Magnetic graphene with core-shell structure, application thereof to pesticide residue detection and application method

A pesticide residue detection and magnetic graphene technology, applied in chemical instruments and methods, measuring devices, inorganic chemistry, etc., can solve problems such as difficult separation, sample contamination, and non-reusable use, achieve excellent magnetic properties, and realize recycling and reuse , Fast and efficient solid-liquid separation effect

Active Publication Date: 2019-02-15
WEIFANG VOCATIONAL COLLEGE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the very large specific surface area of ​​graphene and excellent water solubility, it is difficult to use traditional centrifugation, filtration and elution methods for solid-liquid separation when separating the same sample solution, which is inefficient, cumbersome and easy to operate. Cause sample contamination and reduce detection sensitivity
In addition, because it is difficult to separate and cannot be reused, it is expensive

Method used

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  • Magnetic graphene with core-shell structure, application thereof to pesticide residue detection and application method

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Experimental program
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Effect test

Embodiment 1

[0039] (1) Graphite oxide was synthesized by the Hummers method, graphite oxide was placed in a crucible, and heat treated in a muffle furnace at 1050°C for 30s to obtain graphene.

[0040] (2) the obtained graphene is dissolved in ethylene glycol; the concentration of the ethylene glycol is 5mg / mL, adding (NH 4 )2 FeSO 4 ·6H 2 O, NH 4 Fe(SO 4 ) 2 12H 2 O, under the protection of nitrogen, room temperature ultrasound 10min after uniform dispersion, add ammonia water drop by drop to the solution, 50 ℃ stirring reaction for 60min, graphene and Fe 3 o 4 Co-precipitate, apply an external magnetic field to aggregate and separate, and wash alternately with deionized water and absolute ethanol twice to obtain G-Fe 3 o 4 . Fe 3 o 4 The particle size is 5-10nm; the G-Fe 3 o 4 Middle Fe 3 o 4 The content is 75wt%.

[0041] (3) Ultrasonic disperse silicon dioxide in Tris-HCl buffer solution, adjust the pH value to 8, add dopamine and stir at room temperature for 24 hours,...

Embodiment 2

[0045] (1) Graphite oxide was synthesized by the Hummers method, graphite oxide was placed in a crucible, and placed in a muffle furnace for heat treatment at 1000° C. for 50 seconds to obtain graphene.

[0046] (2) the obtained graphene is dissolved in ethylene glycol; the concentration of the ethylene glycol is 6mg / mL, adding (NH 4 ) 2 FeSO 4 ·6H 2 O, NH 4 Fe(SO 4 ) 2 12H 2 O, under the protection of nitrogen, room temperature ultrasound 10min after uniform dispersion, ammonia water was added dropwise to the solution, stirred and reacted at 51°C for 55min, graphene and Fe 3 o 4 Co-precipitate, apply an external magnetic field to aggregate and separate, and wash alternately with deionized water and absolute ethanol twice to obtain G-Fe 3 o 4 . Fe 3 o 4 The particle size is 8 ~ 12nm; the G-Fe 3 o 4 Middle Fe 3 o 4 The content is 80wt%.

[0047] (3) Ultrasonically disperse silicon dioxide in Tris-HCl buffer solution, adjust the pH value to 8.5, add dopamine and...

Embodiment 3

[0051] (1) Graphite oxide was synthesized by the Hummers method, graphite oxide was placed in a crucible, and placed in a muffle furnace for heat treatment at 1050°C for 30s to obtain graphene;

[0052] (2) the obtained graphene is dissolved in ethylene glycol; the concentration of the ethylene glycol is 3.5mg / mL, adding (NH 4 ) 2 FeSO 4 ·6H 2 O, NH 4 Fe(SO 4 ) 2 12H 2 O, under the protection of nitrogen, room temperature ultrasound 10min after uniform dispersion, ammonia water was added dropwise to the solution, stirred and reacted at 52°C for 50min, graphene and Fe 3 o 4 Co-precipitate, apply an external magnetic field to aggregate and separate, and wash alternately with deionized water and absolute ethanol twice to obtain G-Fe 3 o 4 . Fe 3 o 4 The particle size is 10-12nm; the G-Fe 3 o 4 Middle Fe 3 o 4 The content is 85wt%.

[0053] (3) Ultrasonically disperse silicon dioxide in Tris-HCl buffer solution, adjust the pH value to 8.2, add dopamine and stir at...

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Abstract

The invention discloses magnetic graphene with a core-shell structure, application thereof to pesticide residue detection and an application method. The magnetic graphene, with the core-shell structure, is formed by coating magnetic graphene to the surface of silicon dioxide through the adhesive action of dopamine, wherein the silicon dioxide serves as a core, and the magnetic graphene serves as ashell; the magnetic graphene adopts graphene loaded with Fe3O4. The magnetic graphene is applied to pesticide residue detection, serves as a magnetic solid phase extraction adsorbent, and performs pretreatment on a target sample before purification; the special structure of the graphene is beneficial to enrichment of aromatic or hydrophobic analyte; the magnetic graphene has excellent magnetic property, can rapidly and efficiently realize solid-liquid separation under the action of external magnetic field, and can further realize recycling and reusing.

Description

technical field [0001] The invention relates to the technical field of pesticide detection, in particular to a magnetic graphene. Background technique [0002] Pesticides are a class of drugs widely used in agricultural production, including insecticides such as carbamates, organochlorines, organophosphates, and pyrethroids, as well as agents that regulate plant growth and herbicide. The extensive and long-term use of pesticides has caused pollution of agricultural products, soil, and water. It is harmful to human reproductive system, nervous system, and endocrine system, and is toxic to beneficial insects such as fish and bees. Therefore, international organizations and countries around the world have issued laws and regulations to limit the residues of pyrethroid pesticides in food and the environment. For example, China stipulates that the content of deltamethrin in food should not exceed 0.5mg / kg (raw grain, leaf Vegetables), 0.2mg / kg (fruit vegetables), 0.1mg / kg (fruit...

Claims

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Application Information

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IPC IPC(8): C01B32/194G01N30/06
CPCC01B32/194G01N30/06
Inventor 刘苏亭韩文婧赵东风高庆平刘振龙桑秀杰
Owner WEIFANG VOCATIONAL COLLEGE
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