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Method for preparing extraction probe by means of micro-solid phase extraction based on polymer (methacrylic acid-ethyl glycol dimethacrylate)

A technology of ethylene glycol dimethacrylate and methacrylic acid, applied in separation methods, chemical instruments and methods, solid adsorbent liquid separation, etc., can solve problems such as matrix interference, achieve low detection limit and good extraction effect , good effect of testing repeatability

Inactive Publication Date: 2012-10-03
HOHAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, this material is mostly applied in the form of in-tube solid-phase microextraction or polymer monolithic column in-tube solid-phase microextraction. The content of opiates in human urine and basic drugs in serum have been successfully determined. It is susceptible to matrix interference during the processing of complex samples, so the application of this material in the actual detection of complex samples is greatly limited

Method used

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  • Method for preparing extraction probe by means of micro-solid phase extraction based on polymer (methacrylic acid-ethyl glycol dimethacrylate)
  • Method for preparing extraction probe by means of micro-solid phase extraction based on polymer (methacrylic acid-ethyl glycol dimethacrylate)
  • Method for preparing extraction probe by means of micro-solid phase extraction based on polymer (methacrylic acid-ethyl glycol dimethacrylate)

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Take 1mmol of methacrylic acid, 3mmol of ethylene glycol dimethacrylate, 2mL of acetonitrile and 0.011g of azobisisobutyronitrile in a 5mL centrifuge tube and mix well. 2 Remove oxygen for 15min, seal the centrifuge tube and place it in an oven to heat at 60°C for 15h, take out the product and grind it, pass through a 100-mesh sieve to obtain poly(MAA-EGDMA) powder ( figure 1 for scanning electron microscopy).

[0026] Cut the polypropylene film into 2.0cm×1.5cm, fold the long side in half, heat seal both sides with a small plastic sealing machine to ensure that the edges are sealed neatly, add 20mg poly(MAA-EGDMA) powder to the opening of the film bag through funnel drainage, and heat Seal the opening and cut off the protruding part of the edge, immerse the extraction probe in pure water and methanol successively, clean it by ultrasonic for 5 minutes each at a power of 500w, and dry it for later use.

Embodiment 2

[0028] Take 2mmol of methacrylic acid, 3mmol of ethylene glycol dimethacrylate, 1mL of ethyl acetate and 0.011g of azobisisobutyronitrile in a 5mL centrifuge tube and mix well. 2 Remove oxygen for 15 minutes, seal the centrifuge tube and place it in an oven to heat at 60°C for 15 hours, take out the product, grind it, and pass through a 100-mesh sieve to obtain poly(MAA-EGDMA) powder.

[0029] Cut the polypropylene film into 2.0cm×1.5cm, fold the long side in half, heat seal both sides with a small plastic sealing machine to ensure that the edges are sealed neatly, add 20mg poly(MAA-EGDMA) powder to the opening of the film bag through funnel drainage, and heat Seal the opening and cut off the protruding part of the edge, immerse the extraction probe in pure water and methanol successively, clean it by ultrasonic for 5 minutes each at a power of 500w, and dry it for later use.

Embodiment 3

[0031] Take 3mmol of methacrylic acid, 4mmol of ethylene glycol dimethacrylate, 3mL of toluene and 0.011g of azobisisobutyronitrile in a 5mL centrifuge tube and mix well. 2Remove oxygen for 15 minutes, seal the centrifuge tube and place it in an oven to heat at 60°C for 15 hours, take out the product, grind it, and pass through a 100-mesh sieve to obtain poly(MAA-EGDMA) powder.

[0032] Cut the polypropylene film into 2.0cm×1.5cm, fold the long side in half, heat seal both sides with a small plastic sealing machine to ensure that the edges are sealed neatly, add 20mg poly(MAA-EGDMA) powder to the opening of the film bag through funnel drainage, and heat Seal the opening and cut off the protruding part of the edge, immerse the extraction probe in pure water and methanol successively, clean it by ultrasonic for 5 minutes each at a power of 500w, and dry it for later use.

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Abstract

The invention discloses a method for preparing an extraction probe by means of micro-solid phase extraction based on a polymer (methacrylic acid-ethyl glycol dimethacrylate), belonging to the field of micro-solid phase extraction. The extraction probe comprises a hollow fiber membrane and extracting filler; a membrane bag stops macromolecules and granular impurities by the hollow fibre membrane; the extraction material adsorbs the target micromolecular compounds; trace of organic solvent is used to resolve the target compounds. The extraction filler is polymer (methacrylic acid-ethyl glycol dimethacrylate) with acidic side groups and a hydrophobic skeleton, and has relatively strong adsorption performance for target substances in water; the hollow fibre membrane is a polypropylene membrane that prevents macromolecules and granular impurities form entering so as to eliminate interference of a matrix to a great extent. Therefore, the micro-solid phase extraction has purification function for samples and is used for direct analysis of samples with complicate matrixes; and the analysis range of a substrate is expanded.

Description

technical field [0001] The invention relates to a method for preparing a micro-solid-phase extraction film bag by using a polymer as an extraction filler. Specifically, poly(methacrylic acid-ethylene glycol dimethacrylate) is used as an extraction agent, and a polypropylene film is used as a protective film to carry out the preparation method of the extraction film bag. Background technique [0002] In recent years, sample pretreatment technology has developed rapidly, especially various solvent-free or less-solvent, membrane extraction sample pretreatment technologies have been in-depth research and development, such as liquid phase microextraction (LPME), solid phase microextraction (SPME), Stir bar extraction (SBSE), etc. However, these pretreatment techniques usually require enrichment and purification steps when analyzing some samples with complex matrices, which are cumbersome and consume a large amount of toxic organic solvents. Hollow fiber membrane-protected solid-...

Claims

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Application Information

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IPC IPC(8): B01J20/26B01J20/28B01J20/30B01D15/10C08F222/14C08F220/06
Inventor 王永花金少格王秋英陆光华
Owner HOHAI UNIV
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