Surface-modified molecular-imprinted solid-phase microextraction probe and preparation and application thereof

A molecular imprinting and surface modification technology, applied in the field of extraction probes, can solve the problems of difficult separation, tedious and time-consuming, etc., and achieve the effects of rapid analysis, good adsorption performance, strong selectivity and enrichment ability

Active Publication Date: 2017-10-03
FOSHAN UNIVERSITY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method is cumbersome and time-consuming, requires a large volume of samples for the enrichment of trace targets, and requires multi-step pre-treatment methods to eli

Method used

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  • Surface-modified molecular-imprinted solid-phase microextraction probe and preparation and application thereof
  • Surface-modified molecular-imprinted solid-phase microextraction probe and preparation and application thereof
  • Surface-modified molecular-imprinted solid-phase microextraction probe and preparation and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0043] Example 1 Preparation of solid-phase microextraction probes

[0044] 1. Take 24mL deionized water, add 0.1g methacrylic acid, 0.05g acrylic acid, 0.2g styrene, 0.2g hydroxypropyl acrylate, 1.5g butyl acrylate, 1.5g acrylic acid-2-ethylhexyl functional monomer With 0.05g of octylphenol polyoxyethylene ether and 0.05g of sodium lauryl sulfate emulsifier, and stirred in an emulsifier (20000rpm / min) for 15min to prepare a pre-emulsion for later use.

[0045] 2. Add 13 mL of deionized water, 0.1 g of sodium bicarbonate, and about 7.5 g of pre-emulsion to a four-necked flask equipped with a thermometer, reflux condenser, and agitator, heat up to 80°C under stirring at 250 rpm / min, and then add half 5 mL of 0.11 mol / L potassium persulfate initiator, reacted for 1 h to obtain a blue-blue seed emulsion.

[0046] 3. Reduce the stirring speed, add the remaining pre-emulsion and potassium persulfate solvent dropwise to the seed emulsion within 4h to obtain an acrylate emulsion, an...

Example Embodiment

[0050] Example 2

[0051] 1. Take 24mL deionized water, add 0.3g methacrylic acid, 0.15g acrylic acid, 0.6g styrene, 0.6g hydroxypropyl acrylate, 4.5g butyl acrylate, 4.5g acrylic acid-2-ethylhexyl functional monomer and 0.15g of sodium lauryl sulfate and sec-octylphenol polyoxyethylene ether emulsifier, and stirred in an emulsifier (10000rpm / min) for 15min to prepare a pre-emulsion for later use.

[0052] 2. Add 13 mL of deionized water, 0.1 g of sodium bicarbonate, and about 7.5 g of pre-emulsion to a four-necked flask equipped with a thermometer, reflux condenser, and agitator, heat up to 110 ° C under stirring at 250 rpm / min, and add half 5mL of 0.11mol / L azobisisobutyronitrile initiator, reacted for 3h to obtain blue-blue seed emulsion.

[0053] 3. Reduce the stirring speed, add the remaining pre-emulsion and potassium persulfate solvent dropwise to the seed emulsion within 4h to obtain an acrylate emulsion, and continue to add vinyl tris (β-methoxyethoxy) silane dropwis...

Example Embodiment

[0057] Example 3

[0058] 1. Take 24mL deionized water, add 0.51g methacrylic acid, 0.26g acrylic acid, 1g styrene, 1g hydroxypropyl acrylate, 7.7g butyl acrylate, 7.7g acrylate-2-ethylhexyl acrylate functional monomer and 0.26 g g octylphenol polyoxyethylene ether, 0.26 g of sodium lauryl sulfate emulsifier, and stirred in an emulsifying machine (30000 rpm / min) for 15 min to prepare a pre-emulsion for later use.

[0059] 2. Add 13 mL of deionized water, 0.1 g of sodium bicarbonate, and about 7.5 g of pre-emulsion to a four-necked flask equipped with a thermometer, a reflux condenser, and a stirrer, heat up to 70°C under stirring at 250 rpm / min, and then add half 5 mL of 0.11 mol / L benzoyl peroxide initiator, reacted for 5 h to obtain a blue-blue seed emulsion.

[0060] 3. Reduce the stirring speed, add the remaining pre-emulsion and potassium persulfate solvent dropwise to the seed emulsion within 4h to obtain an acrylate emulsion, and continue to add vinyl tris (β-methoxyet...

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Abstract

The invention discloses a surface-modified molecular-imprinted solid-phase microextraction probe and a preparation method therefor. The surface-modified molecular-imprinted solid-phase microextraction probe disclosed by the invention is obtained through taking malachite green as template molecules, and subjecting an organosilicone modified acrylate molecular imprinting emulsion to a thermal polymerization reaction on a tipped wood fiber substrate, of which the surface is rich in hydroxyl group. The solid-phase microextraction probe can be used for directly carrying out high-selectivity extraction on a trace amount of malachite green and structure-similar compounds with triphenylmethane and amino groups from a variety of complicated matrix samples, and the extracted probe can be used for directly carrying out electrospraying mass spectroscopy on a target object under normal-pressure open conditions, so that the probe has extremely high sensitivity and ideal repeatability.

Description

technical field [0001] The invention belongs to the technical field of extraction probes, and more specifically relates to a surface-modified molecularly imprinted solid-phase microextraction probe and its preparation and application. Background technique [0002] Malachite Green (Malachite Green, MG), also known as aniline green, base block green, etc., is a cationic azo compound, belonging to triphenylmethane dyes, widely used in ceramics, textiles, leather, Food colorants and cytochemical stains. In previous fishery production, malachite green was used as an insect repellant, insecticide and preservative, and was widely used in the prevention and treatment of saprolegniasis, gill mold and parasitic diseases of aquatic animals, but it has persistent, Typical characteristics of persistent organic pollutants such as biotoxicity and bioaccumulation, in recent years, malachite green has become a focus of general attention and research in the fields of biological, food and env...

Claims

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Application Information

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IPC IPC(8): C08F220/18C08F220/06C08F212/08C08F220/28C08F230/08C08J9/26B01J20/26B01J20/30G01N30/06G01N30/08
CPCB01J20/268C08F220/18C08F220/1804C08J9/26C08J2201/0424C08J2333/08G01N30/06G01N30/08G01N2030/062C08F220/06C08F212/08C08F220/281C08F230/08
Inventor 黄艳荧马艳芳杨运云张敏郑文柔刘珍峰李培英
Owner FOSHAN UNIVERSITY
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