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Method for using pyrazosulfuron-ethyl molecularly imprinted polymer for analyzing sulfonylurea herbicide and application thereof

A technology using pyrazosulfuron-methyl molecules and pyrazosulfuron-methyl molecules, which is applied in the field of analysis and detection, can solve the problems of interference detection results, inaccurate quantification, lack of specificity, etc.

Inactive Publication Date: 2013-01-09
JIANGXI AGRICULTURAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the literature reports that the detection of pyrazosulfuron-methyl sulfonylurea herbicides is mainly based on the detection of instruments such as HPLC, LC-MS or CE, and its pretreatment requires multiple liquid-liquid distributions or solid-phase extraction column enrichment, Purification, while the currently used C18 solid-phase extraction filler lacks specificity, will introduce many impurities, interfere with the test results, and cannot be accurately quantified

Method used

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  • Method for using pyrazosulfuron-ethyl molecularly imprinted polymer for analyzing sulfonylurea herbicide and application thereof
  • Method for using pyrazosulfuron-ethyl molecularly imprinted polymer for analyzing sulfonylurea herbicide and application thereof
  • Method for using pyrazosulfuron-ethyl molecularly imprinted polymer for analyzing sulfonylurea herbicide and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0107] Example 1: Analysis of sulfonylurea herbicides in rice

[0108] The implementation steps of this embodiment are as follows:

[0109] First, prepare pyrazosulfuron-methyl molecularly imprinted polymer:

[0110] (i) Polymerization step:

[0111] In a polymerization reaction bottle, 170 μL of α-methacrylic acid functional monomer and 0.2 g of pyrazosulfuron-methyl (their molar ratio 4:1) were dissolved in 16 mL of dichloromethane, and ultrasonically mixed and degassed for 5 min, thus obtaining a Dichloromethane prepolymerization system; then, add 750 μL trimethylolpropane trimethacrylate (TRIM) crosslinking agent, 0.1 g azobisisobutyronitrile initiator to the prepolymerizing system, the α -The molar ratio of methacrylic acid functional monomer, crosslinking agent and initiator is 4:4:1; then ultrasonically mixed and degassed for 5 minutes, and finally filled with nitrogen for 5 minutes. The reaction was heated in a water bath for 24h to obtain a high molecular weight po...

Embodiment 2

[0137] Example 2: Analysis of sulfonylurea herbicides in soil

[0138] Using the pyrazosulfuron-methyl polymer prepared in Example 1, a solid phase extraction column was prepared in the same manner as in Example 1.

[0139] Second, the preparation of the soil test solution

[0140] Take the soil sample from the experimental field of Agricultural University, dry it, crush it, and pass it through a 50-mesh standard mesh sieve. Weigh 5g of the sieved soil powder, put it into a 50mL centrifuge tube, add 10mL of distilled water, stir gently with a glass rod, and let it stand for infiltration for 2h. , then add 10 mL of acetonitrile, stir with a glass rod, let it stand for 1 hour, mix with a vortex mixer for 15 minutes, then centrifuge for 15 minutes at a speed of 4000 r / min, filter with double-layer filter paper, and analyze the obtained filtrate;

[0141] Third, the analysis of the soil test solution

[0142] Before use, the MISPE column was washed with 7.5mL (2.5×3mL) of eluen...

Embodiment 3

[0147] Example 3: Analysis of sulfonylurea herbicides in paddy field water

[0148] Using the pyrazosulfuron-methyl polymer prepared in Example 1, a solid phase extraction column was prepared in the same manner as in Example 1.

[0149] Second, the preparation of the paddy field water test solution

[0150] Take 20 mL of water from the rice field of Agricultural University and filter it with double-layer filter paper, and then filter the obtained filtrate with a 0.45 μm filter membrane. The obtained filtrate is blown dry with nitrogen, and then 3 mL of n-hexane is added, ultrasonically mixed, and set aside for use;

[0151] Third, the analysis of water test solution in paddy field

[0152] Before use, the MISPE column was washed with 7.5mL (2.5×3mL) of eluent (mixture of methanol and acetic acid, the volume ratio of which was 9:1) to remove impurities from the column, and then 5mL (2.5×2mL) of activator (acetonitrile) was used. The mixture with dichloromethane, its volume ra...

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Abstract

The invention relates to a method for using pyrazosulfuron-ethyl molecularly imprinted polymer for analyzing sulfonylurea herbicide. The method includes the steps of molecularly imprinted solid-phase extraction (MISPE) column preparation, herbicide standard material stock solution preparation, herbicide high performance liquid chromatography (HPLC) standard curve drawing, sample purification solution preparation, HPLC analysis of a sample to be analyzed and the like. A sulfonylurea derby solid-phase extraction column used by the method can specially adsorb various analogues of sulfonylurea derby and the like. The method has remarkable selectivity, flow velocity is increased by 50%, analysis time is reduced by 50%, template compound residual amount is almost zero, and false positive caused by residual template compound is avoided. The solid-phase extraction column is remarkable in purification effect, simplifies enrichment and purification of the sample, improves pre-processing efficiency, and can be reused. A detection method combining a molecularly imprinted solid-phase extraction column and an HPLC instrument can be built, and finally a standard detection method of biological samples of agricultural products, water, soil and the like can be built.

Description

【Technical field】 [0001] The invention belongs to analysis and detection technology. More specifically, the present invention relates to a method for analyzing sulfonylurea herbicides using pyrazosulfuron-methyl molecularly imprinted polymers, and also relates to the application of the method in technical fields such as food and agriculture. 【Background technique】 [0002] Sulfonylurea herbicides are currently the most widely used herbicides in the world. The sulfonylurea herbicides widely used in my country include chlorsulfuron-methyl, metsulfuron-methyl, bensulfuron-methyl, ethametsulfuron-methyl, Pyrazosulfuron-methyl, Ethersulfuron-methyl, etc. The application of herbicides saves labor to the greatest extent, improves agricultural production efficiency, improves the degree of agricultural modernization, and greatly reduces the intensity and cost of manual weeding. With the widespread use of such herbicides in agricultural production, their residues and harm to subseque...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
Inventor 汤凯洁罗秋水吴国平熊建华余瑞龙
Owner JIANGXI AGRICULTURAL UNIVERSITY
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