Method for determining quantity of diquat or paraquat residual in food

A determination method and technology of diquat, which are applied in measurement devices, instruments, scientific instruments, etc., to achieve the effects of good repeatability, high sensitivity and easy operation

Inactive Publication Date: 2019-01-11
蒋悦
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Another object of the present invention is to provide a sample pretreatment method to make up for the deficiency th

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0034] Example 1: Detection of Diquat or Paraquat Residues in Apples

[0035] (1) Sample pretreatment

[0036] Weigh 10.0 g of the homogenized apple sample into a 50 mL plastic centrifuge tube with a stopper, add 10 mL of 20% methanol aqueous solution, vortex for 1 min, and centrifuge at 5000 r / min for 5 min. After centrifugation, take 2 mL of the supernatant extract into a centrifuge tube containing 100 mg C18 and 100 mg PSA, vortex for 1 min, and centrifuge at 5000 r / min for 3 min. After the supernatant was passed through a 0.22 μm filter membrane, the obtained sample liquid was determined by liquid chromatography-quadrupole time-of-flight tandem mass spectrometry (LC-Q TOF).

[0037] (2) Preparation of standard working solution

[0038] Weigh 25±0.1mg of the standard product into a 25mL plastic volumetric flask, dissolve it with acetonitrile, and dilute to obtain a 1000.0μg / mL standard stock solution; pipette 1.0mL of the standard stock solution into a 100mL plastic volum...

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Abstract

The invention relates to a method for determining the quantity of diquat or paraquat residual in food. The method comprises the steps of pretreating a sample: firstly extracting the diquat or the paraquat in the food sample by using a methanol aqueous solution; purifying the extract by using C18 and PSA (Primary Secondary Amine) dispersive solid-phase extraction agents; and finally by combining ahigh performance liquid chromatography with a quadrupole time-of-flight mass spectrometry, realizing qualitative and quantitative determination of the diquat or the paraquat residual in the food through the accurate mass number of compound ions. The method disclosed by the invention has the beneficial effects that the matrix interference in the detection of the diquat or the paraquat residual in the food is effectively reduced; the recovery rate of the diquat or the paraquat can be up to 80.8%-97.3%; the relative standard deviation is 3.5%-7.8%; the limit of quantification is 10mug/kg; the method has the advantages of being simple and convenient to operate, fast, accurate, high in sensitivity and good in repeatability; and the method is a supplement and an improvement on a conventional QuEChERS method.

Description

technical field [0001] The invention belongs to the technical field of determination of pesticide residues, in particular to a method for determination of diquat or paraquat residues in food. Background technique [0002] During the planting of fruits, vegetables, grains and other crops, farmland weeds have an important impact on crop yield and quality. The use of herbicides in agricultural production not only saves a lot of heavy weeding manual labor and mechanical weeding operations, but more importantly, reduces the loss of agricultural product yield and quality caused by weeds, and obtains considerable economic benefits. However, with people's attention to food safety issues, the hazards of herbicide residues to human health have also attracted much attention. For example, diquat or paraquat (diquat), which is a moderately toxic herbicide, is a non-selective herbicide of organic heterocycles. Widely used in potatoes, cotton, soybeans, corn, sorghum, flax, sunflower and...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/062
Inventor 蒋悦刘滢佳郑幸子
Owner 蒋悦
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