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A pretreatment method for the determination of multi-pesticide residues in environmental organisms

A pesticide residue and environmental technology, which is applied in the field of pretreatment for the analysis of environmental biological organic pollutants, can solve the problems of not reducing the operation process of multi-step centrifugation and vortexing, and limiting the batch processing speed of multi-pesticide residue detection.

Active Publication Date: 2019-05-17
ZHEJIANG ACADEMY OF AGRICULTURE SCIENCES
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  • Abstract
  • Description
  • Claims
  • Application Information

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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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  • A pretreatment method for the determination of multi-pesticide residues in environmental organisms
  • A pretreatment method for the determination of multi-pesticide residues in environmental organisms
  • A pretreatment method for the determination of multi-pesticide residues in environmental organisms

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 cetylammonium bromide and 200ml water into a 1000ml three-necked flask, stir until it dissolves; put 1000mg Fe into the beaker 3 O 4 And 100ml water; ultrasonic for 10 minutes (dropper stirring), add to a 1000ml three-necked flask; add 200ml water, mechanically stir; add 50mg (about 60ul) concentrated ammonia water, mechanically stir; heat to 60℃ under nitrogen protection, A mixture of 1.4ml ethanol and 2.5ml tetraethylorthosilicate was added dropwise. After the dropwise addition was completed, the reaction was maintained 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 operations 6 times: add 25ml of acetone and ultrasound for 10-15 minutes; finally, the product is separated from the acetone by magnet adsorption. The obtained p...

Embodiment 2

[0062] The concentration of pesticide standard solution mixed with earthworm samples is 0.3mg / L.

[0063] Weigh 2.0g earthworm sample (accurate to ±0.01g) into a 50ml polypropylene centrifuge tube with stopper, add 3ml of water, vortex for 1min, to make the sample completely dispersed. Add 6ml of acetonitrile, vortex for 1min, ultrasonic for 15min, homogenize with a high-speed homogenizer for 1min, add 3.6g MgSO 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 acetonitrile extract and add it to the Fe prepared in Example 1 containing 30mg 3 O 4 -SiO 2 , 20mgZrO 2 , 30mg PSA adsorbent and 150mg MgSO 4 After shaking for 1 min, place it on a magnetic stand for 3 seconds to separate completely. Pipette 0.5ml supernatant into a 2ml centrifuge tube with 0.5ml water, mix well, and filter with 0.22μm filter membrane , Obtain the supernatant for UPLC-MS / MS analysis.

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 a stopper, add 4 ml of water, and vortex for 1 min to completely disperse the sample. Add 8ml of acetonitrile, vortex for 1min, ultrasonic for 15min, homogenize with a high-speed homogenizer for 1min, add 3.6g MgSO 4 And 0.9g NaCl, shake vigorously, centrifuge at 3000r / min for 5min, and take the acetonitrile extract to be purified.

[0067] Accurately pipette 1.0ml acetonitrile extract and add it to the Fe prepared in Example 1 containing 30mg 3 O 4 -SiO 2 , 40mgZrO 2 , 30mg PSA adsorbent and 150mg MgSO 4 In the 2ml centrifuge tube, shake for 1min, place it on the magnetic stand for 2 seconds to complete separation, transfer 0.5ml supernatant to a 2ml centrifuge tube containing 0.5ml water, mix well, and filter with 0.22μm filter membrane , Obtain the supernatant for UPLC-MS / MS analysis.

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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 analysis pretreatment methods for environmental biological organic pollutants. Background technique [0002] With the continuous growth of the agricultural economy, in order to increase the yield and quality of crops, pesticides are used in large quantities, but only 1% of them play a practical role, and about 60% are scattered in the soil. Pesticides remaining in the soil will seriously affect environmental biosafety. Therefore, it is of great significance to establish an analytical method for rapid determination of multiple pesticide residues in the environment. In the soil ecosystem, earthworms are the largest type of terrestrial animal, and they are an important part of controlling the soil ecosystem and energy flow. Earthworms are at the bottom of the food chain, and their contamination will affect the safety of higher-level organisms in the food chain. Therefore, it is often regarded as a representativ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/06
CPCG01N30/06
Inventor 齐沛沛王新全王祥云汪志威王强
Owner ZHEJIANG ACADEMY OF AGRICULTURE SCIENCES
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