Method for measuring residual quantity of thidiazuron and diuron as well as metabolites thereof in cotton
A determination method, the technology of thiadizuron, is applied in the direction of measuring devices, instruments, scientific instruments, etc., to achieve the effect of reducing the amount of use, reducing the interference of impurities, and high recovery rate
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Embodiment 1
[0049] (1) Extraction: Weigh 20.0 g of cotton, place it in a stoppered Erlenmeyer flask, add 50 mL of acetonitrile, 10 mL of distilled water, shake and extract on a shaker for 60 min, add 6.0 g of sodium chloride to the filtrate, shake for 2 min, and let the layers stand still. Collect the upper organic phase, dehydrate it with anhydrous sodium sulfate, concentrate under reduced pressure in a water bath at 40°C to dryness, blow dry with nitrogen, add 10 mL of ethyl acetate, and wait for purification;
[0050] (2) Purification: use a C18 column, pre-spray with 5mL ethyl acetate, load the sample, rinse with 10mL ethyl acetate, collect the eluent, concentrate under reduced pressure in a 40°C water bath, blow dry with nitrogen, and constant volume with 2mL methanol , membrane filtration.
[0051] (3) Determination: Determination by DAD detector, mobile phase: methanol / water, 50 / 50 (V / V) flow rate: 0.5mL / min chromatographic column: XDB-C18, 1.8μm, 4.6×50mm, sample injection: 5 μL,...
Embodiment 2
[0053] (1) Extraction: Weigh 20.0 g of cotton and place it in a stoppered Erlenmeyer flask; add 80 mL of acetonitrile and 20 mL of distilled water, shake and extract on a shaker for 100 min, add 10 g of sodium chloride to the filtrate, shake for 5 min, statically separate layers, and collect The upper organic phase was dehydrated by anhydrous sodium sulfate, concentrated under reduced pressure in a water bath at 40°C to near-dryness, blown dry with nitrogen, and added 20 mL of ethyl acetate to be purified;
[0054] (2) Purification: use a C18 column, pre-spray with 5mL ethyl acetate, load the sample, rinse with 10mL ethyl acetate, collect the eluent, concentrate under reduced pressure in a 40°C water bath, blow dry with nitrogen, and constant volume with 2mL methanol , membrane filtration.
[0055] (3) Determination: Determination by DAD detector, mobile phase: methanol / water, 50 / 50 (V / V) flow rate: 0.5mL / min chromatographic column: XDB-C18, 1.8μm, 4.6×50mm, sample injection: ...
Embodiment 3
[0057] (1) Extraction: Weigh 20.0g of cotton, place it in a stoppered Erlenmeyer flask, add 50mL of acetonitrile, 10mL of distilled water, shake and extract on a shaker for 60min, add 8g of sodium chloride to the filtrate, shake for 4min, statically separate layers, collect The upper organic phase was dehydrated by anhydrous sodium sulfate, concentrated under reduced pressure in a water bath at 40°C to near-dryness, blown dry with nitrogen, and added 10 mL of ethyl acetate to be purified;
[0058] (2) Purification: use a C18 column, pre-spray with 5mL ethyl acetate, load the sample, rinse with 10mL ethyl acetate, collect the eluent, concentrate under reduced pressure in a 40°C water bath, blow dry with nitrogen, and constant volume with 2mL methanol , membrane filtration.
[0059] (3) Determination: Determination by DAD detector, mobile phase: methanol / water, 50 / 50 (V / V) flow rate: 0.5mL / min chromatographic column: XDB-C18, 1.8μm, 4.6×50mm, sample injection: 5 μL, column temp...
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