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Pretreatment method for measuring multiresidues of pesticides in environmental biology

A pesticide residue and environmental technology, applied in the field of pretreatment for the determination of multi-pesticide residues in environmental organisms, can solve the problems of not reducing multi-step centrifugation and vortex operations, limiting the batch processing speed of multi-pesticide residue detection, etc.

Active Publication Date: 2017-08-11
ZHEJIANG ACADEMY OF AGRICULTURE SCIENCES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, most of the relevant research is based on the improvement of the extract solution, purification powder and extraction agent in the QuEChERS method, without reducing the multi-step centrifugation and vortex operation, which limits the batch processing speed of multi-pesticide residue detection, so the QuEChERS method still has great limitations sex

Method used

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  • Pretreatment method for measuring multiresidues of pesticides in environmental biology
  • Pretreatment method for measuring multiresidues of pesticides in environmental biology

Examples

Experimental program
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Effect test

Embodiment 1

[0058] The Fe 3 o 4 -SiO 2 The preparation of magnetic particles includes the following steps:

[0059] Add a mixture of 2g cetyl ammonium bromide and 200ml water to a 1000ml three-necked flask, stir until dissolved; put 1000mg Fe into the beaker 3 o 4 and 100ml of water; ultrasonic for 10 minutes (dropper stirring), added to a 1000ml three-neck flask; 200ml of water was added, mechanically stirred; 50mg (about 60ul) of concentrated ammonia water was added, and mechanically stirred; heated to 60°C under nitrogen protection, And a mixed solution of 1.4ml ethanol and 2.5ml tetraethyl orthosilicate was added dropwise, and after the dropwise addition was completed, the reaction was continued at 60° C. for 12 hours.

[0060] After the reaction, use a magnet to separate the product from the mother liquor; move the product into a 100ml centrifuge tube, and repeat the following operation 6 times: add 25ml of acetone, and sonicate for 10-15 minutes; finally, use a magnet to separat...

Embodiment 2

[0062] The concentration of the mixed pesticide standard solution in the earthworm sample is 0.3mg / L.

[0063] Weigh 2.0g of earthworm samples (accurate to ±0.01g) into a 50ml polypropylene centrifuge tube with stopper, add 3ml of water, and vortex for 1min to completely disperse the sample. Add 6ml of acetonitrile, vortex for 1min, sonicate for 15min, homogenize with a high-speed homogenizer for 1min, add 3.6gMgSO 4 and 0.9g NaCl, shake vigorously, centrifuge at 3500r / min for 3min, and take the acetonitrile extract to be purified.

[0064] Accurately pipette 1.0ml of acetonitrile extract and add to the Fe containing 30mg embodiment 1 preparation 3 o 4 -SiO 2 , 20mgZrO 2 , 30mg PSA adsorbent and 150mg MgSO 4 In a 2ml centrifuge tube, after shaking for 1min, put it on the magnetic stand for 3 seconds to completely separate, pipette 0.5ml supernatant into a 2ml centrifuge tube filled with 0.5ml water, mix well, and filter with a 0.22μm filter membrane , to obtain the super...

Embodiment 3

[0066] Weigh 2.0 g (accurate to ±0.01 g) of the earthworm sample described in Example 2 into a 50 ml polypropylene centrifuge tube with stopper, add 4 ml of water, and vortex for 1 min to completely disperse the sample. Add 8ml of acetonitrile, vortex for 1min, sonicate for 15min, homogenize with a high-speed homogenizer for 1min, add 3.6g of MgSO 4 and 0.9gNaCl, shake vigorously, centrifuge at 3000r / min for 5min, and take the acetonitrile extract to be purified.

[0067] Accurately pipette 1.0ml of acetonitrile extract and add to the Fe containing 30mg embodiment 1 preparation 3 o 4 -SiO 2 , 40mgZrO 2 , 30mg PSA adsorbent and 150mg MgSO 4 In a 2ml centrifuge tube, after shaking for 1min, place it on a magnetic stand for 2 seconds to completely separate, pipette 0.5ml supernatant into a 2ml centrifuge tube filled with 0.5ml water, mix well, and filter with a 0.22μm filter membrane , to obtain the supernatant to be analyzed by UPLC-MS / MS.

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Abstract

The invention provides a pretreatment method for measuring multiresidues of pesticides in environmental biology. The method comprises the steps of mixing environmental biology earthworms with water to obtain an earthworm-water mixed solution; conducting ultrasound mixing on the earthworm-water mixed solution and acetonitrile, afterwards conducting homogenating, mixing a homogenating sizing agent with inorganic salts, and conducting vibrating and solid-liquid separation to obtain an acetonitrile extraction solution; mixing the acetonitrile extraction solution with Fe3O4-SiO2 magnetic particles, ZrO2, a PSA absorbent and a water absorbent to obtain mixed feed liquor; vibrating the mixed feed liquor, conducting magnetic separation and filtering, and then collecting clean liquor. According to the pretreatment method for measuring multiresidues of the pesticides in the environmental biology, aiming at the characteristics that an earthworm matrix is high in fat and protein, ZrO2 and PSA absorbent are selected as a purifying material, and based on the superparamagnetism advantage of a magnetic nano material Fe3O4-SiO2 and the selectivity of the magnetic nano material Fe3O4-SiO2, the pretreatment method for quickly measuring the multiresidues of pesticides in the environmental biology is built, and thus quick and precise measurement of multiresidues of the pesticides in the environmental biology is achieved.

Description

technical field [0001] The invention belongs to the technical field of pesticide residues, and in particular relates to a pretreatment method for measuring multiple pesticide residues in environmental organisms. Background technique [0002] With the continuous growth of the agricultural economy, in order to improve the yield and quality of crops, pesticides are used in large quantities, but only 1% of them play a practical role, and about 60% of them escape into the soil. The pesticides remaining in the soil will seriously affect the environmental biological safety. Therefore, it is of great significance to establish an analytical method for the rapid determination of multi-pesticide residues in the environment. In soil ecosystems, earthworms are the largest group of terrestrial animals, and they are an important part of controlling soil ecosystems and energy flow. Earthworms are at the bottom of the food chain, and their contamination will affect the safety of higher orga...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06
CPCG01N30/06
Inventor 齐沛沛王新全王祥云孙宇涵汪志威徐霞红章虎徐浩王强
Owner ZHEJIANG ACADEMY OF AGRICULTURE SCIENCES
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