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 can be applied in the field of agricultural technology, the food field, and can solve the problems of interfering detection results, inability to accurately quantify, and lack of specificity.

Inactive Publication Date: 2014-09-24
JIANGXI AGRICULTURAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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 the 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 is 4:1) were dissolved in 16 mL of dichloromethane, and ultrasonically mixed and degassed for 5 minutes, thus obtaining a Dichloromethane prepolymerization system; then, add 750μL trimethylolpropane trimethacrylate (TRIM) crosslinking agent, 0.1g azobisisobutyronitrile initiator to the prepolymerization system, the α - The molar ratio of methacrylic acid functional monomer, cross-linking agent and initiator is 4:4:1; followed by ultrasonic mixing and degassing for 5 minutes, and finally filling with nitrogen for 5 minutes, sealing immediately, and tightening the lid tightly, at a temperat...

Embodiment 2

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

[0138] The pyrazosulfuron-methyl polymer prepared in Example 1 was used to prepare a solid-phase extraction column in the same manner as in Example 1.

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

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

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

[0142] Before using the MISPE column, use 7.5mL (2.5×3mL) eluent (a mixture of methanol and acet...

Embodiment 3

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

[0148] The pyrazosulfuron-methyl polymer prepared in Example 1 was used to prepare a solid-phase extraction column in the same manner as in Example 1.

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

[0150] Take 20mL of water from Nongda’s rice field and filter it with double-layer filter paper, then filter the obtained filtrate with a 0.45μm filter membrane, blow dry the obtained filtrate with nitrogen, then add 3mL of n-hexane, ultrasonically mix it, and set aside;

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

[0152] Before using the MISPE column, use 7.5mL (2.5×3mL) eluent (a mixture of methanol and acetic acid, the volume ratio is 9:1) to wash off the impurities of the column, and then use 5mL (2.5×2mL) activator (acetonitrile and dichloromethane mixture, the volume ratio of 1:1) for activation. Take 1mL of the above-mentioned ready-to-use soluti...

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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 Patents(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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