in ethanol and water (3:7, V / V) containing 5mM phosphate buffered saline (PBS), pH 7.4 system, and all spectra were added at 25°C for 15 minutes test the result. Pipette 25μL of the probe stock solution (1mM) into a 5mL colorimetric tube, then add 1.5mL ethanol, 250μL of 100mMPBS, then pipette 25μL of the above analyte stock solution (10mM) into the colorimetric tube, and then set it with ultrapure water. Make up to 5mL. Shake well, let it stand for 15min, then measure. The result is as figure 2 shown.

[0034] From figure 2 It can be see...

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Abstract

The invention relates to a method for detecting the concentration of hydrazine, and particularly relates to preparation and application of 4-bromobutyric acid ester naphthalimide compounds serving as a hydrazine ratio fluorescent probe. The probe can be used for identifying hydrazine with high selectivity and performing sensitively quantitative and qualitative analysis on hydrazine by a fluorescence method, and can quickly give response to hydrazine so as to realize instant detection on hydrazine. The probe has stable property and can be stored and used for a long time. Furthermore, the probe can be used for performing accurately quantitative analysis on hydrazine by using a ratio fluorescence method, and has a relatively strong interference resistance. The probe has a relatively mild synthesizing condition, only needs one-step reaction, and has simple synthesis.

Description

technical field [0001] The invention relates to a detection method of hydrazine concentration. Specifically, the method of the present invention relates to the application of 4-bromobutyrate naphthalimide compounds as hydrazine ratiometric fluorescent probes and their high selectivity for hydrazine recognition. Background technique [0002] Hydrazine (NH 2 NH 2 ), as an important industrial chemical, is widely used in many fields, such as medicine, emulsifier, dyestuff and textile, catalyst, corrosion inhibitor and pesticide involved in military, aerospace, industry and agriculture. Hydrazine is flammable and explosive, and is best known as a high-energy fuel in rocket propulsion systems. Hydrazine has a strong reducing ability and is also used in the corrosion protection of metals. In the field of extraction, hydrazine is also used as a plant growth regulator. In the pharmaceutical field, hydrazine is used as an antibacterial drug. However, hydrazine is also toxic. Wi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/06G01N21/64C07D221/14
CPCC09B57/08G01N31/22
Inventor 叶龙武张艳
Owner 晋江尚京富本环保科技有限公司
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