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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 eliminate matrix interference
Another difficulty in analysis is that malachite green is a water-soluble polar compound, which is very difficult to separate from polar complex matrices

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

Embodiment 1

[0043] The preparation of embodiment 1 solid-phase microextraction probe

[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 2-ethylhexyl acrylate functional monomer And 0.05g octylphenol polyoxyethylene ether, 0.05g sodium lauryl sulfate emulsifier, stir 15min in emulsifier (20000rpm / min) and prepare pre-emulsion for subsequent use.

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

[0046] 3. Reduce the stirring speed, drop the remaining pre-emulsion and potassium persulfate solvent into the seed emulsion within 4 hours to obtain an acrylate emulsion, and continue to drop vin...

Embodiment 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 2-ethylhexyl acrylate functional monomer With 0.15g sodium lauryl sulfate and secondary octylphenol polyoxyethylene ether emulsifier, stir 15min in emulsifying machine (10000rpm / min) and prepare pre-emulsion for subsequent use.

[0052] 2. Add 13mL of deionized water, 0.1g of sodium bicarbonate, and about 7.5g of pre-emulsion into a four-neck flask equipped with a thermometer, reflux condenser, and stirrer, raise the temperature to 110°C under stirring at 250rpm / min, and then add half 5mL of 0.11mol / L azobisisobutyronitrile initiator, after reacting for 3h, a bluish seed emulsion was obtained.

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

Embodiment 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 2-ethylhexyl acrylate functional monomer and 0.26 g octylphenol polyoxyethylene ether, 0.26g sodium lauryl sulfate emulsifier, stirred in an emulsifier (30000rpm / min) for 15min to prepare a pre-emulsion for subsequent use.

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

[0060] 3. Reduce the stirring speed, drop the remaining pre-emulsion and potassium persulfate solvent into the seed emulsion within 4 hours to obtain an acrylate emulsion, and continue to drop vinyl tris (β-methoxyethoxy) silane, After reacting for...

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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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