Method for analyzing and detecting four kinds of heterocyclic pesticides in environmental water sample

A detection method and a heterocyclic technology, applied in the field of pesticide detection, can solve the problems of high cost of use and maintenance of gas chromatography-mass spectrometry, low service life of extraction fibers, and easy blockage of columns, and save analysis time and cost. , easy operation, mild reaction conditions

Inactive Publication Date: 2017-08-18
QINGDAO TECHNOLOGICAL UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, the commonly used sample pretreatment technology, solid phase extraction, has defects such as long extraction time, easy blockage of extraction column, and the need for special equipment; solid phase microextraction has the problem of low service life of extraction fibers; dispersion liquid microextraction Extraction operations require the use of expensive centrifuges
Martins et al. disclose a method for the simultaneous determination of multiple pesticide residues in surface water and industrial wastewater by solid-phase extraction and gas chromatography-tandem mass spectrometry, which can accurately determine multiple pesticide residues in water samples, but the pretreatment process of this method The use of solid-phase column extraction takes a long time, the column is easy to clog and has a limited service life, and the gas chromatography-mass spectrometry used is expensive to use and maintain, making it difficult to apply on a large scale
At present, there is no report on the use of magnetic metal-organic framework material MOF-5 for the enrichment analysis of heterocyclic pesticides

Method used

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  • Method for analyzing and detecting four kinds of heterocyclic pesticides in environmental water sample
  • Method for analyzing and detecting four kinds of heterocyclic pesticides in environmental water sample
  • Method for analyzing and detecting four kinds of heterocyclic pesticides in environmental water sample

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] The analysis and detection method of four kinds of heterocyclic pesticides in the environmental water samples involved in the embodiment specifically includes the following steps:

[0062] Step 1: Preparation of magnetic metal organic framework material MOF-5:

[0063] (1) Dissolve 1.0 g of ferric chloride hexahydrate in 20 mL of ethylene glycol, then add 3 g of sodium acetate and 10 mL of ethanolamine, and stir to dissolve;

[0064] (2) The mixture prepared in step (1) was reacted for 8h at 200°C in the solvothermal reaction kettle, and the obtained mixture in the solvothermal reaction kettle was washed with ultrapure water to obtain ferric iron tetraoxide ( NH 2 -Fe 3 o 4 ), the prepared NH 2 -Fe 3 o 4 Vacuum dry at 60°C for 12 hours;

[0065] (3) Dissolve 0.5065g terephthalic acid in 40mL N,N dimethylamide (DMF), 2.302g hexahydrate and zinc nitrate (Zn(NO 3 ) 2 ·6H 2 O) be dissolved in 50mL DMF, and it is slowly added dropwise in the DMF solution that is di...

Embodiment 2

[0075] This embodiment investigates the main factors affecting the extraction recovery of four heterocyclic pesticides, calculates the optimum value of each factor when the extraction recovery is the highest, and then determines the four heterocyclic pesticides under the condition of the optimum value of each factor. The parameters related to the working curve of the pesticide and the detection limit and precision of the method, the specific process includes the following steps:

[0076] Step 1: Calculate the optimal value of each factor when the extraction recovery of the four heterocyclic pesticides is the highest:

[0077] (1) The investigation of the amount of adsorbent to the extraction recovery

[0078] In this example, the effect of the amount of adsorbent on the extraction recovery rate was investigated, and 4, 6, 7, 8, and 10 mg of magnetic metal-organic framework material MOF-5 were weighed in 20 mL of simulated water samples, and the four heterocyclic pesticides in ...

Embodiment 3

[0099] Determination of residues of four heterocyclic pesticides in Nuocheng Reservoir of Qingdao City, Qianhan Reservoir of Qingdao City, and the Yellow River. After collecting three kinds of water samples, filter them with rapid qualitative filter paper with a pore size of 80-120 μm, and then use a 0.45 μm filter membrane Filtration; the filtered water sample is measured by the method described in Example 1, and the accuracy test is carried out by the method described in Example 2, and the concentrations of four kinds of heterocyclic pesticides are respectively prepared as 5 μg / L, 50 μg / L, and 100 μg The actual water samples with low, medium and high concentrations of / L were tested for the standard recovery rate, and each concentration point was measured 3 times, and the average value, relative standard deviation and standard recovery rate of the three determinations were calculated; among them, the three None of the four heterocyclic pesticides were detected in the water sa...

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Abstract

The invention belongs to the field of pesticide detection, and relates to a method for analyzing and detecting four kinds of heterocyclic pesticides in an environmental water sample. The four kinds of heterocyclic pesticides comprise carbendazim, triazolone, chlorfenapyr and fenpyroximate. The method for analyzing and detecting the four kinds of heterocyclic pesticides in the environmental water sample comprises the following steps: preparing amino ferroferric oxide by taking ferric trichloride hexahydrate as a raw material with the assistance of ethylene glycol, sodium acetate and ethanol amine; preparing a magnetic metal organic framework MOF-5 from the prepared amino ferroferric oxide; measuring the four kinds of heterocyclic pesticides by taking the prepared magnetic MOF-5 as a magnetic solid-phase extraction material and taking an efficient liquid chromatography as a measuring instrument. The method has the advantages of easiness and convenience in operation, adoption of readily-available raw materials, high accuracy of measuring result, average recycling rate of 80.30 to 108.33 percent, relative standard deviation of 2.96 to 7.94 percent, good extraction effect, accurate analysis result, high reproducibility and wide market prospect.

Description

[0001] Technical field: [0002] The invention belongs to the field of pesticide detection, and relates to a method for analyzing and measuring four kinds of heterocyclic pesticides in water samples, using magnetic solid phase extraction (MSPE) technology, using magnetic metal organic framework material MOF-5 solid phase extraction-high performance liquid phase Chromatography was used to determine four heterocyclic pesticides including carbendazim, triadimefon, chlorfenapyr and pyraflux in environmental water samples. [0003] Background technique: [0004] Farmland weeds, pests and diseases have caused great losses to agricultural production, and the application of pesticides has greatly reduced the intensity and cost of manual weeding and prevention of pests and diseases, and improved the modernization level of agriculture. However, the pollution of water resources caused by the use of pesticides is one of the main challenges affecting the sustainable development of the envir...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/74
Inventor 马继平吴阁格李爽
Owner QINGDAO TECHNOLOGICAL UNIVERSITY
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