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Method of convenient detection of dithiocarbamate pesticide

A technology of dithiocarbamic acid and salts, applied in the field of analytical chemical detection, can solve the problems of stability and selectivity of nanomaterials, detection of pesticide residues, bulky and other problems, and achieves high sensitivity, good accuracy, and rapid analysis. Effect

Active Publication Date: 2018-09-04
海南特谱农业科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, rapid detection of pesticide residues remains challenging as these methods may be affected by the stability and selectivity of nanomaterials
Recently, atomic emission spectrometry (AES) with high stability and selectivity for special elements has been successfully applied to the determination of pesticides. However, traditional bench-top AES instruments are usually bulky, expensive, high power consumption, and portable instruments. Difficult to quickly detect pesticide residues in the field

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Example 1: Detection of Zinc Residue in Cucumber

[0021] 1. After preparing the cucumber sample homogenate, weigh 5g sample, add 0.1g L-cysteine, 20mL EDTA extract (0.2mol / L), homogenize at high speed for 1min, centrifuge at 4000rpm for 3min, take the supernatant As a sample solution. Take 2mL sample solution and 5mL carrier liquid (methanol+water) mixed to obtain the detection solution, and then input the liquid chromatographic column for separation, and qualitative the pesticides in the sample solution according to the retention time.

[0022] 2. The detection solution (a mixture of sample solution and carrier liquid) separated by a liquid chromatography column and a reducing solution (SnCl 2 / HCl solution, in which SnCl 2 The concentration is 10g L -1 , HCl concentration is 2.0mol L -1 ) After mixing 15mL, use microwave radiation with a power of 300W to reduce the zinc disulfide in the test solution to carbon disulfide (CS 2 ), and then mixed with helium at a flow rate o...

Embodiment 2

[0024] Example 2: Detection of Zinc Residue in Cowpea

[0025] 1. After preparing the cowpea sample homogenate, weigh 5g sample, add 0.1g L-cysteine, 25mL EDTA extract (0.2mol / L), homogenize at high speed for 1min, centrifuge at 4000rpm for 3min, take the supernatant As a sample solution. Take 2mL sample solution and 10mL carrier liquid (methanol+water) mixed to obtain the detection solution, and then input into the liquid chromatographic column for separation, according to the retention time to determine the type of pesticides in the sample solution.

[0026] 2. The detection solution (a mixture of sample solution and carrier liquid) separated by a liquid chromatography column and a reducing solution (SnCl 2 / HCl solution, in which SnCl 2 The concentration is 20g L -1 , The concentration of HCl is 2.5mol L -1 ) After mixing 25mL, use 700W microwave radiation to reduce the zinc disulfide in the test solution to carbon disulfide (CS 2 ), and then mixed with helium at a flow rate of ...

Embodiment 3

[0028] Example 3: Detection of Zinc Residue in Grapes

[0029] 1. After preparing the homogenate of the grape sample, weigh 5 g of the sample, add 0.1 g of L-cysteine, 20 mL of EDTA extract (0.2 mol / L), homogenize at high speed for 1 min, centrifuge at 4000 rpm for 3 min, and take the supernatant As a sample solution. Take 2mL of sample solution and 15mL of carrier liquid (methanol+water) to mix to obtain the detection solution, and then input it into the liquid chromatographic column for separation, and qualitatively determine the types of pesticides in the sample solution according to the retention time.

[0030] 2. The detection solution (a mixture of sample solution and carrier liquid) separated by a liquid chromatography column and a reducing solution (SnCl 2 / HCl solution, in which SnCl 2 The concentration is 25g L -1 , The concentration of HCl is 3.0mol L -1 ) After 30mL of mixing, use microwave radiation with a power of 500W to reduce the zinc disulfide in the test solution...

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PUM

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Abstract

The invention belongs to the field of analytical chemical detection and relates to a method of convenient detection of a dithiocarbamate pesticide. The method comprises the steps of drawing a standardcurve, mixing and conveying a sample solution and a carrier solution into a liquid chromatography column for separation, reducing to carbon disulfide through microwave radiation after mixing with a reduction solution, mixing with carrier gas, performing cooling and gas-liquid separation, exciting a CS2 emission spectrum through a DBD (dielectric barrier discharge) device, selecting 257.94nm as acharacteristic emission line of CS2, performing quantitation by using peak area, and obtaining a concentration of the dithiocarbamate pesticide in the sample solution. According to the method, DTCs (dithiocarbamates) are reduced to CS2 by microwave-assisted SnCl2; the method has a good reduction effect; DBD microplasma is used for exciting the CS2 emission spectrum; the peak area is used for quantitation; the detection and analysis of pesticide residue is achieved; the method is subjected to few interference, and is high in sensitivity, quick, simple and convenient in analysis and low in cost;and device miniaturization and portability are facilitated.

Description

Technical field [0001] The invention belongs to the field of analytical chemistry detection, and relates to a rapid detection method for pesticide residues, in particular to a high-sensitivity microwave-assisted reduction of stannous chloride / hydrochloric acid solution-microplasma excitation emission spectrometry for the determination of dithiocarbamate pesticides The detection method. Background technique [0002] Dithiocarbamates (DTCs) are a general term for a class of organosulfur pesticides and are traditional protective fungicides, which account for 30% of the world's fungicides market. The current measurement methods for DTCs usually use SnCl 2 Revert it to CS 2 , And then use gas chromatography and gas chromatography tandem mass spectrometry for analysis. Kazos et al used gas chromatography tandem mass spectrometry (Chemosphere.2007, 68(11), 2104-2110.), Wang Yanli used headspace gas chromatography to study mancozeb and its metabolite ETU in tomatoes and cucumbers. Resi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/73
CPCG01N21/73
Inventor 韩丙军何燕李雅钱兵彭黎旭
Owner 海南特谱农业科技有限公司