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Method of detecting flusilazole, fipronil, chlorfenapyr and fenpyroximate in environmental water sample

A determination method and flusilazole technology are applied in the field of detection of pesticide residues in environmental water samples, which can solve the problems of high cost and consumption, single residue can not meet the requirements of rapid and accurate detection, time-consuming and labor-intensive, etc., achieving simple operation and saving detection time. and cost, the effect of accurate analysis results

Inactive Publication Date: 2014-03-05
QINGDAO TECHNOLOGICAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, single-residue detection can no longer meet the requirements of rapid and accurate detection in practical applications, and it is time-consuming, laborious, and costly.
At present, there is no simultaneous detection method for the four pesticide residues of flusilazole, fipronil, chlorfenapyr and pyraflux in environmental water samples

Method used

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  • Method of detecting flusilazole, fipronil, chlorfenapyr and fenpyroximate in environmental water sample
  • Method of detecting flusilazole, fipronil, chlorfenapyr and fenpyroximate in environmental water sample
  • Method of detecting flusilazole, fipronil, chlorfenapyr and fenpyroximate in environmental water sample

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Experimental program
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specific Embodiment approach

[0030] A method for the determination of flusilazole, fipronil, chlorfenapyr and pyrazafen in environmental water bodies, using solid phase extraction-liquid chromatography for determination, using multi-walled carbon nanotubes as solid phase extraction adsorbents, the obtained The specific steps of the method are as follows:

[0031] (1) Load 150 mg of multi-walled carbon nanotubes into a solid-phase extraction column with a packing height of about 1 cm, and seal both ends with polyethylene porous sieve plates;

[0032] (2) The solid phase extraction column was activated with ethyl acetate, methanol and water respectively;

[0033] (3) 1L water sample with a concentration of 0.2μg / L passes through the solid phase extraction column described in step (1) at a rate of 5mL / min;

[0034] (4) Use 10mL ethyl acetate as the eluent to elute the target substance from the adsorbent;

[0035] (5) The eluent was blown dry with nitrogen gas at room temperature, and the volume was adjuste...

experiment example

[0038] (1) Investigation on extraction recovery rate of different extraction columns

[0039] The selection of solid phase extraction column material is the most important factor affecting the efficiency of solid phase extraction. The present invention compares the use of multi-walled carbon nanotubes and other three kinds of commercial solid phase extraction small columns SupelcleanENVI-Carb, SupelcleanLC-18, Extraction recovery of target compound by Cleanert ODSSPE. The result shows: for 4 kinds of compounds that the present invention analyzes, the extraction recovery rate of multi-walled carbon nanotube column can be compared with commercialized C 18 The extraction recoveries of the columns were comparable, however, the SupelcleanLC-18 was expensive. Moreover, multi-walled carbon nanotubes and C 18 The functional groups and adsorption mechanism of multi-walled carbon nanotubes are different, and the four kinds of compounds of flusilazole, fipronil, chlorfenapyr and pyracl...

Embodiment 2

[0054] Measure four kinds of pyrazoles and pyrrole pesticides (i.e. flusilazole, fipronil, chlorfenapyr and For the residual amount of pyraclofen), the water sample was filtered with a 0.45 μm filter membrane before determination.

[0055] Adopt solid-phase extraction-liquid chromatography to measure, multi-walled carbon nanotubes are used as solid-phase extraction adsorbent, and the concrete steps of described method are as follows:

[0056] (1) Load 150 mg of multi-walled carbon nanotubes into a solid-phase extraction column with a packing height of about 1 cm, and seal both ends with polyethylene porous sieve plates;

[0057] (2) The solid phase extraction column was activated with ethyl acetate, methanol and water respectively;

[0058] (3) 1L water sample with a concentration of 0.2μg / L passes through the solid phase extraction column described in step (1) at a rate of 5mL / min;

[0059] (4) Use 10mL ethyl acetate as the eluent to elute the target substance from the adso...

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Abstract

The invention relates to detection methods of pesticide residues in environmental water samples, and particularly relates to a method of detecting flusilazole, fipronil, chlorfenapyr and fenpyroximate in an environmental water sample. The method specifically comprises the following steps: filling a 150mg multiwalled carbon nanotube in a solid phase extraction column, wherein the filling height is about 1cm, and sealing two ends by a polyethylene porous sieve plate; respectively activating the solid phase extraction column by ethyl acetate, methanol and water; passing through 1L of water sample through the solid phase extraction column at a rate of 5mL / min; eluting by taking 10mL of ethyl acetate as an eluant; and feeding the eluant which is dried by nitrogen at constant temperature and metered by acetonitrile to 0.2mL in volume for liquid chromatogram analysis. The method provided by the invention has higher sensitivity and precision, and is simple and convenient to operate, thereby greatly saving the detection time and cost. The average recovery rate is 92.2-105.9%, and the analysis result is accurate.

Description

technical field [0001] The invention relates to a method for detecting pesticide residues in environmental water samples, in particular to a method for determining flusilazole, fipronil, chlorfenapyr and pyrazafen in environmental water samples by solid-phase extraction-liquid chromatography. Background technique [0002] Flusilazole, fipronil, chlorfenapyr and pyraclofen are four important pesticides in pyrazole and pyrrole derivatives. They are an important class of heterocyclic compounds with high efficiency, good bactericidal ability, and low toxicity. It is mainly used in the fields of weeding and insecticide, and is recommended by many pesticide experts as one of the preferred varieties to replace highly toxic organophosphorus pesticides. This kind of pesticide has been widely used in the comprehensive control of pests in rice, vegetables, fruit trees and ornamental plants, but its entry into the water will cause water pollution, thereby causing harm to the human body....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 马继平卢曦闫凤丽姜莲华
Owner QINGDAO TECHNOLOGICAL UNIVERSITY
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