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An analytical method applied to the determination of sulfonylurea herbicide residues in plants

A technology of sulfonylureas and analysis methods, which is applied in the field of determination of sulfonylurea herbicide residues in plants, can solve the problems of lack of concentration steps, reduce the detection sensitivity of herbicides, etc., achieve less solvent consumption, less impurities, Simple Effects of Sample Handling

Inactive Publication Date: 2017-08-25
NANJING INST OF ENVIRONMENTAL SCI MINIST OF ECOLOGY & ENVIRONMENT OF THE PEOPLES REPUBLIC OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the disadvantage of the QuEChERS method is the lack of a concentration step, which will reduce the detection sensitivity of this type of herbicide

Method used

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  • An analytical method applied to the determination of sulfonylurea herbicide residues in plants
  • An analytical method applied to the determination of sulfonylurea herbicide residues in plants
  • An analytical method applied to the determination of sulfonylurea herbicide residues in plants

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Experimental program
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Effect test

preparation example Construction

[0022] (2) Preparation of extraction head for QuEChERS method:

[0023] The bottom and top of the extraction head are filled with sieve plates, and the middle part is filled with 400 mg anhydrous magnesium sulfate, 200 mg N-propylethylenediamine (PSA), 200 mg silica gel C 18 , 30 mg graphitized carbon black powder (GCB). Insert the extraction tip into the pipette for use (e.g. figure 1 shown).

[0024] (3) Sample processing:

[0025] Weigh 2.5 g of fresh rice plant samples into a 50 mL plastic centrifuge tube, add 10 mL of formic acid / acetonitrile (2:98, V / V) mixed solution, add 3 g of NaCl, and use a high-speed tissue grinder at 15000 r / min , homogenized for 1 min. Centrifuge at 4000 rpm for 3 min. Use the designed extraction apparatus (as follows figure 1 Shown) that is, the pipette connected with the extraction head slowly absorbs 4 mL of the supernatant, stands still for 30 s, discharges the liquid in the extraction head into a 5 mL centrifuge tube, adds 100 µL of ch...

Embodiment

[0036] Use the scheme of the present invention to detect the sulfonylurea herbicides in rice plants, the results show:

[0037] The concentration and peak area of ​​10 sulfonylurea herbicides showed good linearity in the range of 0.01-500 ng / mL

[0038] relationship, correlation coefficient r 2 >0.997. The average recovery rate was 82.9~108.0% in the spiked concentration range of 5~50 μg / kg, the relative standard deviation RSD<9.8%, and the minimum detection concentration LOQ: 0.082~0.244 μg / kg. The method is simple, rapid and accurate, and can meet the requirements for the detection of sulfonylurea herbicide residues in rice plants.

[0039] 1. Linearity of the method

[0040] Prepare the mixed standard stock solution with rice plant blank extract respectively to prepare mixed standard solutions with 6 concentrations of 0.01, 0.02, 0.05, 50, 100, and 500ng / mL for sample injection, and the concentration ( x ) vs peak area ( y ) as a standard curve, the linear range is be...

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Abstract

The invention discloses an analysis method applied to measuring residual quantity of sulfonylurea herbicide in plants. The method comprises the first step of preparing a stock solution, the second step of preparing extraction head through a QuEChERS method, the third step of processing samples and the fourth step of setting detection conditions of UPLC-MS / MS and conducting sample introduction. The method has the advantages that pretreatment is conducted through an extraction device, the sample purifying process is simple and quick, samples can be obtained through simple absorbing-pushing, results are accurate, and detection is quick; secondly, a sieve in the extraction head allows dispersion extraction, adsorbent, salt and other particulate matter can be removed out of the solution, the number of impurities is reduced, and convenience is brought to accurate quantitation; quantitation is accurate, sensitivity is high, operation is easy and quick, the consumption of the solvent is small, and the requirement for pesticide residue analysis can be met; the improved QuEChERS-method device is used for measuring the residue quantity of 10 kinds of sulfonylurea herbicide in plants.

Description

technical field [0001] The invention relates to an analysis method for determining the residual amount of sulfonylurea herbicides in plants, and belongs to the technical field of determining the residual amount of sulfonylurea herbicides in plants. Background technique [0002] Sulfonylurea herbicides are currently the largest class of herbicides in the world. Over the past 20 years, they have become the most active and effective field for the development of new herbicide varieties. 30% of the new pesticides developed in recent years are herbicides of this type agent. Sulfonylurea herbicides are high-efficiency, low-toxicity, broad-spectrum pesticides, which consist of three parts: aromatic ring, urea bridge and heterocyclic ring. 3.3~5.2. Due to the advantages of low dosage, high activity and low toxicity, this kind of herbicide is widely used in field weeding of rice, rapeseed, wheat, barley and corn and other crops. However, with the development and wide application of...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/06
CPCG01N30/06G01N2030/062
Inventor 宋宁慧郭敏石利利张芹
Owner NANJING INST OF ENVIRONMENTAL SCI MINIST OF ECOLOGY & ENVIRONMENT OF THE PEOPLES REPUBLIC OF CHINA
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