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A LCMSMS method for the rapid and simultaneous detection of chlorothalonil and its metabolites in fruits and vegetables

A technology of vegetables and fruits and chlorothalonil, which is applied in the field of pesticide residue detection, can solve the problems of low efficiency and heavy workload, and achieve the effect of simple and fast method

Active Publication Date: 2022-01-04
梅里埃检测技术(青岛)有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Chlorothalonil is a non-polar pesticide, which is usually detected by gas chromatography and gas chromatography-mass spectrometry, while 4-hydroxychlorothalonil has a hydroxyl polar group in its molecular structure, and is usually detected by liquid chromatography-electrospray tandem mass spectrometry For detection, the parent and metabolites are detected separately, the workload is large and the efficiency is low; therefore, it is necessary to establish a detection method for simultaneous detection of chlorothalonil parent and metabolites

Method used

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  • A LCMSMS method for the rapid and simultaneous detection of chlorothalonil and its metabolites in fruits and vegetables
  • A LCMSMS method for the rapid and simultaneous detection of chlorothalonil and its metabolites in fruits and vegetables
  • A LCMSMS method for the rapid and simultaneous detection of chlorothalonil and its metabolites in fruits and vegetables

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Embodiment 1

[0050] A kind of LCMSMS method for rapid simultaneous detection of chlorothalonil and its metabolites in vegetables and fruits, the specific steps are as follows:

[0051] Step (1) Weighing of the sample: Weigh 10g of the head cabbage sample, put it in a 50 mL polystyrene centrifuge tube, add acidity regulator and 10 mL of acetonitrile, the acidity regulator is 1.0mL of 10% sulfuric acid;

[0052] Step (2) Sample extraction: Place the centrifuge tube containing the sample in step (1) on a shaker for 1000 times / min to shake vigorously for 1 minute, add 1 g of sodium chloride and 4 g of anhydrous magnesium sulfate in sequence, and immediately Shake to disperse, shake vigorously on an oscillator at 1000 times / min for 1 minute, then centrifuge at 3500 r / min for 5 minutes to obtain a matrix solution, filter it through a nylon filter membrane into a sample injection vial and wait for sample injection analysis;

[0053] Step (3) Preparation of standard curve: the specific steps are a...

Embodiment 2

[0064] Except that taking the sample as cucumber in step (1), other steps are the same as in Example 1.

Embodiment 3

[0066] Except that taking the sample in step (1) is an apple, other steps are the same as in Example 1.

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Abstract

The invention provides a LCMSMS method for rapid and simultaneous detection of chlorothalonil and its metabolites in vegetables and fruits, comprising: step (1) weighing of sample; step (2) extraction of sample; step (3) standard curve preparation; step (4) measurement and result calculation. Through the technical scheme of the present invention, the problem that the chlorothalonil standard product is easily degraded is overcome; the pretreatment method of dispersed solid phase extraction using sulfuric acid acidification-acetonitrile extraction or phosphoric acid acidification-acetonitrile extraction, and atmospheric pressure chemical ionization liquid A phase chromatography-triple quadrupole tandem mass spectrometry detection method can simultaneously detect chlorothalonil and the metabolite 4-hydroxychlorothalonil in fruits and vegetables. The recovery rate and relative standard deviation are in line with the relevant provisions of GB 27404. The recovery rate and precision of the method meet the requirements of trace analysis. analyze.

Description

technical field [0001] The invention relates to the technical field of pesticide residue detection, in particular to a LCMSMS method for rapid and simultaneous detection of chlorothalonil and its metabolites in vegetables and fruits. Background technique [0002] Chlorothalonil (chlorothalonil), chemical name 2,4,5,6-tetrachloro-1,3-dicyanobenzene, is a broad-spectrum high-efficiency protective fungicide developed by Diamond Shamrock Chem.Co. in the United States in 1963. It is the most widely used fungicide in agricultural production at home and abroad. The main metabolite of chlorothalonil is 4-hydroxychlorothalonil (chlorothalonil-4-hydroxy), also known as SDS-3701, chemical name: 4-hydroxy-2,5,6-trichloro-1,3-phthalonitrile , compared with the parent chlorothalonil, the metabolite 4-hydroxychlorothalonil is more toxic. In recent years, the harm of chlorothalonil to the environment and aquatic organisms has attracted increasing attention. [0003] In May 2020, the Euro...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/72
CPCG01N30/02G01N30/06G01N30/72G01N2030/062
Inventor 毕瑞锋张义霞付萌张伟伟邓锁成赵春华
Owner 梅里埃检测技术(青岛)有限公司
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