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Method of simultaneously detecting dicofol and pyrethroid pesticides in food

A technology of pyrethroids and dicofol, which is applied in the detection field of pesticide residues, can solve the problems of strong hydrophobicity and influence on the application of purification adsorbents, achieve high recovery rate, ensure stability and versatility

Inactive Publication Date: 2017-06-20
彭晓俊
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the lack of active functional groups on the surface of untreated multi-walled carbon nanotubes, strong hydrophobicity, insoluble and infusible, they will agglomerate into a dense network, which affects their application as purification adsorbents.

Method used

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  • Method of simultaneously detecting dicofol and pyrethroid pesticides in food
  • Method of simultaneously detecting dicofol and pyrethroid pesticides in food
  • Method of simultaneously detecting dicofol and pyrethroid pesticides in food

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] 1. Example 1: Preparation of modified multi-walled carbon nanotubes

[0041] Weigh 50g of multi-walled carbon nanotubes and place them in a 500mL flask, add 50mL of concentrated sulfuric acid, ultrasonicate for 30min, then add 30mL of concentrated nitric acid into the flask, ultrasonicate for 30min, let stand, use a straw to remove the supernatant mixed acid clear liquid, then add 1000mL Dilute with ultrapure water, filter the diluted solution through a 0.22 μm polytetrafluoroethylene microporous membrane, wash the filtrate with water until the pH of the filtrate is 7, and dry the obtained black solid in a vacuum oven at 50°C to obtain oxidized Modified multi-walled carbon nanotubes.

[0042] figure 1 TEM images of multi-walled carbon nanotubes before and after oxidative modification, represented by figure 1 It can be seen that the multi-walled carbon nanotubes obtained after oxidation modification are evenly dispersed, have a certain aspect ratio, and the length dist...

Embodiment 2

[0043] 2. Example 2: Detection of dicofol and pyrethroid pesticide residues in tangerine peel and tangerine peel Pu'er tea samples

[0044] This example is based on the improved QuEChERS method and gas chromatography-mass spectrometry to determine the residual amount of dicofol and pyrethroid pesticides in tangerine peel and its products. Specific steps are as follows:

[0045] (1) Absorb dicofol, bifenthrin, fenpropathrin, cyhalothrin, permethrin, cypermethrin, flucyvalerate, fenvalerate and deltamethrin pesticides with a concentration of 100 μg / mL respectively The standard product was diluted to volume with ethyl acetate-n-hexane mixed solution with a volume ratio of 1:1, and the concentrations of 0.010 μg / mL, 0.020 μg / mL, 0.050 μg / mL, 0.10 μg / mL, and 0.40 μg were prepared respectively. / mL, 1.0μg / mL mixed standard solution, and then perform gas chromatography-mass spectrometry on the mixed standard solution, take the quantitative ion chromatogram peak area as the ordinate ...

Embodiment 3

[0054] 3. Example 3: Detection of dicofol and pyrethroid pesticide residues in apples, rice, bananas, and citrus samples

[0055] The difference between this example and Example 2 is that in step 2, weigh 2.00 g of crushed apples, rice, bananas, and citrus samples in a 50 mL centrifuge tube with a stopper, add 2 mL of ultrapure water, shake for 1 min, and ultrasonically for 5 min. Add 5mL of ethyl acetate-n-hexane mixed solution with a volume ratio of 1:1, sonicate for 5min, centrifuge at 3000r / min for 5min, absorb the supernatant, then add 3mL of ethyl acetate-n-hexane mixed solution with a volume ratio of 1:1 and repeat Extract, combine supernatants and mix well.

[0056] Among them, the total ion chromatogram of the mixed standard solution of 0.01μg / mL is as follows image 3 Shown; The total ion current chromatogram of tangerine peel sample and the total ion chromatogram of dried tangerine peel Pu'er tea sample are respectively as shown in embodiment 1 Figure 4 and Fig...

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Abstract

The invention relates to a method of simultaneously detecting dicofol and pyrethroid pesticides in a food. The method comprises the following steps of: making a standard curve; performing ultrasonic centrifugal extraction on a sample with an extraction liquid to obtain a supernatant liquid; purifying the supernatant liquid by using a modified multi-walled carbon nanotube to obtain a sample purifying liquid; and performing gas chromatograph-mass spectrum assay on the sample purifying liquid. By taking the modified multi-walled carbon nanotube as a purifying adsorbent, an improved QuEChERS method and a gas chromatograph-mass spectrometer are combined and applied to simultaneously detecting dicofol and pyrethroid pesticides in apples, a rice, bananas, citrus, pericarpium citri reticulatae and a pericarpium citri reticulatae Pu'er tea sample. The method is simple to operate, high in accuracy and good in stability and meets the requirement of trace analysis.

Description

technical field [0001] The invention relates to a method for detecting pesticide residues, in particular to a method for simultaneously detecting dicofol and pyrethroid pesticides in food. Background technique [0002] Herbivorous mites are one of the main pests that harm agricultural products. The use of dicofol is the main means of preventing and controlling mites. Pyrethroid pesticides have a chemical structure similar to natural pyrethrins. Because of their high efficiency, broad spectrum, low toxicity, and low residue , has the characteristics of fast knockdown speed, wide range of action, and low toxicity to humans, and is widely used in the prevention of agricultural product diseases and pests. Therefore, it is of positive effect to formulate analytical methods for dicofol and pyrethroid pesticide residues in food. [0003] The QuEChERS (Quick, Easy, Cheap, Effective, Rugged, Safe) method is a rapid sample pretreatment technology for agricultural product testing deve...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/72G01N30/12G01N30/14G01N30/06
CPCG01N30/02G01N30/06G01N30/12G01N30/14G01N30/72G01N2030/146Y02A50/30
Inventor 彭晓俊蔡璇梁伟华伍长春
Owner 彭晓俊
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