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Preparation method of solid-phase extraction small column for molecular imprinting of substituted carbamide pesticide

A solid-phase extraction column and molecular imprinting technology, applied in chemical instruments and methods, and other chemical processes, can solve problems such as incomplete purification, inability to separate and retain, and inability to enrich the components to be tested, and achieve high efficiency. Effect

Inactive Publication Date: 2009-08-05
ANHUI AGRICULTURAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These column packings adsorb the target pesticides, so that the interfering co-extracted substances are washed and removed to achieve the purpose of purification and enrichment; The components to be tested cannot be enriched, and impurities whose retention properties are weaker than those of the components to be tested cannot be separated, resulting in incomplete purification

Method used

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  • Preparation method of solid-phase extraction small column for molecular imprinting of substituted carbamide pesticide

Examples

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Effect test

Embodiment 1

[0030] (1) Preparation of molecularly imprinted polymer microspheres of substituted urea pesticides

[0031] (1). The molar ratio of template molecule, functional monomer and crosslinking agent is 1:2; the volume ratio of the total volume of diluent and crosslinking agent to water is 1:10; the concentration of polyvinyl alcohol 400 (PVA400) 4%; 8mmoL functional monomer methacrylic acid and 1mmol template molecular substituted urea pesticides were dissolved in the diluent, and ultrasonically acted for 5min; 40mmoL crosslinking agent ethylene glycol dimethacrylate (EGDMA), 120mg initiator (AIBN) and 15mL diluent were mixed, sonicated for 5-10min; the above three solutions were mixed, degassed by sonication for 5min; stirred at a constant temperature of 350rpm at 60°C for 20h;

[0032] (2). Stir the molecularly imprinted polymer microspheres prepared by the above reaction in 80°C water for 60 minutes, then cool down and filter, wash with double distilled water 3 times after filtr...

Embodiment 2

[0045] (1) Preparation of molecularly imprinted polymer microspheres of substituted urea pesticides

[0046](1). The molar ratio of template molecule, functional monomer and crosslinking agent is 1: 4; the volume ratio of the total volume of diluent and crosslinking agent to water is 1: 8; the concentration of polyvinyl alcohol 400 is 4 %; 8mmol functional monomer methacrylic acid and 1mmol template molecule substituted urea pesticides were dissolved in the diluent, and ultrasonicated for 5-10min; 5mL cross-linking agent ethylene glycol dimethacrylate (EGDMA), 120mg initiator (AIBN) and 15mL of diluent were mixed, sonicated for 5-10min; the above three solutions were mixed, and stirred at a constant temperature of 400rpm at 60°C for 22h;

[0047] (2). Stir the molecularly imprinted polymer microspheres prepared by the above reaction in 80°C water for 60 minutes, then cool down and filter, wash with double distilled water 3 times after filtration, wash 3 times with 20mL methano...

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Abstract

The invention discloses a method for preparing a molecularly imprinted solid-phase extraction column of substituted urea pesticide, which belongs to the technical field of food safety. The method comprises the following steps: preparing a template molecule substituted urea pesticide, a functional monomer methacrylic acid and a cross-linking agent ethylene dimethacrylate into a molecularly imprinted polymer microsphere of the substituted area pesticide through suspension polymerization according to a mol ratio of the template molecule to the functional monomer to the cross-linking agent of 1:2-8:20; and weighing the molecularly imprinted polymer microsphere of the substituted urea pesticide to be filled in an empty pipe of polypropylene solid-phase extraction column to prepare the molecularly imprinted solid-phase extraction column of the substituted urea pesticide. The molecularly imprinted solid-phase extraction column of the substituted urea pesticide can be used for selective purification and selective enrichment of an extracted solution of a residual sample of the substituted urea pesticide in inspected food and environment. Compared with common liquid-liquid extraction method and C18 solid-phase extraction method, the method has the characteristics of easiness, rapidness, high purification efficiency and the like.

Description

technical field [0001] The present invention relates to a method in the technical field of food safety, specifically, to a molecularly imprinted solid phase of substituted urea pesticides for highly selective separation, purification and enrichment of substituted urea pesticide residues in food and environmental samples Preparation of extraction cartridges. Background technique [0002] Substituted urea pesticides are a class of pesticides derived from urea as the core structure. The general chemical structure is as follows: [0003] [0004] It replaces urea pesticides with moderate toxicity and low water solubility. It is mostly used as a soil treatment agent for controlling annual gramineous weeds such as barnyardgrass and annual dicotyledonous weeds such as amaranth in various dryland crops such as cereals. [0005] For the residues of substituted urea pesticides, there are many detection methods. At present, developed countries have stricter and stricter detection l...

Claims

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Application Information

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IPC IPC(8): B01J20/285
Inventor 汤锋岳永德花日茂操海群唐俊
Owner ANHUI AGRICULTURAL UNIVERSITY
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