Detection method of chlopyrifos pesticide and three metabolites thereof in soil

Abstract

The invention discloses a detection method of chlopyrifos pesticide and three metabolites thereof in soil. The method is as below: first weighing a soil sample, adding anhydrous sodium sulfate and anhydrous magnesium sulfate, then adding an acetic acid acetonitrile solution, carrying out ultrasonic extraction, and centrifuging; concentrating the acetonitrile extract obtained after the centrifugation, and then setting to a constant volume with a mobile phase, transferring to a a centrifugal tube filled with a mixed filler, and conducting ultrasonic treatment and centrifugation; placing a supernatant in a machine, detecting by using a liquid chromatogram analysis method, so as to obtain contents of chlorpyrifos pesticide and three metabolites thereof in soil. The invention uses soil as the matrix, and employs a matrix dispersive solid phase extraction technique for pretreatment on the sample; and the method can simultaneously detect chlorpyrifos pesticide and three metabolites thereof, and has the characteristics of accurate detection, high efficiency, fastness 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...

Examples

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...

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...

Examples

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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