Method for purifying and detecting fipronil and metabolite thereof in eggs

A technology of fipronil and detection method, which is applied in the field of purification and detection of fipronil and its metabolites in eggs, can solve the problems of low detection accuracy, high quantitative limit, and insufficient detection sensitivity, and achieve reliable results High performance, accurate qualitative and quantitative, and simple analysis

Active Publication Date: 2020-08-25
CHENGDU INST OF BIOLOGY CHINESE ACAD OF S
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] The object of the present invention is to provide a method for purifying and detecting fipronil and its metabolites in eggs, to solve the problem of fipronil and its metabolites in eggs existing in the prior art. Purification and detection method, its quantification limit is high, the detection sensitivity is not enough, and the technical problems of detection accuracy are not high

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  • Method for purifying and detecting fipronil and metabolite thereof in eggs
  • Method for purifying and detecting fipronil and metabolite thereof in eggs
  • Method for purifying and detecting fipronil and metabolite thereof in eggs

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Embodiment 1

[0040] A method for purifying and detecting fipronil and its metabolites in eggs, comprising the following steps:

[0041] (1) Preparation of magnetic nanomaterials

[0042] A1, take 0.72g sodium citrate, 4.8g sodium acetate and 3.0g FeCl 3 ·6H 2 O, dissolved in 300mL ethylene glycol and added to the autoclave, reacted at 200°C for 12h; 3 o 4 Nanoparticles were magnetically separated under the action of an external magnetic field (separation of solution and magnetic nanoparticles by an external magnet), washed twice with distilled water, washed once with absolute ethanol, and freeze-dried at -50°C for 12h to obtain Fe 3 o 4 Nanoparticles;

[0043] A2, take by weighing the Fe of 0.3g prepared in step A1 3 o 4 Add the nanoparticles into the reaction vessel, add 150mL of hydrochloric acid (0.1M) and sonicate for 15min; then wash 4 times with distilled water; add 240mL of methanol, 60mL of water and 3.0mL of ammonia solution into the reaction vessel, then add 1.5mL of TEOS...

Embodiment 2

[0076] A method for purifying and detecting fipronil and its metabolites in eggs, comprising the following steps:

[0077] (1) Preparation of magnetic nanomaterials

[0078] A1, take 0.72g sodium citrate, 4.8g sodium acetate and 3.0g FeCl 3 ·6H 2 O, dissolved in 150mL ethylene glycol and added to the autoclave, reacted at 190°C for 13h; 3 o 4 Nanoparticles were magnetically separated under the action of an external magnetic field, washed twice with distilled water and once with absolute ethanol, and freeze-dried at -50°C for 12 hours to obtain Fe 3 o 4 Nanoparticles;

[0079] A2, take by weighing the Fe of 0.3g prepared in step A1 3 o 4 Add the nanoparticles into the reaction vessel, add 150mL of hydrochloric acid (0.1M) and sonicate for 15min; then wash with distilled water 4 times; add 240mL of methanol, 60mL of water and 3.0mL of ammonia solution into the reaction vessel, then add 0.6mL of TEOS was reacted at room temperature for 24 hours; magnetically separated und...

Embodiment 3

[0099] A method for purifying and detecting fipronil and its metabolites in eggs, comprising the following steps:

[0100] (1) Preparation of magnetic nanomaterials

[0101] A1, take 0.72g sodium citrate, 4.8g sodium acetate and 3.0g FeCl 3 ·6H 2 O, dissolved in 600mL ethylene glycol and added to the autoclave, reacted at 200°C for 12h; 3 o 4 Nanoparticles were magnetically separated under the action of an external magnetic field, washed twice with distilled water and once with absolute ethanol, and freeze-dried at -50°C for 12 hours to obtain Fe 3 o 4 Nanoparticles;

[0102] A2, take by weighing the Fe of 0.3g prepared in step A1 3 o 4 Add nanoparticles into the reaction vessel, add 150mL hydrochloric acid (0.1M) and sonicate for 15min; then wash 4 times with distilled water; add 240mL methanol, 60mL water and 3.0mL ammonia solution to the reaction vessel, then add 3mL of TEOS was reacted at room temperature for 24 hours; magnetically separated under the action of an ...

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Abstract

The invention provides a method for purifying and detecting fipronil and metabolite thereof in eggs, and solves the technical problems of relatively high quantification limit, insufficient detection sensitivity and low detection accuracy of a method for purifying and detecting fipronil and metabolite thereof in eggs in the prior art. The method comprises the following steps: (1) preparing a magnetic nano material; (2) carrying out sample pretreatment; and (3) carrying out detection and analysis by adopting an ultra-high performance liquid chromatography-Q-Exactive high-resolution mass spectrum. According to the method disclosed by the invention, the detection limit and the quantification limit can reach 0.002 to 0.005 [mu] g / kg and 0.006 to 0.015 [mu] g / kg; the method has the advantages ofsimplicity, convenience and quickness in analysis, higher sensitivity and accuracy, better reproducibility, accuracy in quantification, higher recovery rate and capability of accurately analyzing thecontent of fipronil and metabolite thereof in the eggs.

Description

technical field [0001] The invention relates to the technical field of detection of fipronil and its metabolites, in particular to a method for purifying and detecting fipronil and its metabolites in eggs. Background technique [0002] Fipronil is a new type of phenylpyrazole insecticide widely used in agricultural pest control. Phenylpyrazole is a neurotoxic substance that can bind to the ionotropic γ-aminobutyric acid receptor (GABAR) of insects and interfere with the pathway of chloride ions. It has certain excitatory effects at sublethal doses, and at high doses will result in death. In addition, fipronil can form three main metabolites through oxidation, reduction, hydrolysis and photolysis: fipronil sulfone, fipronil sulfoxide and fluoroformil. According to animal experiments, long-term intake of food contaminated with fipronil can damage the liver, kidney and thyroid functions of animals. In July 2017, Belgian authorities found that fipronil was detected in eggs pr...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/08G01N30/14G01N30/72B82Y15/00B82Y40/00
CPCG01N30/02G01N30/06G01N30/08G01N30/14G01N30/72B82Y15/00B82Y40/00G01N2030/062G01N2030/146
Inventor 廖循赵艳白小琳
Owner CHENGDU INST OF BIOLOGY CHINESE ACAD OF S
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