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A kind of detection method of indazole sulfasulfame and its metabolite it-4 residue

A technology of indazole sulfame and IT-4, which is applied in the detection field of indazole sulfame and its metabolite IT-4 residues, and achieves the effect of good purification effect, simple operation and little interference

Inactive Publication Date: 2015-12-09
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

At present, there are no relevant reports at home and abroad on the residue analysis of indazole sulfasulfame and its toxic metabolite IT-4, and it is still in a blank stage at home and abroad

Method used

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  • A kind of detection method of indazole sulfasulfame and its metabolite it-4 residue
  • A kind of detection method of indazole sulfasulfame and its metabolite it-4 residue
  • A kind of detection method of indazole sulfasulfame and its metabolite it-4 residue

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] Example 1: Detection of the residual amount of indazole sulfame in cucumber

[0057] (1) extraction

[0058] Weigh 5.0g cucumber sample into a 50mL capped centrifuge tube, pipette 10mL acetonitrile into the centrifuge tube, shake and extract on a vortex mixer for 1min, add 4g anhydrous magnesium sulfate, 1g sodium chloride, 1g sodium citrate and 0.5 g of disodium hydrogen citrate, immediately oscillated in a vortex mixer for 2 min, and then centrifuged at 4000 r / min for 5 min.

[0059] (2) purification

[0060] Pipette 1 mL of the extract into a 1.5 mL centrifuge tube, add 150 mg of anhydrous magnesium sulfate, 50 mg of PSA, and 50 mg of GCB adsorbent, 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.

[0061] (3) UHPLC-MS / MS detection

[0062] UHPLC detection conditions are:

[0063] Thermo Scientific TSQ Quantum Ultra;

[0064] Chromatographic column:...

Embodiment 2

[0097] Example 2: Detection of residues of indazole sulfame metabolite IT-4 in soil

[0098] (1) extraction

[0099] Weigh 10.0g of soil sample into a 50mL capped centrifuge tube, add water to moisten it, pipette 20mL of acetonitrile into the centrifuge tube, shake and extract on a vortex mixing oscillator for 1min, add 8g of anhydrous magnesium sulfate, 2g of sodium chloride, 2g of sodium citrate and 1.0g of disodium hydrogen citrate were immediately shaken in a vortex mixer for 2min, and then centrifuged at 4000r / min for 5min.

[0100] (2) purification

[0101] Pipette 1 mL of the extract into a 1.5 mL centrifuge tube, add 150 mg of anhydrous magnesium sulfate and 50 mg of PSA adsorbent, 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.

[0102] (3) UHPLC-MS / MS detection

[0103] UHPLC detection conditions are:

[0104] Thermo Scientific TSQ Quantum Ultra; ...

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Abstract

The invention provides a detection method of residual quantity of indazole flusulfamide and metabolite IT-4 thereof. The method comprises the following steps: (1) preparing standard solutions, namely weighing a standard substance, dissolving and making up to volume through an organic solvent to prepare a standard stock solution, and gradually diluting the standard stock solution to prepare the standard working solutions with serial concentration; (2) extracting a residue from a sample; (3) purifying, namely weighing an extracting solution in the step (2), placing the weighed solution in a centrifuge tube, and then adding an adsorbent, and centrifuging to obtain supernatant; (4) detecting by ultra high performance liquid chromatography-tandem mass spectrometry (UHPLC-MSMS); (5) establishing a standard curve; and (6) analyzing a result. The detection method provided by the invention is capable of fast, flexibly and accurately determining the residual quantity of indazole flusulfamide and metabolite IT-4 thereof, and a new detection technology is provided for detecting the novel bactericide, indazole flusulfamide, and metabolite thereof.

Description

technical field [0001] The invention belongs to the technical field of trace analysis, and in particular relates to a method for detecting residues of indazole sulfastrobin and its metabolite IT-4. Background technique [0002] Indazole sulfasulfame is a triazole sulfonamide fungicide created by Nissan Chemical Company, Japan, with a novel and unique structure, which was first reported in 2003. The agent is mainly effective against oomycetes and proteobacteria. It has strong persistent effect, is resistant to rain, and has stable effects on various diseases. It is a promising fungicide. As a new type of drug, there is still a large blindness in the use of indazole sulfame in agricultural production. Due to the lack of relevant researches on indazole sulfasulfame at home and abroad, it is necessary to carry out in-depth and extensive research on the detection method and residue behavior of indazole sulfastrolide, in order to provide technical support for standardizing drug ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/88G01N30/06
Inventor 王秀国李义强徐茜陈志厚林勇翟明泉赵海刚王凤龙孔凡玉宋超周杨全
Owner TOBACCO RES INST CHIN AGRI SCI ACAD
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