Method for measuring residual quantity of paraquat and diquat in food

A determination method and technology for paraquat, applied in measuring devices, instruments, scientific instruments, etc., can solve the problems of inability to detect paraquat and diquat residues, and achieve the effect of accurate analysis, guaranteeing healthy development and improving sensitivity

Inactive Publication Date: 2014-05-28
刘靖靖
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  • Abstract
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Problems solved by technology

[0008] Another object of the present invention is to provide a sample pretreatment method to make up for the deficiency that the existing internationally widely recognized QuEChERS method cannot be used for the detection of paraquat and diquat residues

Method used

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  • Method for measuring residual quantity of paraquat and diquat in food
  • Method for measuring residual quantity of paraquat and diquat in food
  • Method for measuring residual quantity of paraquat and diquat in food

Examples

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Embodiment 1

[0041] Example 1: Detection of paraquat and diquat residues in apples

[0042] (1) Sample pretreatment

[0043] Weigh 10.0 g of the homogenized apple sample into a 50 mL stoppered plastic centrifuge tube, add 10 mL of aqueous methanol, vortex for 1 min, and centrifuge at 5000 r / min for 5 min. After centrifugation, take 2 mL of supernatant extract to fill with 100 mg C 18 and 100mg PSA in a centrifuge tube, vortex for 1min, and centrifuge at 5000r / min for 3min. 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).

[0044] (2) Preparation of standard working solution

[0045] Weigh 25±0.1mg of paraquat and diquat standard substances into 25mL plastic volumetric flasks, dissolve them with acetonitrile, and make the standard stock solution concentration 1000.0μg / mL; pipette the standard stock solutions of paraquat and diquat respective...

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Abstract

The invention relates to a method for measuring the residual quantity of paraquat and diquat in food. During pretreatment on a sample, paraquat and diquat in a food sample are extracted by a methanol solution, the extract liquid is purified by C18 and PSA dispersive solid-phase extraction agents, and finally, qualitative and quantitative measurement on the residual paraquat and diquat in the food is achieved through the precise mass number of compound ions with the combination of high performance liquid chromatography-quadrupole rod flight time tandem mass spectrum. The average recycling rate of paraquat is 80.6%-96.8%, the relative standard deviation of paraquat is 3.9%-7.1%, the limit of quantitation of paraquat is 10 microgram / kg, the recycling rate of diquat is 80.8%-97.3%, the relative standard deviation of diquat is 3.5%-7.8%, and the limit of quantitation of diquat is 10 microgram / kg. The method can effectively alleviate matrix interference to residual detection on paraquat and diquat in food, has the advantages of simplicity and convenience in operation, rapidness, accuracy, high sensitivity and good repeatability, and is supplement and 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 paraquat and diquat 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. [0003] The chemical name of paraquat is 1,1,-dimethyl-4,4,-bipyridyl cation, which belongs to organic heterocyclic quaternary ammonium salt herbicides. As a broad-spectrum herbicide, it is widely used. In 2011...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
Inventor 刘靖靖王境堂吴振兴
Owner 刘靖靖
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