Preparation and application of novel fluorescent probe and test paper for hydrazine hydrate detection

A fluorescent probe, hydrazine hydrate technology, applied in the field of analytical chemistry, can solve the problems of inability to adapt to the market demand for rapid detection, requiring tens of minutes or even hours, and low detection accuracy, achieving fast response, low cost, Sensitive effect

Inactive Publication Date: 2020-12-22
HUNAN TARGETING DETECTION TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, these reported fluorescent probes have some limitations, including: 1. There are few types of probes, mainly turn-on type, which is greatly affected by the detection environment and the detection accuracy is low; 2. The response speed is slow, Most probes need tens of minutes or even several hours to complete the response after adding hydrazine hydrate, which cannot meet the market demand for rapid detection

Method used

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  • Preparation and application of novel fluorescent probe and test paper for hydrazine hydrate detection
  • Preparation and application of novel fluorescent probe and test paper for hydrazine hydrate detection
  • Preparation and application of novel fluorescent probe and test paper for hydrazine hydrate detection

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Synthesis and structural characterization of compound 2 (ethyl 7-hydroxy-2-oxo-2H-chromene-3-carboxylate)

[0043] Dissolve 2,4-dihydroxybenzaldehyde (2.76 g, 20 mmol) in 10 mL of absolute ethanol at room temperature, add diethyl malonate (6.40 g, 40 mmol) and piperidine 20 mmol, heat up to 90 oC under reflux, TLC monitoring reaction until complete. After the reaction was taken down and allowed to cool, absolute ethanol was removed by rotary evaporation, and the remaining liquid was dropped into water drop by drop, and a large number of yellow solids were seen to precipitate. After suction filtration and washing of the filter cake, 3.76 g of a yellow solid product was obtained after drying, with a yield of 80.5%. 1 H NMR (400MHz, DMSO-d 6 ): δ (ppm) = 11.08 (s, 1H), 8.87 (s, 1H), 7.75 (d, J = 8.8 Hz, 1H),6.84 (dd, J 1 = 8.8 Hz, J 2 = 2.4 Hz, 1H), 6.72 (d, J = 2.4 Hz, 1H), 4.26 (q, J = 7.2 Hz, 2H), 1.30 (t, J = 7.2 Hz, 3H).

[0044] Synthesis and struct...

Embodiment 2

[0051] Preparation of fluorescent probe master solution

[0052] Accurately weigh 4.10 mg of the product obtained from the above separation with a purity of more than 99% and carefully transfer it to a 50 mL volumetric flask, add CH at room temperature 3 CN, shake well to dissolve it completely, and finally dilute to the mark to obtain 1 mM probe mother solution. During the test, 20 μL of the above solution was measured with a micro-injector each time, dissolved in the test system, and the total volume of each test was guaranteed to be 2 mL. At this time, the concentration of the fluorescent probe in the test system was 10 μL. μM.

Embodiment 3

[0054] Preparation of hydrazine hydrate mother liquor

[0055] Hydrazine hydrate was prepared into 5 mL stock solutions with different concentration gradients (0.1 mM, 0.2 mM, 0.4 mM, 0.7 mM, 1 mM, 1.5 mM, 2.0 mM, 2.5 mM, 3.0 mM, 3.5 mM, 4.0 mM) with PBS buffer solution. The small molecules and inorganic salts required for the remaining tests were respectively prepared into mother solutions with a concentration of 3 mM in PBS buffer solution.

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Abstract

The invention relates to preparation and application of a novel fluorescent probe and test paper for hydrazine hydrate detection, and belongs to the technical field of analytical chemistry. The fluorescent probe takes a benzothiazole mother nucleus as a parent and acetyl as a recognition site, and the chemical structure of the fluorescent probe is shown as a formula (I). When the fluorescent probereacts with hydrazine hydrate, acetyl is hydrolyzed into hydroxyl, a fluorescent substance with high fluorescence emission capacity is generated in a PBS-CH3CN (10 mM, 3: 7, v / v, pH=7.4) buffer solution, fluorescence is changed from blue to green, and ratio type detection of hydrazine hydrate is realized. Besides, the fluorescent probe only responds to hydrazine hydrate, does not respond to smallmolecules such as methylamine, ethylamine, ethylenediamine, butylamine, dodecylamine, n-hexylamine, octadecylamine, aniline, Cys and GSH, and can realize specific recognition of hydrazine hydrate. Inaddition, the fluorescent probe provided by the invention can also be used for rapid detection of hydrazine hydrate in the environment, and has a very good application prospect. Formula I is shown.

Description

technical field [0001] The invention belongs to the technical field of analytical chemistry, and relates to the preparation and application of a novel fluorescent probe and test paper that can be used for the detection of hydrazine hydrate, and is particularly designed for the application of the fluorescent molecular probe in the detection of hydrazine hydrate in systems such as the environment. Background technique [0002] Hydrazine hydrate (N 2 h 4 •H 2 O), also known as hydrazine hydrate, is a colorless, transparent, alkaline oily liquid that absorbs moisture easily. Hydrazine hydrate has strong reducibility and is widely used in the field of pesticide, medicine and fine chemical industry. In addition, it can also be used as a chemical foaming agent and slow-release agent in heating systems, and as a high-energy fuel and explosive raw material in rocket propulsion systems. At the same time, hydrazine hydrate is highly toxic, and its harm to the environment and human ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D417/04C09K11/06G01N21/64
CPCC07D417/04C09K11/06G01N21/643C09K2211/1088C09K2211/1037G01N2021/6439
Inventor 不公告发明人
Owner HUNAN TARGETING DETECTION TECH CO LTD
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