ZrO2 nanoparticle modified three-dimensional graphene material and application thereof in organophosphorus pesticide detection

An organophosphorus pesticide and nanoparticle technology, applied in the field of analytical chemistry, can solve the problems of poor sensitivity and accuracy, and achieve the effects of low detection limit, enhanced stability and wide linear range.

Active Publication Date: 2021-04-20
QINGDAO AGRI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the complexity of the food matrix, the diversity of ingredients, and the traces of organophosphorus pesticide residues, it is difficult to detect directly by instruments, and the sensitivity and accuracy of detection are poor

Method used

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  • ZrO2 nanoparticle modified three-dimensional graphene material and application thereof in organophosphorus pesticide detection
  • ZrO2 nanoparticle modified three-dimensional graphene material and application thereof in organophosphorus pesticide detection
  • ZrO2 nanoparticle modified three-dimensional graphene material and application thereof in organophosphorus pesticide detection

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] ZrO 2 The preparation method of the three-dimensional graphene material modified by nanoparticles is as follows: figure 1 As shown, the specific steps are as follows:

[0052] (a) Put a 1.2cm diameter metal mesh sheet (200 mesh, 0.05mm thick wire, 74 micron holes) in 10% dilute hydrochloric acid for 12 hours of corrosion, and dry;

[0053] (b) placing the rough metal mesh sheet after corrosion in APTES for 12h to realize the amination of the metal mesh;

[0054] (c) 0.02g polydiallyldimethylammonium chloride is added in 100mL graphene oxide suspension (w / w, 0.1%), then the metallic mesh of step (b) amination is placed in it, Add 0.001g of N,N-hydroxysuccinimide and 0.001g of 1-(3-dimethylpropyl)-3-ethylcarbodiimide as a catalyst, and react at 70°C for 2 hours;

[0055] (d) Repeat (b) and (c) three times successively for the metal mesh obtained in step (c), to obtain a graphene oxide-modified metal mesh;

[0056] (e) the graphene oxide modified metal net that step (d...

Embodiment 2

[0061] ZrO 2 The preparation method of the three-dimensional graphene solid-phase extraction column modified by nanoparticles:

[0062] The empty solid-phase extraction column used in this example has an inner diameter of 1.2 cm and a volume of 3 mL, and the extraction material is ZrO 2 Nanoparticle-modified three-dimensional graphene; firstly, the lower sieve plate (with a pore size of 10 μm) is loaded into the solid-phase extraction empty column, and then the prepared 2-10 pieces of ZrO 2 The three-dimensional graphene material modified by nanoparticles is filled into the empty column of solid phase extraction, and then the upper sieve plate (with a pore size of 10 μm) is loaded into it and compacted to obtain ZrO 2 Nanoparticle-modified three-dimensional graphene solid-phase extraction column.

Embodiment 3

[0064] Using ZrO 2 Nanoparticle-modified three-dimensional graphene solid-phase extraction column for the detection of organophosphorus pesticides:

[0065] Solid Phase Extraction:

[0066] 1. at first with 4mL acetonitrile and 4mL water to the ZrO prepared by embodiment 2 2 Nanoparticle-modified three-dimensional graphene solid-phase extraction column for elution and activation;

[0067] ② Use a peristaltic pump to drive 20mL of the organophosphorus pesticide working solution to pass through the ZrO 2 The flow rate of the nanoparticle-modified three-dimensional graphene solid-phase extraction column is 1mL / min to ensure that the organophosphorus pesticide molecules are adsorbed on the surface of the prepared extraction material;

[0068] ③ Then drive 1mL of acetonitrile through ZrO 2 The three-dimensional graphene solid-phase extraction column modified by nanoparticles, the flow rate is 0.8mL / min, and the eluate is obtained for use.

[0069] High-performance liquid chrom...

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Abstract

The invention discloses a ZrO2 nanoparticle modified three-dimensional graphene material and application thereof in organophosphorus pesticide detection, and belongs to the technical field of analytical chemistry. The ZrO2 nanoparticle modified three-dimensional graphene material disclosed by the invention is a three-dimensional graphene material constructed by taking a metal net as a matrix, bonding poly(diallyldimethylammonium chloride) reinforced graphene oxide aerogel and depositing ZrO2 nanoparticles on the surface of the graphene aerogel; a solid-phase extraction column prepared by taking the material as a filling material can realize high-efficiency extraction of the organophosphorus pesticide, and then the organophosphorus pesticide is analyzed and detected by using high performance liquid chromatography. The method for detecting the organophosphorus pesticide by adopting the solid-phase extraction column is wide in linear range, low in detection limit and high in sensitivity, can be used for enriching and detecting the organophosphorus pesticide in vegetables, and not only has relatively strong matrix anti-interference capability, but also has good enriching and purifying performance and a wide application prospect.

Description

technical field [0001] The invention belongs to the technical field of analytical chemistry, in particular to a ZrO 2 Nanoparticle-modified three-dimensional graphene materials and their application in the detection of organophosphorus pesticides. Background technique [0002] Organophosphorus pesticides are a class of highly effective insecticides and herbicides. They are currently one of the most widely used types of pesticides and play an important role in increasing crop yields. However, excessive residues will cause pollution of water, air, soil, vegetables, fruits and processed food, which will have a certain impact on the ecological environment and human health. Food poisoning incidents caused by organophosphorus pesticide residues occur from time to time. According to statistics, food poisoning caused by organophosphorus pesticides ranks first in my country. Therefore, it is very important to strengthen the detection of organophosphorus pesticide residues in food. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06G01N30/02
CPCB01J20/286B01J20/3204B01J20/324B01J20/3236B01J20/3289B01J20/3092B01J20/28007
Inventor 侯秀丹丁荣杨庆利吴薇赵海燕
Owner QINGDAO AGRI UNIV
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