Method for treating pyrethroid pesticide residue soil environment sample before measurement
A technology for pyrethroid and pesticide residues, which is applied in the field of processing soil environmental samples before the determination of pyrethroid pesticide residues, and can solve the problem of increasing difficulty in extraction, separation, purification and enrichment of pyrethroid pesticides, as well as the composition of Complex, organic solvent consumption and other problems, to achieve the effect of saving organic solvent, good effect and low measurement cost
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Embodiment 1
[0017] 1. Soil sample crushing: Freeze-dry the collected soil environmental samples, grind and crush them with a planetary ball mill, and pass through a 100-mesh stainless steel sieve.
[0018] 2. Extraction: Accurately weigh 5 grams of soil sample into a 150 ml corked Erlenmeyer flask, add 25 ml of petroleum ether / acetone (volume ratio 2:1) as the extractant, shake well and soak for 2 hours, then ultrasonicate at 100 Hz Extract for 20 minutes, after standing for stratification, transfer the supernatant to a 125 ml separatory funnel, repeat the above extraction process once, transfer the supernatant to a separatory funnel, add 30 ml of 2% sodium sulfate aqueous solution , shake for 3 minutes and then stand for 10 minutes to separate the organic and aqueous phases.
[0019] 3. Concentration: the upper organic phase was dried with 10 g of anhydrous sodium sulfate, and concentrated to 1 ml by rotary evaporation at 40°C.
[0020] 4. Purification: use glass chromatography silica g...
Embodiment 2
[0023] 1. Soil sample crushing: Freeze-dry the collected soil environmental samples, grind and crush them with a planetary ball mill, and pass through a 100-mesh stainless steel sieve.
[0024] 2. Extraction: Accurately weigh 8 grams of soil samples into a 150 ml corked Erlenmeyer flask, add 25 ml of petroleum ether / acetone (volume ratio 2:1) as the extractant, shake well and soak for 2 hours, then ultrasonicate at 100 Hz Extract for 20 minutes, after standing for stratification, transfer the supernatant to a 125 ml separatory funnel, repeat the above extraction process once, transfer the supernatant to a separatory funnel, add 30 ml of 2% sodium sulfate aqueous solution , shake for 3 minutes and then stand for 10 minutes to separate the organic and aqueous phases.
[0025] 3. Concentration: the upper organic phase was dried with 10 g of anhydrous sodium sulfate, and concentrated to 1 ml by rotary evaporation at 40°C.
[0026] 4. Purification: use glass chromatography silica ...
Embodiment 3
[0029] 1. Soil sample crushing: Freeze-dry the collected soil environmental samples, grind and crush them with a planetary ball mill, and pass through a 100-mesh stainless steel sieve.
[0030] 2. Extraction: Accurately weigh 10 grams of soil samples into a 150 ml corked Erlenmeyer flask, add 25 ml of petroleum ether / acetone (volume ratio 2:1) as the extractant, shake well and soak for 2 hours, then ultrasonicate at 100 Hz Extract for 20 minutes, after standing for stratification, transfer the supernatant to a 125 ml separatory funnel, repeat the above extraction process once, transfer the supernatant to a separatory funnel, add 30 ml of 2% sodium sulfate aqueous solution , shake for 3 minutes and then stand for 10 minutes to separate the organic and aqueous phases.
[0031] 3. Concentration: the upper organic phase was dried with 10 g of anhydrous sodium sulfate, and concentrated to 1 ml by rotary evaporation at 40°C.
[0032] 4. Purification: use glass chromatography silica...
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