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A detection method of chlorpyrifos pesticide and its three metabolites in soil

A chlorpyrifos pesticide and detection method technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of limited and rare detection items, and achieve the effects of improving extraction efficiency, reducing losses, and simple pretreatment

Inactive Publication Date: 2016-08-31
INST OF ENVIRONMENT & SUSTAINABLE DEV IN AGRI CHINESE ACADEMY OF AGRI SCI
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  • Description
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Problems solved by technology

[0003] At present, the methods for chlorpyrifos residues in soil mainly use gas chromatography, liquid chromatography and gas-liquid chromatography-mass spectrometry methods, and the detection items are limited to chlorpyrifos and its main metabolite 3,5,6-trichloro-2-pyridinol (TCP) , and the detection methods for the other two metabolites of chlorpyrifos: 3,5,6-2-methoxy-pyridine (TMP) and chlorpyrifos oxide (Chlorpyrifos-Oxon) are still rare

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  • A detection method of chlorpyrifos pesticide and its three metabolites in soil
  • A detection method of chlorpyrifos pesticide and its three metabolites in soil
  • A detection method of chlorpyrifos pesticide and its three metabolites in soil

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Embodiment 1

[0033] In this embodiment, taking black soil as an example, a mixed standard solution of chlorpyrifos pesticide and its three metabolite compounds was prepared, and 0.01, 0.05 and 0.1mg / Kg pesticide standard were added for recovery, and each content level was repeated 3 times.

[0034] Firstly, weigh 5.0 g of a uniformly prepared sample into a 50 mL centrifuge tube, add pesticide standards at the above three concentrations, and repeat 3 times for each concentration level. Then the soil sample containing chlorpyrifos and its three metabolites was vortexed and left for 2 hours to allow the pesticide to fully adsorb to the soil. Then add 0.5 g of anhydrous sodium sulfate and 4.0 g of anhydrous magnesium sulfate, add 20 mL of 1% acetic acid acetonitrile solution, ultrasonically extract for 10 min, and centrifuge at 5000 r / min for 5 min. Then it was concentrated to dryness, and the volume was adjusted to 2 mL with acetonitrile:water (0.1% acetic acid) 90:10. Concentrated and const...

Embodiment 2

[0048] In this example, purple clay was taken as an example to prepare a mixed standard solution of chlorpyrifos pesticide and its three metabolite compounds, and add 0.01, 0.05 and 0.1mg / Kg pesticide standard substances for recovery, and repeat 3 times for each content level.

[0049] Firstly, weigh 5.0 g of a uniformly prepared sample into a 50 mL centrifuge tube, add pesticide standards at the above three concentrations, and repeat 3 times for each concentration level. Then the soil sample containing chlorpyrifos and its three metabolites was vortexed and left for 2 hours to allow the pesticide to fully adsorb to the soil. Then add 0.8 g of anhydrous sodium sulfate and 5.0 g of anhydrous magnesium sulfate, add 25 mL of 1% acetic acid acetonitrile solution, ultrasonically extract for 15 min, and centrifuge at 7500 r / min for 5 min. Then it was concentrated to dryness, and the volume was adjusted to 2 mL with acetonitrile: water (0.1% acetic acid) 40:60. Concentrated and cons...

Embodiment 3

[0063] In this embodiment, taking red soil as an example, a mixed standard solution of chlorpyrifos pesticide and its three metabolite compounds was prepared, and 0.01, 0.05 and 0.1mg / Kg pesticide standard were added for recovery, and each content level was repeated 3 times.

[0064] Firstly, weigh 5.0 g of a uniformly prepared sample into a 50 mL centrifuge tube, add pesticide standards at the above three concentrations, and repeat 3 times for each concentration level. Then the soil sample containing chlorpyrifos and its three metabolites was vortexed and left for 2 hours to allow the pesticide to fully adsorb to the soil. Then add 0.6 g of anhydrous sodium sulfate and 5.0 g of anhydrous magnesium sulfate, add 30 mL of 1% acetic acid acetonitrile solution, ultrasonically extract for 20 min, and centrifuge at 5500 r / min for 5 min. Then it was concentrated to dryness, and the volume was adjusted to 2 mL with acetonitrile: water (0.1% acetic acid) 50:50. Concentrated and consta...

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Abstract

The invention discloses a method for detecting chlorpyrifos pesticide and three metabolites thereof in soil. Firstly weigh the soil sample, add anhydrous sodium sulfate and anhydrous magnesium sulfate, then add acetic acid acetonitrile solution, after ultrasonic extraction, carry out centrifugation; concentrate the acetonitrile extract obtained after centrifugation, then use the mobile phase to make up volume, transfer to the container put into a centrifuge tube with mixed filler, ultrasonically, centrifuge, take the supernatant and filter, then put it on the machine, and use the liquid chromatography analysis method to detect, and obtain the content of chlorpyrifos pesticide and its three metabolites in the soil. The invention uses soil as a matrix, uses matrix dispersion solid phase extraction technology to pretreat samples, and can simultaneously measure the detection of chlorpyrifos pesticide and its three metabolites. The method has the characteristics of accurate detection, high efficiency, rapidity and low price.

Description

technical field [0001] The invention belongs to the technical field of environmental detection methods, and in particular relates to a detection method of chlorpyrifos pesticide and three metabolites thereof in soil. Background technique [0002] With the prohibition of highly toxic pesticides such as methamidophos, chlorpyrifos (Chlorpyrifos) has been widely used and promoted as an alternative pesticide. In recent years, people have monitored and detected chlorpyrifos and its metabolites in soil and water respectively, and people have also paid great attention to the residue and distribution of chlorpyrifos and its metabolites in the environment. It is urgent and important to develop a pretreatment and analysis method for chlorpyrifos pesticide and its three metabolites in soil, in order to find out the residual content and distribution of chlorpyrifos and its three metabolites in soil, and to evaluate planting safety. [0003] At present, the methods for chlorpyrifos resi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/08G01N30/14
Inventor 孙宝利陕红董一威黄金丽仝乘风
Owner INST OF ENVIRONMENT & SUSTAINABLE DEV IN AGRI CHINESE ACADEMY OF AGRI SCI