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Magnetic porous carbon-based QuEChERS purification material and application thereof in sample pretreatment and tobacco pesticide residue detection

A technology for sample pretreatment and purification of materials, which is applied in the field of pesticide residue detection, can solve the problems that limit the further application of QuEChERS technology, the adsorption capacity of matrix interferences is not strong enough, and the specific surface area of ​​purification materials is limited, so as to achieve simplified pretreatment process and high stability The effect of the property and the simple preparation method

Active Publication Date: 2021-11-26
ZHENGZHOU TOBACCO RES INST OF CNTC
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, how to choose the appropriate combination of two or more purification materials still has a certain degree of blindness, and the dosage ratio of different purification materials needs to be optimized, which makes the experimental process very cumbersome.
In addition, the shortcomings of conventional purification materials that need to match the matrix limit the further application of QuEChERS technology in the detection of pesticide residues
The reason is that the main problem is that the adsorption capacity of existing purification materials for matrix interferences is not strong enough: on the one hand, due to the single active site of the purification materials, it can only adsorb and remove matrix interferences of specific properties; on the other hand, it is limited by the purification The specific surface area of ​​the material is limited, and two-dimensional materials such as graphene are easy to agglomerate during actual use, resulting in a sharp decrease in the actual specific surface area

Method used

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  • Magnetic porous carbon-based QuEChERS purification material and application thereof in sample pretreatment and tobacco pesticide residue detection
  • Magnetic porous carbon-based QuEChERS purification material and application thereof in sample pretreatment and tobacco pesticide residue detection
  • Magnetic porous carbon-based QuEChERS purification material and application thereof in sample pretreatment and tobacco pesticide residue detection

Examples

Experimental program
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Effect test

Embodiment 1

[0033] According to the literature "Sono-assisted preparation of highly-efficient peroxidase-like Fe 3 o 4 magnetic nanoparticles for catalytic removal of organic pollutantswith H 2 o 2. Ultrason. Sonochem. 2010, 17: 526-533", the preparation of magnetic Fe by ultrasonic-assisted reverse co-precipitation 3 o 4 nanoparticles, dispersed in 50 mL of methanol to obtain the first solution (containing about 4 mmol Fe 3 o 4 ); 2.62 g of 2-methylimidazole (32 mmol) and 2.32 g of cobalt nitrate hexahydrate (8 mmol) were weighed and dissolved in 50 mL of methanol to obtain the second solution and the third solution, respectively. The second solution was added to the first solution with stirring at room temperature. After reacting for 1 h, the third solution was added to the above reaction solution, and the reaction was continued for 24 h. The resulting precipitate was collected by magnetic recovery, washed several times with water and methanol, and dried in a vacuum oven at 35 °...

Embodiment 2

[0035] Weigh 0.93 g of commercially available magnetic Fe 3 o 4 Nanoparticles (4 mmol), 3.53 g of 2-isopropylimidazole (32 mmol) and 2.38 g of zinc nitrate hexahydrate (8 mmol) were dissolved in 50 mL of methanol to obtain the first, second and third solutions, respectively . The second solution was added to the first solution with stirring at room temperature. After reacting for 1 h, the third solution was added to the above reaction solution, and the reaction was continued for 24 h. The resulting precipitate was collected by magnetic recovery, washed several times with water and methanol, and dried in a vacuum oven at 35 °C to obtain Fe 3 o 4 / MOFs composites. Will Fe 3 o 4 The / MOFs composite was calcined in a tube furnace in a nitrogen atmosphere at 400 °C, and the resulting product was the magnetic porous carbon-based QuEChERS purification material.

Embodiment 3

[0037] According to the literature "Sono-assisted preparation of highly-efficient peroxidase-like Fe 3 o 4 magnetic nanoparticles for catalytic removal of organic pollutantswith H 2 o 2 . Ultrason. Sonochem. 2010, 17: 526-533", the preparation of magnetic Fe by ultrasonic-assisted reverse co-precipitation 3 o 4 nanoparticles, dispersed in 50 mL of methanol to obtain the first solution (containing about 4 mmol Fe 3 o 4 ); 2.62 g of 2-methylimidazole (32 mmol) and 2.38 g of zinc nitrate hexahydrate (8 mmol) were weighed and dissolved in 50 mL of methanol to obtain the second solution and the third solution, respectively. The second solution was added to the first solution with stirring at room temperature. After reacting for 1 h, the third solution was added to the above reaction solution, and the reaction was continued for 24 h. The resulting precipitate was collected by magnetic recovery, washed several times with water and methanol, and dried in a vacuum oven at 35 °C...

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Abstract

The invention relates to a magnetic porous carbon-based QuEChERS purification material and application thereof in sample pretreatment and tobacco pesticide residue detection, a preparation method comprises the following steps: preparing magnetic Fe3O4 nano-particles by adopting an ultrasonic-assisted reverse coprecipitation method, further preparing a Fe3O4 / MOFs composite material based on the magnetic Fe3O4 nano-particles, taking the obtained composite material as a precursor, and preparing the magnetic porous carbon-based QuEChERS purification material prepared by adopting a high-temperature calcination mode. The magnetic porous carbon-based QuEChERS purification material is used for replacing a purification material in a traditional QuEChERS sample pretreatment method, most impurities can be removed by independently using the magnetic porous carbon-based QuEChERS purification material, the purification purpose is achieved, and combined use of multiple purification materials is not needed; the purification material has the magnetic recovery performance, multiple times of centrifugation in pretreatment are avoided, the pretreatment process is simplified, and the analysis efficiency is improved; and when the purification material is applied to tobacco pesticide residue detection, the recovery rate and the precision are relatively good.

Description

technical field [0001] The invention belongs to the technical field of pesticide residue detection, and in particular relates to a magnetic porous carbon-based QuEChERS purification material and its application in sample pretreatment and tobacco pesticide residue detection. Background technique [0002] The use of pesticides can prevent the invasion of tobacco by diseases and insect pests, thereby improving the quality of tobacco production. However, the extensive use of pesticides has resulted in pesticide residues in tobacco. Since the pesticides that need to be analyzed and determined are often trace components in tobacco, and there are many types, different chemical structures and properties, the complex tobacco matrix poses great challenges to its accurate quantitative detection. QuEChERS (Quick-Easy-Cheap-Effective-Rugged-Safety) is a rapid sample pretreatment technology developed based on solid-phase extraction technology and matrix solid-phase dispersion technology....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/062
Inventor 陈满堂刘绍锋潘立宁陈黎刘瑞红樊美娟崔华鹏王晓瑜赵乐刘惠民
Owner ZHENGZHOU TOBACCO RES INST OF CNTC
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