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Method for detecting triazine herbicide residues in agricultural products through molecular imprinting and dispersive solid-phase extraction

A technology of molecular imprinting and dispersing solid phase, applied in chemical instruments and methods, material separation, analysis of materials, etc., can solve problems such as low purification efficiency, reduce matrix effects, improve accuracy and precision, and overcome the difficulty in controlling flow rate. Effect

Active Publication Date: 2018-10-09
KUNMING UNIV OF SCI & TECH
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The problem to be solved by the present invention is to provide a molecular imprinting-dispersive solid-phase extraction method for detecting triazine herbicide residues in agricultural products for the defects of traditional molecularly imprinted polymers, such as complex preparation process, uneven particles, and long adsorption time. The method can simply and quickly prepare molecularly imprinted nanospheres with small particle size and high uniformity, and the prepared molecularly imprinted nanospheres have good selective adsorption capacity and high imprinting factor for template molecules and their structural analogues; This kind of molecularly imprinted nanospheres is used as an adsorbent to develop a pretreatment method for dispersed solid phase extraction, which effectively overcomes the defects of difficult control of the flow rate and low purification efficiency of traditional solid phase extraction, and can achieve a variety of triazines in agricultural products. Herbicide Trace Residue Analysis

Method used

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  • Method for detecting triazine herbicide residues in agricultural products through molecular imprinting and dispersive solid-phase extraction
  • Method for detecting triazine herbicide residues in agricultural products through molecular imprinting and dispersive solid-phase extraction
  • Method for detecting triazine herbicide residues in agricultural products through molecular imprinting and dispersive solid-phase extraction

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Effect test

Embodiment 1

[0027] Example 1: This molecular imprinting-dispersive solid-phase extraction method for detecting triazine herbicide residues in agricultural products, the specific content is as follows:

[0028] Add 50.66mg of siclofen, 0.081mL of methacrylic acid, and 40mL of acetonitrile into a 100mL borosilicate glass bottle, sonicate for 3 minutes, put it in a refrigerator at 4°C, and let it stand for 12 hours to seal and self-assemble to obtain a template-monomer complex; Add 30mg of azobisisobutyronitrile, 0.597mL of ethylene glycol dimethacrylate, pass into high-purity N 2 15min, then heat-initiated precipitation polymerization in a 60°C water bath at a speed of 60rpm for 48h; after the reaction, centrifuge at 10,000rpm to obtain polymer particles, and then use a Soxhlet extraction device to mix methanol-acetic acid (9:1, v / v) Wash the template molecules in the polymer particles with the eluent, replace the eluent every 8 hours, and elute for 16 hours until the template molecules c...

Embodiment 2

[0035] Embodiment 2: The method of this molecular imprinting-dispersed solid phase extraction to detect triazine herbicide residues in agricultural products, the specific contents are as follows:

[0036] (1) Add 63.33 mg of xicaojing, 0.127 mL of acrylic acid, and 50 mL of methanol into a 100 mL borosilicate glass bottle, ultrasonicate for 3 min, put it in a -5°C refrigerator, and let stand for 12 h to seal and self-assemble to obtain a template-monomer complex; 35 mg of azobisisobutyronitrile, 0.746 mL of trimethylolpropane trimethacrylate were added to it, and high-purity N was added. 2 15min, then thermally induced precipitation polymerization at 50°C water bath and rotating speed of 100rpm for 20h; after the reaction, centrifuged at 10000rpm to obtain polymer particles, and then used a Soxhlet extraction device to extract methanol-acetic acid mixed solution (20:1, v / v) Wash the template molecules in the polymer particles with the eluent, replace the eluent every 8 hours...

Embodiment 3

[0041] Embodiment 3: The method of this molecular imprinting-dispersed solid phase extraction to detect triazine herbicide residues in agricultural products, the specific contents are as follows:

[0042] Add 53.92 mg atrazine, 0.101 mL trifluoromethacrylic acid, 50 mL dichloromethane to a 100 mL borosilicate glass bottle, ultrasonicate for 5 min, put it in a 10°C refrigerator for 12 hours, seal and self-assemble to obtain a template-monomer complex ; Add 30mg azobisisobutyronitrile, 0.746mL ethylene glycol dimethacrylate to it, feed high-purity N 2 15min, then thermally induced precipitation polymerization reaction at 70°C water bath and rotating speed of 120rpm for 15h, after the reaction, centrifuged at 12000pm to obtain polymer particles; ) is the eluent to wash the polymer particles; the eluent is replaced every 8 hours, and atrazine cannot be detected from the supernatant by HPLC after elution; after elution, the polymer is washed with methanol and acetone in turn The ...

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Abstract

The invention discloses a method for detecting triazine herbicide residues in agricultural products through molecular imprinting and dispersive solid-phase extraction. The method comprises the following steps: taking triazine compounds as template molecules, adding the template molecules, a functional monomer, a cross-linking agent and an initiator into a pore-foaming agent, and preparing molecularly-imprinted nano-microspheres through a precipitation copolymerization method; activating the molecularly-imprinted nano-microspheres, then taking the activated molecularly-imprinted nano-microspheres as adsorption materials of dispersive solid-phase extraction, and detecting various triazine herbicides in complex agricultural product substrates with combination of the molecularly-imprinted nano-microspheres and UPLC-MS / MS. The molecularly-imprinted nano-microspheres prepared by the method have high selective adsorption on the template molecules and structural analogs of the template molecules; meanwhile, the particle diameter distribution is uniform; the detection reproducibility is improved; the defects that the flow rate is difficultly controlled and the reproducibility is low in theconventional solid-phase extraction column are overcome; the detection requirements of trace triazine pesticide residues in various substrates can be met.

Description

technical field [0001] The invention relates to the field of synthesis and separation engineering of functional polymer materials, in particular to a method for detecting triazine herbicide residues in agricultural products by molecular imprinting-dispersion solid-phase extraction. Background technique [0002] The adsorbent used in the sample pretreatment process is required to be able to selectively adsorb the target analyte, similar to the recognition of natural antibodies to receptors and enzymes to substrates. Proteins are highly denatured in extreme temperature, pH, and organic solvents, so the biorecognition process is very demanding on the environment. In order to overcome the above limitations, artificially synthesized receptor molecular imprinting technology has received extensive attention in recent years. Molecularly imprinted polymers synthesized by molecularly imprinted technology are complementary to templates in three-dimensional space and adsorption sites, ...

Claims

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Application Information

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IPC IPC(8): C08J9/28C08F222/14C08F220/06B01J13/14B01J20/26B01J20/28B01J20/30G01N30/02G01N30/06C08L35/02
CPCB01J13/14G01N30/02G01N30/06C08F222/10C08J9/28B01J20/268B01J20/28021C08J2335/02G01N2030/062C08F222/103C08F222/102C08F220/06
Inventor 顾丽莉韩毅李志君彭健陶军孔光辉师君丽
Owner KUNMING UNIV OF SCI & TECH
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