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Method for detecting organochlorine pesticide in soil

A detection method and organochlorine technology, applied in the field of analysis and detection, can solve the problems of expensive instruments and equipment, low analyte concentration, short operation time, etc., and achieve the effects of high efficiency, accurate qualitative and quantitative, and less solvent.

Pending Publication Date: 2020-09-11
TAIZHOU UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the complexity of the soil matrix and the low concentration of analytes, it is always challenging to extract pesticides and remove matrix interference, which is also a weak link in the detection of pesticide residues in soil at home and abroad.
At present, the pretreatment methods commonly used in soil samples include extraction and purification, such as liquid-liquid extraction, Soxhlet extraction, solid-phase microextraction, fast solvent extraction, etc. Although these methods are mature and stable, they are energy-intensive, time-consuming, and expensive A large number of toxic and harmful organic reagents, such as Soxhlet extraction, although the cost is low, but it takes a long time, and the rapid solvent extraction has a short operation time and high extraction efficiency, but the equipment is very expensive

Method used

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  • Method for detecting organochlorine pesticide in soil
  • Method for detecting organochlorine pesticide in soil
  • Method for detecting organochlorine pesticide in soil

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] 1.1 Blank soil sample preparation

[0032] Collect a batch of soil near the drinking water source, remove impurities such as grass roots, sand and gravel, put it on the sample tray, spread it to a thickness of about 20mm, freeze-dry it, pass it through a 60-mesh sieve, and grind it evenly to obtain the soil sample to be tested. The traditional method of rapid solvent extraction-solid phase extraction column purification was used to test the 8 kinds of organochlorine pesticides in the samples, and the soil samples whose detection concentration was lower than the detection limit of the method were selected as the blank soil samples for testing.

[0033] 1.2 Preparation of spiked soil for testing

[0034] Accurately weigh 50.0 g of the blank soil for testing, add 10 mL of mixed standard solution of 8 kinds of organochlorine pesticides in n-hexane with a concentration of 1.0 mg / L, add 10 mL of n-hexane solvent to immerse the soil, stir under a fume hood to mix evenly, Then...

Embodiment 2

[0038] The application has also tested the chromatographic condition optimization and internal standard selection of above-mentioned detection method, and test result is as follows.

[0039] 2.1 Optimization of chromatographic conditions

[0040] The purpose of optimizing the chromatographic conditions is to make the separation and detection time the shortest and the effect the best, and at the same time make the detection sensitivity of the chromatogram reach the highest. According to the principle of similar miscibility, since organochlorine pesticides are weakly polar substances, HP-5 capillary column was selected. The gas chromatogram of the standard mixed solution of 8 kinds of organochlorine pesticides is as follows: figure 2 As shown, the experimental results show that under the chromatographic conditions, the target compound and the internal standard can be separated well, which can meet the experimental requirements.

[0041] 2.2 Internal standard selection

[004...

Embodiment 3

[0044] The present application has also tested the above-mentioned detection method. By investigating the type of dispersant, eluent and elution volume, the ratio of sample to dispersant, the recovery rate and standard deviation of organochlorine pesticides under different conditions are measured. The test results are as follows.

[0045] 3.1 Drawing of standard curve

[0046] Using n-hexane as a solvent, accurately pipette the stock solutions of 8 kinds of mixed organochlorine pesticides, prepare standard solutions with concentrations of 50, 100, 150, 200, and 250 μg / L, and add 80 ppb of 13 C 12 -PCB-153 is used as an internal standard, with the concentration ratio as the abscissa and the peak area as the ordinate to draw a standard curve. The calculated standard curve equation and correlation coefficient are shown in Table 1. As can be seen from the data in Table 1, at 50 The linear correlations of the eight organochlorine pesticides within the mass concentration range of ~...

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Abstract

The invention discloses a matrix solid-phase dispersion extraction-gas chromatography method for analyzing a soil organochlorine pesticide, and relates to the field of soil monitoring and detection. The key points of the technical scheme are that a gas chromatography is used and a matrix solid-phase dispersion extraction method is mainly utilized, and through optimizing chromatographic conditions,the method aims to achieve the purposes of shortest separation and detection time, best effect and highest detection sensitivity of chromatography by mainly utilizing a matrix solid-phase dispersionextraction method and optimizing chromatographic conditions. The method is applied to the test of an actual sample, is high in accuracy and sensitivity and good in reproducibility, and can meet the detection requirements on organochlorine pesticide residues.

Description

technical field [0001] The invention belongs to the field of analysis and detection, and in particular relates to a method for detecting soil organochlorine pesticides. Background technique [0002] Organochlorine pesticides are organic compounds containing organochlorine elements used to prevent and control plant diseases and insect pests. Typical organochlorine pesticides such as DDT and HCH have efficient insecticidal, weeding and sterilizing effects. However, since these two pesticides are not easy to decompose and transform like other organic pollutants, they remain in the environment for a long time and can enter the human body through the food chain, causing harm to human health. It has the characteristics of long half-life, difficult to decompose and lipophilicity. Although my country banned the use of such pesticides in 1983, they are still detected in environmental media such as sediment and soil. [0003] For the detection of HCH, DDT and other organochlorine pe...

Claims

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Application Information

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IPC IPC(8): G01N30/88G01N30/06
CPCG01N30/88G01N30/06G01N2030/884G01N2030/062
Inventor 余彬彬金燕仙严朝朝章心怡魏文婉陈啸陈昊伍佳慧张嫣秋
Owner TAIZHOU UNIV
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