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A kind of method for detecting the residual amount of dioxatrazone in wheat planting

A method for biscarbazone and residues, which is applied in the field of detecting biscarbazone residues in the process of wheat planting, can solve problems such as blank detection methods for biscarbazone residues, and achieves high sensitivity, simple operation and separation effect. Good results

Active Publication Date: 2021-03-12
INST OF PLANT PROTECTION SHANDONG ACAD OF AGRI SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] For this reason, the technical problem to be solved by the present invention is to provide a method for detecting the residual amount of bisfentrazone in the wheat planting process, so as to solve the problem of the blank detection method of the residual amount of bisfentrazone in the prior art

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  • A kind of method for detecting the residual amount of dioxatrazone in wheat planting
  • A kind of method for detecting the residual amount of dioxatrazone in wheat planting
  • A kind of method for detecting the residual amount of dioxatrazone in wheat planting

Examples

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Embodiment 1

[0050] The detection of bisfentrazone residual amount in the wheat flour of embodiment 1

[0051] In this embodiment, the residual amount of bisfentrazone contained in wheat flour is detected, which specifically includes the following steps:

[0052] (1) Sample pretreatment: Weigh 2 g of well-mixed wheat flour to be tested, put it in a 50 mL centrifuge tube, add 10 mL of acetonitrile (containing 1% v / v formic acid) to mix, mechanically shake for 30 min, and add 3 g of chlorine Mix with sodium chloride, shake vigorously for 5 minutes, then let stand for 15 minutes, centrifuge at 4000r / min for 5 minutes, and collect the upper acetonitrile phase;

[0053] (2) Quantitatively absorb 2mL of the upper acetonitrile phase, transfer it to a 15mL centrifuge tube that has been added with 0.2gPSA and 0.05gGCB in advance, vortex and mix for 1min, and centrifuge at 5000r / min for 5min, then take the supernatant and pass through 0.22μm Filter the membrane to obtain the sample solution, which ...

Embodiment 2

[0089] The detection of bisfentrazone residual amount in the wheat plant of embodiment 2

[0090] In this embodiment, the detection of bisfentrazone residue contained in wheat plants specifically includes the following steps:

[0091] (1) Sample pretreatment: Take the plant sample to be tested, cut it into small pieces of about 1cm, and mix thoroughly; then weigh 2g of the treated wheat plant and place it in a 50mL centrifuge tube, add 15mL distilled water to soak for 20min, then add 10mL Acetonitrile (containing 1% v / v formic acid), shake mechanically for 30 minutes, add 6 g of sodium chloride, shake vigorously for 5 minutes, let stand for 15 minutes, centrifuge at 4000 r / min for 5 minutes, and collect the upper acetonitrile phase;

[0092] (2) Quantitatively absorb 2mL of the upper acetonitrile phase, transfer it to a 15mL centrifuge tube that has been added with 0.2gPSA and 0.05gGCB in advance, vortex and mix for 1min, and centrifuge at 5000r / min for 5min, then take the sup...

Embodiment 3

[0110] It can be seen that the method of the present invention can effectively detect the residual amount of bisfentrazone in wheat plants. The detection of bisfentrazone residue in the soil of embodiment 3

[0111] In this example, the detection of bisfentrazone residue contained in the wheat planting soil specifically includes the following steps:

[0112] (1) Sample pretreatment: Take the soil sample to be tested, crush it, sieve it, mix it well, and accurately weigh 2.0 g of the processed soil sample into a 50 mL centrifuge tube, add 10 mL of acetonitrile (containing 1% v / v formic acid), shake mechanically for 30 min, add 3.0 g of sodium chloride, shake vigorously for 2 min, centrifuge at 4000 r / min for 5 min, and collect the upper acetonitrile phase;

[0113] (2) Quantitatively absorb 2mL of the upper acetonitrile phase, transfer it to a 15mL centrifuge tube that has been added with 0.2gPSA and 0.05gGCB in advance, vortex and mix for 1min, and centrifuge at 5000r / min fo...

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Abstract

The invention belongs to the technical field of pesticide residue detection, and in particular relates to a method for detecting the residual amount of bisfentrazone in the wheat planting process. The method for detecting the residual amount of bisfentrazone in wheat planting described in the present invention uses dispersive solid phase extraction technology to establish a simple and fast sample pretreatment method, and in combination with HPLC-MS / MS technology, it can be used for wheat flour and wheat plants and wheat planting soil for effective detection of bisfentrazone residues, the average recoveries of bisfentrazone were 88.9‑92.2%, 86.2%‑90.1% and 89.2‑91.2%, respectively, and the average relative standard deviation (RSD) They are 1.6-2.2%, 1.1%-2.1% and 0.9-1.8%, respectively, and the detection limit is 0.005mg / kg. The test results show that the method is easy to operate, fast, and the separation effect is good. The accuracy and precision can reach The requirements of quantitative analysis have the advantages of high sensitivity, good repeatability, easy operation, rapidity and accuracy.

Description

technical field [0001] The invention belongs to the technical field of pesticide residue detection, and in particular relates to a method for detecting the residual amount of bisfentrazone in the wheat planting process. Background technique [0002] Bisfentrazone, the chemical name is 1,3-dimethyl-4-(2-(methylsulfonyl)-4-trifluoromethylphenyl)-1H-pyrazol-5-yl 1,3-di Methyl-1H-pyrazole-4-carboxylate is a HPPD (p-hydroxyphenylpyruvate dioxygenase) inhibitor herbicide developed by Qingdao Qingyuan Agricultural Crown Co., Ltd. [0003] [0004] HPPD widely exists in various organisms. In plants, HPPD can catalyze the conversion of p-hydroxypyruvate into homogentisic acid, and then into plastoaldehyde and tocopherol, which are important substances required for electron transfer in photosynthesis. When HPPD is inhibited, it will cause tyrosine accumulation and plastoquinone deficiency in plant meristems, and the plants will appear yellowing symptoms within 3-5 days, followed b...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
Inventor 李瑞娟于建垒宋国春刘同金李如美张雪莲赵亚
Owner INST OF PLANT PROTECTION SHANDONG ACAD OF AGRI SCI
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