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Preparation method of oxime-containing compound and method for detecting organophosphorus ester compounds with oxime-containing compound

An organophosphate and compound technology, which is applied in the fields of environmental science, test chemistry and analytical chemistry, can solve the problems of insensitive detection of organophosphate compounds, poor stability of AChE, and complex hydrolase steps, and achieves fast and stable detection. The effect of good performance, sensitivity and high selectivity detection

Inactive Publication Date: 2019-05-10
MATERIAL INST OF CHINA ACADEMY OF ENG PHYSICS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the direct electrochemical method is simple and easy to operate, but it is only suitable for a very small number of organophosphate compounds with self-redox reactions; the acetylcholinesterase inhibition method is widely used in the detection of nerve agents and organophosphorus pesticides, but AChE is stable. Poor performance, difficult to preserve, and insensitive to the detection of low-toxicity organophosphate compounds; organophosphate hydrolase method is also suitable for broad-spectrum organophosphate compounds, but the steps of synthesizing such hydrolase are complex

Method used

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  • Preparation method of oxime-containing compound and method for detecting organophosphorus ester compounds with oxime-containing compound
  • Preparation method of oxime-containing compound and method for detecting organophosphorus ester compounds with oxime-containing compound
  • Preparation method of oxime-containing compound and method for detecting organophosphorus ester compounds with oxime-containing compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] 344 mg of 2-hydroxy-1-naphthaldehyde was weighed into a reaction flask, 6 mL of ethanol was added, followed by 167 mg of hydroxylamine hydrochloride. The mixture was heated to reflux at 65 °C overnight. After cooling to room temperature, the solid was collected using a rotary evaporator and purified on a short silica gel column, eluting with ethyl acetate and petroleum ether. Finally, 324 mg of a light pink solid was obtained, which was an oxime-containing compound prepared in this example.

Embodiment 2

[0031] 212 mg of benzaldehyde was weighed into the reaction flask, 6 mL of ethanol was added, followed by 167 mg of hydroxylamine hydrochloride. The mixture was heated to reflux at 65 °C overnight. After cooling to room temperature, the concentrated mixture was collected using a rotary evaporator and purified on a short silica gel column, eluting with ethyl acetate and petroleum ether. Finally, 183 mg of liquid oily product was obtained, which was an oxime-containing compound prepared in this example.

Embodiment 3

[0033] Weigh 340 mg of acetylnaphthalene into the reaction flask, add 6 mL of ethanol, and then add 318 mg of anhydrous sodium carbonate and 208 mg of hydroxylamine hydrochloride. The mixture was heated to reflux at 65 °C overnight. After cooling to room temperature, the sodium carbonate was removed, and the concentrated mixture was collected using a rotary evaporator and purified on a short silica gel column, eluting with ethyl acetate and petroleum ether. Finally, 264 mg of white needle-like solid was obtained, which was an oxime-containing compound prepared in this example.

[0034] The above three examples respectively provide a method for preparing oxime-containing compounds. Since the selected raw materials are different, there are also differences in the structural formula of the final product. The above three are only examples provided. figure 1 Also provided are 5 structural formulas of oxime-containing compounds that can be obtained, and its preparation is the same ...

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Abstract

The invention discloses a preparation method of an oxime-containing compound and a method for detecting organophosphorus ester compounds with the oxime-containing compound. The preparation method of the oxime-containing compound comprises dissolving a reaction substrate into a reaction solution, then adding in hydroxylamine hydrochloride, and heating the mixture for reaction; cooling the reacted mixture to room temperature, collecting reaction products and purifying the reaction products on a silica gel column, eluting the reaction products with organic solvent to obtain the product of the oxime-containing compound. The method for detecting the organophosphorus ester compounds with the oxime-containing compound comprises (1) adding an organophosphorus ester compound to be detected into a solution with the oxime-containing compound as the probe, and after reaction is completed, performing fluorescence detection; (2) adding in the oxime-containing compound into a two-dimensional carbideor nitride, then loading the two-dimensional carbide or nitride on a glassy carbon electrode and immersing the glassy carbon electrode into the solution to be detected, and after reaction is completed, performing electrochemical detection. The method for detecting the organophosphorus ester compound with the oxime-containing compound has the advantages of high detecting speed and sensitivity, highselectivity and stability, low false positive and the like and accordingly has a broad application prospect.

Description

technical field [0001] The invention relates to the fields of environmental science, test chemistry and analytical chemistry, in particular to a preparation method of an oxime-containing compound and a method for using the compound to detect organic phosphate compounds. Background technique [0002] Nerge Agents are the most toxic chemical agents today, which can poison or kill enemy humans, animals and plants on a large scale. They are mainly divided into two categories: fluorophosphate ester and cyanophosphate compound. Organic phosphate compounds. In addition, organophosphorus pesticides (Organophosphorus Pesticides, OPs) used to control plant diseases, insects, and pests also belong to organophosphate compounds. This type of compound binds to acetylcholine esterase (AChE) through electrophilic phosphorus, inhibits the activity of AChE, and makes AChE lose the ability to decompose acetylcholine (ACh), ACh accumulates in the effect site, resulting in excessive excitation ...

Claims

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Application Information

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IPC IPC(8): C07C249/08C07C251/48C07C251/42G01N21/64
Inventor 朱婧赵鹏翔向世帅黄德顺杨晓娇岳国宗
Owner MATERIAL INST OF CHINA ACADEMY OF ENG PHYSICS
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