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Method for detecting multicomponent residuals in organophosphorus pesticide in sediment by virtue of dispersive solid-phase extraction-gas chromatographic mass spectrometry

A gas chromatography-mass spectrometry and organophosphorus pesticide technology, which is used in measurement devices, material separation, and analysis of materials, etc., can solve the problems of cumbersome purification steps, limited application, and large amount of solvent used to achieve good impurity removal and purification effect and reduce interference. , the effect of fewer steps

Active Publication Date: 2017-01-25
MARINE FISHERIES RES INST OF ZHEJIANG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Pesticide residue removal and purification methods are mostly used for solid phase extraction column purification and gel permeation chromatography purification, the purification steps are cumbersome and the amount of solvent used is large
As a sample pretreatment method, matrix dispersive solid-phase extraction has been widely used in the analysis of vegetable samples with little organic matter, but its application in environmental samples rich in organic matter is limited.

Method used

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  • Method for detecting multicomponent residuals in organophosphorus pesticide in sediment by virtue of dispersive solid-phase extraction-gas chromatographic mass spectrometry
  • Method for detecting multicomponent residuals in organophosphorus pesticide in sediment by virtue of dispersive solid-phase extraction-gas chromatographic mass spectrometry
  • Method for detecting multicomponent residuals in organophosphorus pesticide in sediment by virtue of dispersive solid-phase extraction-gas chromatographic mass spectrometry

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Determination of 16 kinds of organophosphorus pesticides in a certain sea area sediment of Zhoushan in embodiment 1

[0019] (1) Sample solvent extraction: Accurately weigh 5.0g of a sediment sample from a sea area in Zhoushan into a 50mL centrifuge tube, add 20mL of acetonitrile + ethyl acetate (1:1 volume ratio) into the centrifuge tube, vortex for 2min, and extract by ultrasonic After 15 minutes, centrifuge at a speed of 5000r / min for 5 minutes, filter the supernatant into a 150mL rotary steamer, and repeatedly vortex and ultrasonically extract the residue with 20mL acetonitrile+ethyl acetate (1:1 volume ratio). Conditional centrifugation, filter the supernatant in the above 150mL rotary evaporator, and combine the extracts;

[0020] (2) Copper powder removal: add 1g of copper powder to the combined extract, concentrate the extract by rotary evaporation at 35°C to dryness, add acetonitrile to dissolve and dilute to 1.0mL;

[0021] (3) Purification by matrix dispersi...

Embodiment 2

[0026] Determination of 16 kinds of organophosphorus pesticides in a certain reservoir sediment of embodiment 2

[0027] (1) Sample solvent extraction: Accurately weigh 5.0g of a reservoir sediment sample into a 50mL centrifuge tube, add 20mL of acetonitrile + ethyl acetate (1:1 volume ratio) into the centrifuge tube, vortex for 2min, and ultrasonically extract for 15min Afterwards, centrifuge at a speed of 5000r / min for 5min, filter the supernatant into a 150mL rotary evaporator, use 20mL acetonitrile + ethyl acetate (1:1 volume ratio) to repeatedly vortex and ultrasonically extract the residue, and use the same conditions as above Centrifuge, filter the supernatant into the above-mentioned 150mL rotary evaporator, and combine the extracts;

[0028] (2) Copper powder removal: add 1g of copper powder to the combined extract, concentrate the extract by rotary evaporation at 35°C until almost dry, add acetonitrile to dissolve and dilute to 1.0mL;

[0029] (3) Purification by ma...

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Abstract

The invention discloses a method for detecting multicomponent residuals in an organophosphorus pesticide in a sediment by virtue of dispersive solid-phase extraction-gas chromatographic mass spectrometry. The method comprises the following steps of: 1, extracting a sample solvent so as to obtain extract liquid; 2, performing copper powder purification so as to obtain purification liquid; and 3, performing dispersive solid-phase extraction purification and gas chromatographic-mass spectrometry detection, and performing quantification by virtue of an external standard method. The method disclosed by the invention is convenient to operate, good in reproducibility, accurate in qualitative property and relatively high in recovery rate, is capable of rapidly analyzing multicomponent residuals in the organophosphorus pesticide in the sediment, and is capable of conveniently, rapidly and accurately measuring a trace organophosphorus pesticide in the sediment so as to realize quantitative and qualitative analysis on the trace organophosphorus pesticide in the sediment.

Description

technical field [0001] The invention relates to the technical field of environmental quality and safety detection, in particular to a method for detecting multi-component residues of organophosphorus pesticides in sediments by combining dispersive solid-phase extraction-gas chromatography-mass spectrometry. Background technique [0002] Organophosphorus pesticides are a class of pesticides that occupy the largest share in my country's pesticide market and are widely used. In theory, organophosphorus pesticides are considered to be easily degradable, difficult to bioaccumulate, and have less impact on the ecology. They were once considered as substitutes for organochlorine pesticides. In fact, organophosphorus pesticides can form phosphorylated cholinesterase with cholinesterase in the organism, thereby causing toxicity to the organism. At the beginning of 2010, the "poisonous cowpea" incident caused a sensation throughout the country, and organic phosphorus was detected in ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88G01N30/06
CPCG01N30/06G01N30/88
Inventor 孙秀梅金衍健郝青胡红美钟志郭远明
Owner MARINE FISHERIES RES INST OF ZHEJIANG