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A method for detecting quizalofop-p-ethyl and its metabolite residues in complex matrix

A technology of quizalofop-p-ethyl and its metabolites, which is applied in the field of detection of quizalofop-p-p-p-p and its metabolites residues in complex matrices, and can solve the problem of the large difference in the polarity of quizalofop-p-p-p-p-p-p and its metabolites, the purification method to remove impurities, and the purification effect to reproduce Poor performance and other problems, to achieve good purification effect, rapid detection, and improve the effect of detection accuracy

Active Publication Date: 2019-10-11
TOBACCO RES INST CHIN AGRI SCI ACAD +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Found through literature retrieval to prior art, although can guarantee the extraction efficiency of quizalofop-p-p-ethyl in simple matrix at present about the assay method of quizalofop-p-ethyl residual amount at present, there are following deficiencies: 1) adopt liquid-liquid distribution or solid The purification method of phase extraction is not only complicated to operate and wastes reagents, but also has poor reproducibility for the purification of complex samples containing a large amount of pigments, oils, and impurities, and impurity peaks can easily interfere with the detection results
2) The polarity of quizalofop-p-ethyl and quizalofop-acid is quite different, and it is difficult to remove impurities through a liquid-liquid partition or solid-phase extraction purification method. Two or more methods need to be used for purification. The operation is complicated and the middle is very easy. loss of residue

Method used

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  • A method for detecting quizalofop-p-ethyl and its metabolite residues in complex matrix
  • A method for detecting quizalofop-p-ethyl and its metabolite residues in complex matrix
  • A method for detecting quizalofop-p-ethyl and its metabolite residues in complex matrix

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] Embodiment 1: the detection of quizalofop-ethyl residues in tobacco leaves

[0062] (1) extraction

[0063] Weigh 2.0g of tobacco leaf sample into a 50mL centrifuge tube with a cover, pipette 10mL of acetonitrile into the centrifuge tube, shake and extract on a vortex mixing oscillator for 1min, add 4g of anhydrous magnesium sulfate, 1g of sodium chloride, and immediately mix in a vortex Oscillate for 2 min with an oscillator, and then centrifuge at 4000 r / min for 5 min.

[0064] (2) purification

[0065] Pipette 1 mL of the extract into a 1.5 mL centrifuge tube, add 10 mg of multi-walled carbon nanotubes and 50 mg of PSA, vortex on a vortex mixer for 2 min, and centrifuge at 6000 r / min for 2 min. Aspirate the supernatant, pass through a 0.22 μm filter membrane, and wait for the test.

[0066] (3) HPLC-MS / MS detection

[0067] HPLC detection conditions are:

[0068] Thermo Scientific TSQ Quantum Ultra;

[0069] Column: SunFire C18 Column, 4.6μm, 2.1mm×100mm;

...

Embodiment 2

[0103] Example 2: Detection of quizalofop-p-ethyl metabolite residues in tea

[0104] (1) extraction

[0105] Weigh 2.0g of tobacco leaf sample into a 50mL centrifuge tube with a cover, pipette 10mL of acetonitrile into the centrifuge tube, shake and extract on a vortex mixing oscillator for 1min, add 4g of anhydrous magnesium sulfate, 1g of sodium chloride, and immediately mix in a vortex Oscillate for 2 min with an oscillator, and then centrifuge at 4000 r / min for 5 min.

[0106] (2) purification

[0107] Pipette 1 mL of the extract into a 1.5 mL centrifuge tube, add 10 mg of multi-walled carbon nanotubes and 10 mg of C18, vortex on a vortex mixer for 2 min, and centrifuge at 6000 r / min for 2 min. Aspirate the supernatant, pass through a 0.22 μm filter membrane, and wait for the test.

[0108] (3) HPLC-MS / MS detection

[0109] HPLC detection conditions are:

[0110] Thermo Scientific TSQ Quantum Ultra;

[0111] Column: SunFire C18 Column, 4.6μm, 2.1mm×100mm;

[0112...

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Abstract

The invention provides a method for detecting quizalofop-p-ethyl and metabolite residues of quizalofop-p-ethyl in a complex matrix. The method is a matrix solid-phase dispersion extraction method and comprises steps as follows: (1), extraction of residues in a sample; (2), purification: an extraction solution obtained in the step (1) is weighed and taken, a purifying agent is added to the extraction solution, and a mixed solution is subjected to matrix solid-phase dispersion extraction; (3), preparation of a standard solution; (4), detection with HPLC-MS / MS (high performance liquid chromatography-tandem mass spectrometry); (5), establishment of a standard curve; (6), result analysis. The detection method can determine quizalofop-p-ethyl and the metabolite residues of quizalofop-p-ethyl rapidly, sensitively and accurately, and a new detection technology is provided for detection of herbicide quizalofop-p-ethyl and the metabolite residues of quizalofop-p-ethyl.

Description

technical field [0001] The invention belongs to the technical field of trace analysis, and in particular relates to a method capable of detecting quizalofop-pyl-ethyl and its metabolite residues in complex matrices. Background technique [0002] Quizalofop-p-ethyl is a phenoxycarboxylate systemic conduction-type stem and leaf treatment herbicide developed by Nissan Chemical Industry Co., Ltd. of Japan. Its mechanism of action is mainly: inhibition of cell fatty acid synthesis, inhibition of acetyl CoA carboxylase, destruction of meristem growth, and death of weeds. Studies have found that quizalofop-p-ethyl has mutagenic effects on the human body, and it has been listed as a phase-out list by the European Union and other countries. However, in my country, quizalofop-p-ethyl is still widely produced and used as an excellent herbicide, and is widely used in agricultural production. In addition, the state has seldom set limits on quizalofop-p-ethyl in various crops, and lacks...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
Inventor 王秀国李义强徐茜林勇翟明泉赵海刚陈丹尤祥伟陈志厚林伟徐辰生刘通
Owner TOBACCO RES INST CHIN AGRI SCI ACAD