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LCMSMS method for rapidly and simultaneously detecting chlorothalonil and metabolites thereof in vegetables and fruits

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: 2021-07-13
梅里埃检测技术(青岛)有限公司
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  • Summary
  • 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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  • LCMSMS method for rapidly and simultaneously detecting chlorothalonil and metabolites thereof in vegetables and fruits
  • LCMSMS method for rapidly and simultaneously detecting chlorothalonil and metabolites thereof in vegetables and fruits
  • LCMSMS method for rapidly and simultaneously detecting chlorothalonil and metabolites thereof in vegetables and fruits

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Embodiment 1

[0050] A 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 10 g of cabbage sample, put it in a 50 mL polystyrene centrifuge tube, add an acidity regulator and 10 mL of acetonitrile, and the acidity regulator is 1.0 mL of 10% sulfuric acid;

[0052] Step (2) Extraction of the sample: Place the centrifuge tube containing the sample in step (1) on a vibrator for 1,000 times / min and vigorously shake for 1 minute, add 1 g of sodium chloride and 4 g of anhydrous magnesium sulfate in sequence, and immediately Shake to disperse, vibrate vigorously for 1 minute at 1000 times / min on a shaker, and centrifuge at 3500 r / min for 5 minutes to obtain a matrix solution, which is filtered through a nylon filter into an injection vial for analysis;

[0053] Step (3) Preparation of standard curve: the specific steps are as follows;

[0054] Step (31) Sta...

Embodiment 2

[0064] Other steps are the same as in Example 1, except that the sample is weighed as cucumber in step (1).

Embodiment 3

[0066] Other steps are the same as in Example 1, except that the sample is weighed as apple in step (1).

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Abstract

The invention provides an LCMSMS method for rapidly and simultaneously detecting chlorothalonil and metabolites thereof in vegetables and fruits. The LCMSMS method comprises the following steps: (1) weighing a sample; (2) extracting the sample; (3) preparing a standard curve; and (4) conducting determination and result calculation. According to the technical scheme, the problem that a chlorothalonil standard substance is liable to degrade is solved; a dispersive solid-phase extraction pretreatment method adopting sulfuric acid acidification-acetonitrile extraction or phosphoric acid acidification-acetonitrile extraction and an atmospheric pressure chemical ionization liquid chromatography-triple quadrupole tandem mass spectrometry detection method are established, and chlorothalonil and a metabolite 4-hydroxychlorothalonil in vegetables and fruits can be detected at the same time. The recovery rate and the relative standard deviation both meet relevant provisions of GB 27404, the recovery rate and the precision of the method both meet the requirements of trace analysis, and the method is simple and rapid and is suitable for rapid and simultaneous analysis of chlorothalonil and 4-hydroxychlorothalonil in vegetables and fruits.

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 sterilization developed by American Diamond Shamrock Chem.Co. in 1963 It is the most widely used fungicide in agricultural production at home and abroad. The main metabolite of chlorothalonil is 4-hydroxychlorothalonil-4-hydroxy, also known as SDS-3701, chemical name: 4-hydroxy-2,5,6-trichloro-1,3-phthalonitrile , the metabolite 4-hydroxychlorothalonil was more toxic than the parent chlorothalonil. In recent years, the harm of chlorothalonil to the environment and aquatic organisms has attracted increasing attention. [0003] In May 2020, the EU officially banned chlorothalonil. ...

Claims

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Application Information

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Patent Type & Authority Applications(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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