Method for purifying and detecting pirimicarb by utilizing molecularly imprinted polymer (MIP)

A technology of molecular imprinting and anti-pirimicarb, applied in the field of biochemistry, can solve the problems of no practical application, stay in the evaluation stage of polymer physical characteristics and adsorption performance, etc., and achieve the effect of improving sensitivity, good specificity and high capacity

Inactive Publication Date: 2012-07-04
SHANGHAI JIAO TONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this article only stays at the evaluation stage of polymer physical characteristics and adsorption performance, and has no practical application.
So far, there is no report on the application of pirimicarb molecularly imprinted polymer solid-phase extraction columns to fruit and vegetable samples prepared by surface polymerization.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] 1. Preparation of pirimicarb molecularly imprinted polymers

[0025] Mix pirimicarb (template molecule) 0.2mmol, functional monomer trifluoromethacrylic acid (TFMAA) and cross-linking agent ethylene glycol dimethacrylate (EDMA) according to the molar ratio of 1:4:20, Dissolve in 20mL pore-forming agent (heptane), place in an ampoule, and pre-polymerize for 2 hours. Add 0.08mmol of initiator 4,4'-azo-bis(4-cyanovaleric acid)-silica gel (ACPA-silica gel), fill with nitrogen for 5 minutes, seal in vacuum, and thermally polymerize in an oil bath at 65°C for 24 hours. The template molecules were removed by Soxhlet extraction for 12 hours, and the composition of the extractant was methanol-water-acetic acid mixture (7:2:1, V / V / V). 20 μl of the eluate was taken, and after the elution was detected by HPLC, the polymer was dried at 60° C. for 24 hours.

[0026] 2. Preparation of pirimicarb molecularly imprinted polymer solid phase extraction cartridges

[0027] First wash the...

Embodiment 2

[0033] 1. Preparation of pirimicarb molecularly imprinted polymers

[0034]Mix pirimicarb (template molecule) 0.2mmol, functional monomer trifluoromethacrylic acid (TFMAA) and cross-linking agent ethylene glycol dimethacrylate (EDMA) according to the molar ratio of 1:4:20, Dissolve in 20mL pore-forming agent (heptane), place in an ampoule, and pre-polymerize for 2 hours. Add 0.08mmol of initiator 4,4'-azo-bis(4-cyanovaleric acid)-silica gel (ACPA-silica gel), fill with nitrogen for 5 minutes, seal in vacuum, and thermally polymerize in an oil bath at 70°C for 20 hours. The template molecules were removed by Soxhlet extraction for 12 hours, and the composition of the extractant was methanol-water-acetic acid mixture (7:2:1, V / V / V). 20 μl of the eluate was taken, and after the elution was detected by HPLC, the polymer was dried at 60° C. for 24 hours.

[0035] 2. Preparation of pirimicarb molecularly imprinted polymer solid phase extraction cartridges

[0036] First wash the ...

Embodiment 3

[0042] 1. Preparation of pirimicarb molecularly imprinted polymers

[0043] Mix pirimicarb (template molecule) 0.2mmol, functional monomer trifluoromethacrylic acid (TFMAA) and cross-linking agent ethylene glycol dimethacrylate (EDMA) according to the molar ratio of 1:4:20, Dissolve in 20mL pore-forming agent (heptane), place in an ampoule, and pre-polymerize for 2 hours. Add 0.08 mmol of initiator 4,4'-azo-bis(4-cyanovaleric acid)-silica gel (ACPA-silica gel), fill with nitrogen gas for 5 minutes, seal in vacuum, and thermally polymerize in an oil bath at 70°C for 30 hours. The template molecules were removed by Soxhlet extraction for 12 hours, and the composition of the extractant was methanol-water-acetic acid mixture (7:2:1, V / V / V). 20 μl of the eluate was taken, and after the elution was detected by HPLC, the polymer was dried at 60° C. for 24 hours.

[0044] 2. Preparation of pirimicarb molecularly imprinted polymer solid phase extraction cartridges

[0045] First was...

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PUM

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Abstract

The invention provides a method for purifying and detecting pirimicarb by utilizing a molecularly imprinted polymer (MIP), belonging to the biochemical technical field. The method comprises the following steps: mixing and dissolving pirimicarb template molecules, a functional monomer of trifluoromethyl acrylic acid and a cross-linking agent of ethylene glycol dimethacrylate in heptane, and addingan initiator of 4,4'-azo-2(4-cyanovaleric acid)-silica gel to the obtained mixed solution; filling up nitrogen for 5-10 minutes, sealing an ampoule under protection of the nitrogen, carrying out water bath and heat preservation at 65-70 DEG C for reacting for 20-30 hours, and then removing the template molecules through soxhlet extraction; drying the polymer without the template molecules at 60 DEG C for staying overnight to obtain the MIP of the pirimicarb; filling the MIP of the pirimicarb into a solid-phase extraction column tube; and activating a solid-phase extraction column, adding sample fruit and vegetable extracting solution, washing the solid-phase extraction column, eluting, purifying and finally collecting the pirimicarb. The method of the invention can make up the pretreatment disadvantage for detecting the pirimicarb in the existing fruit and vegetable environment, simply, rapidly, specifically and efficiently enrich and purify a trace amount of the pirimicarb, and improve the existing detection sensitivity.

Description

technical field [0001] The invention relates to a method in the field of biochemical technology, in particular to a method for purifying and detecting pirimicarb by using a molecularly imprinted polymer. Background technique [0002] Pirimicarb is a carbamate insecticide, its English name is primicarb, and its chemical name is 5,6-dimethyl-2-dimethylamino-4-pyrimidinyl-dimethylaminomethyl esters. The drug can control all aphids except cotton aphids that are resistant to organophosphorus insecticides, and is often used for the control of aphids in fruits and vegetables. Due to the over-limit and over-range use of pirimicarb, the resulting pressure on the environment and food safety has become increasingly prominent. The toxic action mechanism of carbamate pesticides is similar to that of organophosphorus pesticides. It mainly inhibits the activity of cholinesterase, causing the hydroxyl group of serine in the active center of the enzyme to be carbamylated, thus losing the a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D239/47G01N30/08
Inventor 孙向军唐波陈秋宇
Owner SHANGHAI JIAO TONG UNIV
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