Detection method of residual quantity of indazole flusulfamide and metabolite IT-4 thereof
A technology of indazolamide and IT-4, which is applied in the detection field of indazolamide and its metabolite IT-4 residues, and achieves the effects of improving service life, simple operation and little interference.
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Embodiment 1
[0056] Example 1: Detection of the residual amount of indazole sulfastrobin 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 c...
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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