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Method for simultaneously measuring residue contents of five weedicides with different structures in soil

A herbicide and residue technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of large consumption of organic solvents, long analysis time, high detection limit, etc., to achieve optimized detection conditions, simple processing procedures, and reduced use volume effect

Inactive Publication Date: 2014-12-31
GANZHOU TOBACCO SCI RES INST
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Problems solved by technology

The present invention adopts dispersed solid phase extraction (DSPE) in combination with dispersed liquid liquid microextraction (DLLME) as the pretreatment technology of soil sample, and utilizes high performance liquid chromatography (High performance liquid chromatography, HPLC) to measure, has overcome existing method It can quickly and accurately detect five kinds of metsulfuron-methyl, bensulfuron-methyl, promethazone, atrazine and quinclorac Residues of herbicides with different structures, accurate determination results, less interference

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  • Method for simultaneously measuring residue contents of five weedicides with different structures in soil
  • Method for simultaneously measuring residue contents of five weedicides with different structures in soil
  • Method for simultaneously measuring residue contents of five weedicides with different structures in soil

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Embodiment 1

[0047] The present invention simultaneously measures three types of herbicides with five different structures in soil: metsulfuron-methyl (sulfonylureas), bensulfuron-methyl (sulfonylureas), promethazin (triazines), atrazine (triazines) Azines) and the method for quinclorac (quinoline carboxylic acids) residual amount may further comprise the steps:

[0048] (1), weighing samples: accurately weigh 10.0 g of air-dried soil samples passed through a 250 μm sieve, and place them in a 50 mL plastic centrifuge tube;

[0049] (2) Acetonitrile extraction: add 20.0 mL of acetonitrile mixed solution containing 5% acetic acid, vortex for 2 min, add 1.0 g of sodium chloride and 4.0 g of anhydrous magnesium sulfate, immediately shake for 30 s, and centrifuge at 4000 r / min for 5 min;

[0050] (3) Solid-phase extraction: 5.0 mL of the supernatant was transferred to a centrifuge tube containing 0.0750 g of C18 and 1.0 g of anhydrous magnesium sulfate, vortexed for 30 s, centrifuged at 4000 r / ...

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Abstract

The invention discloses a method for simultaneously measuring the residue contents of five weedicides with different structures in soil, and belongs to the technical field of physicochemical detection of pesticide residues in the soil. Specifically, the residue contents of three types of five weedicides with different structures in the soil are directly measured by a high-performance liquid chromatographic (HPLC) instrument by combining dispersive solid-phase extraction (DSPE) with dispersive liquid-liquid microextraction (DLLME). According to the method, the defects and the condition limitations in the prior art are overcome, a method for pre-treating a soil sample and the detection conditions of the instrument are optimized, a DSPE-DLLME-HPLC method is built for simultaneously detecting three types of five weedicides (metsulfuron methyl, bensulfuron methyl, prometryn, atrazine and quinclorac) with different structures in the soil, the linear correlation coefficients are all more than 0.99, the detection limit is 1.5-3.1 ngg<-1>, the average recovery rate is 74.9-90.1%, the relative standard deviation (RSD) is 4.0-5.7%, both the accuracy and the precision meet the residue detection requirements, and the method has the characteristics of low organic solvent consumption, good purification and concentration effects, high sensitivity, simplicity for performing and the like.

Description

technical field [0001] The invention relates to the technical field of physical and chemical detection of pesticide residues in soil, in particular to a method for simultaneously measuring the residues of five herbicides with different structures in soil. Background technique [0002] Quinoline carboxylic acids, sulfonylureas and triazines, as commonly used herbicides, have been widely used in agricultural production, but they also cause pollution of soil, water, air and agricultural products. In addition, quinoline carboxylic acids, sulfonylureas and triazines have relatively stable chemical properties, are difficult to degrade in the environment, have a long residual effect period, and cause phytotoxicity to sensitive crops that will seriously affect their yield and quality. The detection of quinoline carboxylic acid, sulfonylurea and triazine herbicide residues in complex matrices such as soil and agricultural products is very important, not only can effectively avoid the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
Inventor 钟秋瓒申昌优唐明刘小平彭耀东陈荣华肖先仪张超群刘毅杨庆根
Owner GANZHOU TOBACCO SCI RES INST
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