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

Inactive Publication Date: 2015-02-25
SHENYANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Due to the complex composition of the soil and the residues and interference of other organic pollutants such as polycyclic aromatic hydrocarbons, organochlorine and organophosphorus pesticides, it is more difficult to extract, separate, purify and enrich pyrethroid pesticides
At present, there are reports on the pretreatment methods for the detection of pyrethroid pesticide residues in soil environmental samples, but there is a problem that the amount of organic solvent is consumed in the process of extraction and purification.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

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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Abstract

The invention discloses a method for treating a pyrethroid pesticide residue soil environment sample before measurement, and relates to a method for analyzing and pretreating organic pollutants in soil environment samples. The method comprises the following steps: grinding a soil sample; performing freeze drying on the collected soil environment sample, grinding and crushing; extracting, namely accurately weighing the soil sample, adding petroleum ether / acetone, performing ultrasonic extraction, and adding 2 percent of sodium sulfate aqueous solution into a supernatant; concentrating, namely drying an upper-layer organic phase by virtue of anhydrous sodium sulfate, evaporating and concentrating; purifying by adopting a glass chromatography silica-gel column method, and performing wet column packing; concentrating and making up to the volume, namely dissolving and making up to the volume by using chromatographic n-hexane, and measuring the content of pyrethroid by adopting a gas chromatograph or a gas chromatograph-mass spectrometer. According to the method, multiple pyrethroid pesticide compounds can be extracted from the soil environment samples and are purified; according to the method, the cost is low, reproducibility and stability are high, and methods and technical supports are provided for detection and evaluation of pyrethroid pesticides in the soil environment samples.

Description

technical field [0001] The invention relates to a method for pre-analyzing organic pollutants in soil environment samples, in particular to a method for pre-determining soil environment samples with pyrethroid pesticide residues. Background technique [0002] Pyrethroid pesticides are a class of phenoxy-containing cyclopropane esters imitated according to the chemical structure of natural pyrethrins. Because of their high efficiency, low toxicity and rapid metabolism, pyrethroid pesticides have been used since 1973. Since its birth in 2010, it has been used more and more widely in crop deinsectization and sanitation pest control. At present, with the prohibition of some highly toxic organophosphorus and carbamate pesticides in production, the usage of pyrethroid pesticides is second only to organophosphorus pesticides, ranking second in the insecticide market. At present, there are more than 70 varieties of pyrethroids that have been commercialized in the world, and the com...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/08G01N30/14
Inventor 宋雪英梁茹晶胡爽胡晓钧李玉双罗庆杨继松侯永侠
Owner SHENYANG UNIV
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