A solid-phase extraction detection method for neonicotinoid insecticides and their transformation products in water

A technology for conversion products and neonicotinoids, which is applied in measurement devices, instruments, scientific instruments, etc., can solve the problems of low recovery rate, loss of target compounds, and large differences, and achieve good adsorption performance, low matrix effect, and operation methods. Simple and accurate results

Active Publication Date: 2022-03-08
JINAN UNIVERSITY
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  • Abstract
  • Description
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  • Application Information

AI Technical Summary

Problems solved by technology

However, the commonly used hydrophilic-lipophilic balance (HLB) solid-phase extraction column is not ideal for the extraction of highly polar neonicotinoid insecticides, especially their transformation products
For example, the target compound will be lost during the processing of the sample to be tested, the recovery rate is low, and the accuracy of the test method cannot be guaranteed; in addition, there are many types of neonicotinoid insecticides and their transformation products, with huge differences, and it is difficult to simultaneously detect All compounds tested

Method used

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  • A solid-phase extraction detection method for neonicotinoid insecticides and their transformation products in water
  • A solid-phase extraction detection method for neonicotinoid insecticides and their transformation products in water
  • A solid-phase extraction detection method for neonicotinoid insecticides and their transformation products in water

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Comparison of Adsorption Effects of Mixed Adsorbent SPE Columns with HLB, WAX and WCX SPE Columns

[0041]The new mixed adsorbent solid-phase extraction method of the present invention was compared with the commonly used HLB, WAX and WCX solid-phase extractions on the adsorption effects of neonicotinoid insecticides and their conversion products.

[0042] 1) 200 mg of mixed adsorbent, HLB, WAX and WCX solid-phase extraction fillers with a mass ratio of HLB: WAX: WCX = 2: 1: 1 were respectively dry-processed under the condition of vacuuming on the solid-phase extraction system. Put it into a 6mL polypropylene empty tube solid phase extraction column, and fix the upper and lower ends of the mixed filler through the sieve plate, that is, each solid phase extraction column with different fillers.

[0043] 2) Activation: each solid phase extraction cartridge was activated with 5mL methanol and 5mL pure water sequentially.

[0044] 3) Sample loading: set the pH to 7, mix 14 ...

Embodiment 2

[0049] Example 2 Different proportioning mixed adsorbent extraction effect

[0050] 1) Fill 200 mg of mixed adsorbent with a mass ratio of HLB: WAX: WCX = 4: 1: 1, and put it into a 6 mL polypropylene empty tube by dry method under the condition of vacuuming on the solid phase extraction system In the solid phase extraction column, the upper and lower ends of the mixed filler are fixed by the sieve plate, which is the mixed adsorbent solid phase extraction column.

[0051] 2) Activation: The mixed solid phase extraction cartridge was activated with 5mL methanol and 5mL pure water in sequence.

[0052] 3) Sample loading: 200 mL of a mixed aqueous solution of 14 neonicotinoid insecticides and their transformation products (Dr. Ehrenstorfer Gmbh, Augsburg, Germany) with a theoretical spiked concentration of 1000 ng / L was adjusted with dilute hydrochloric acid. After the pH value of the aqueous solution was 4, it was loaded through the sample loading tube at a flow rate of 2-3 mL...

Embodiment 3

[0057] Example 3 Extraction Effect of Different Proportioning Mixed Adsorbents

[0058] 1) Fill 200 mg of mixed adsorbents with a mass ratio of HLB:WAX:WCX=1:2:2, and put them into empty tubes made of 6 mL polypropylene by dry method under the condition of vacuuming on the solid phase extraction system In the solid phase extraction column, the upper and lower ends of the mixed filler are fixed by the sieve plate, which is the mixed adsorbent solid phase extraction column.

[0059] 2) Activation: The mixed solid phase extraction cartridge was activated with 5mL methanol and 5mL pure water in sequence.

[0060] 3) Sample loading: 200 mL of a mixed aqueous solution of 14 neonicotinoid insecticides and their transformation products (Dr. Ehrenstorfer Gmbh, Augsburg, Germany) with a theoretical spiked concentration of 1000 ng / L was adjusted with dilute hydrochloric acid. After the pH value of the aqueous solution was 4, it was loaded through the sample loading tube at a flow rate o...

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Abstract

The invention belongs to the technical field of insecticide detection and discloses a solid-phase extraction detection method for neonicotinoid insecticides and transformation products thereof in water. It specifically includes the following steps: (1) activating the solid phase extraction column; (2) adding a recovery rate indicator after adjusting the pH value of the water sample, and then extracting the water sample in the solid phase extraction column; (3) extracting the solid phase extraction column. After the phase extraction column is dried in vacuum, the eluent is obtained by elution, and then an internal standard compound is added; (4) Detecting the concentration of the target compound. The present invention adopts self-loading mixed adsorbent solid-phase extraction small column with simple and convenient operation method, can simultaneously analyze neonicotinoid insecticides and their transformation products in water, and has a good effect on neonicotinoid insecticides and their transformation products Adsorption performance, the detection limit in surface water is 0.56-5.43ng / L, and the matrix effect is -7.58%-21.1%.

Description

technical field [0001] The invention belongs to the technical field of insecticide detection, and in particular relates to a solid-phase extraction detection method for neonicotinoid insecticides and transformation products thereof in water. Background technique [0002] Neonicotinoid insecticides are a new type of insecticides that are currently used on a large scale after traditional insecticides such as organochlorines, organophosphorus, and pyrethroids. They have been registered for use in more than 120 countries, accounting for the global More than 25% of the insecticide market, mainly acetamiprid, clothianidin, dinotefuran, imidacloprid, nitenpyram, thiacloprid, thiamethoxam. Neonicotinoid insecticides are highly water-soluble and can easily enter the water environment system. Their harm to non-target aquatic organisms has gradually been recognized and paid attention to by people. On the other hand, the parent compounds of neonicotinoid insecticides in the environment...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
CPCG01N30/02G01N2030/045G01N2030/009
Inventor 熊晶晶谭保祥李慧珍马雪游静
Owner JINAN UNIVERSITY
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