Micro-extraction monolithic column of ionic liquid polymer capillary tube and preparation method thereof

An ionic liquid and capillary technology, which is applied in the fields of polymer materials and analytical chemistry, can solve the problems such as the monolithic ionic liquid column, which affects the stability and extraction performance of the column, and achieves easy regulation of reaction conditions, uniform internal structure and pore size distribution. , the effect of long service life

Active Publication Date: 2014-06-04
FUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, when pretreating complex samples, the easy swelling and shedding of the polymer material itself in organic solvents affects the stability of the column and the improvement of extraction performance to a certain extent.
However, there have been no research reports on ionic liquid monolithic columns that can be used for capillary solid-phase microextraction.

Method used

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  • Micro-extraction monolithic column of ionic liquid polymer capillary tube and preparation method thereof
  • Micro-extraction monolithic column of ionic liquid polymer capillary tube and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Mix 0.05 g lauryl methacrylate and 0.05 g 1-allyl-3-octylimidazolium hexafluorophosphate binary monomer, 0.15 g ethylene glycol dimethacrylate crosslinker, 0.003 g Azobisisobutyronitrile initiator and mixed porogen (n-propanol 0.3 g, butanediol 0.3 g) were mixed at room temperature and ultrasonically oscillated for 20 min to obtain a reactant solution, which was injected into a vinyl-treated capillary. Both ends were sealed, immersed in a water bath at 60°C to initiate the polymerization reaction for 15 h; after the reaction was completed, the column was washed with methanol to remove unreacted monomers, cross-linking agents and porogens in the capillary, and 1-ene was obtained after drying Propyl-3-octylimidazole ionic liquid-dodecyl methacrylate-ethylene glycol dimethacrylate polymer monolithic column for capillary microextraction.

[0019] figure 1 A and B show the global and local images of the SEM images of the monolithic column. The figure shows that after dopi...

Embodiment 2

[0024] 0.05 g dodecyl methacrylate monomer, 0.15 g ethylene glycol dimethacrylate crosslinking agent, 0.003 g azobisisobutyronitrile initiator and mixed porogen (n-propanol 0.3 g, Butanediol 0.3 g), mixed at room temperature and ultrasonically oscillated for 20 min to obtain a reactant solution, injected into a vinyl-treated capillary, sealed at both ends, immersed in a 60°C water bath to initiate polymerization for 15 h; after the reaction was completed, Rinse the column with methanol to remove unreacted monomers, cross-linking agents and porogens in the capillary, and dry to obtain dodecyl methacrylate-ethylene glycol dimethacrylate polymer capillary solid-phase microextraction monolithic column.

[0025] figure 1 C and D show the global and local images of the SEM images of the monolithic microextraction column. It can be seen from the figure that, compared with the ionic liquid polymer microextraction monolithic column in Example 1, the ionic liquid-free polymer microex...

Embodiment 3

[0027]0.05 g lauryl methacrylate and 0.05 g 1-allyl-3-hexylimidazolium hexafluorophosphate binary monomer, 0.2 g ethylene glycol dimethacrylate crosslinker, 0.003 g AZBN initiator and mixed porogen (n-propanol 0.3 g, butanediol 0.3 g) were mixed at room temperature and ultrasonically oscillated for 20 min to obtain a reactant solution, which was injected into a vinyl-treated capillary tube. The end was sealed, and immersed in a 70°C water bath to initiate a polymerization reaction for 16 h; after the reaction was completed, the column was washed with methanol to remove unreacted monomers, cross-linking agents and porogens in the capillary, and dried to obtain 1-allyl - 3-hexylimidazole ionic liquid - dodecyl methacrylate - ethylene glycol dimethacrylate polymer monolithic column for capillary microextraction.

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Abstract

The invention discloses a micro-extraction monolithic column of an ionic liquid polymer capillary tube and a preparation method thereof. The method comprises the following steps: by adopting imidazolium ionic liquids and dodecyl methacrylate as functional monomers, taking ethylene glycol dimethyl acrylic ester as a cross-linking agent, taking normal propyl alcohol and butanediol as pore-foaming agents and taking azodiisobutyronitrile as an initiator, evenly mixing the raw materials at room temperature in an oscillating manner, and injecting into a vinyl-modified quartz capillary tube; sealing, and carrying out thermal initiation one-step polymerization, so as to obtain the micro-extraction monolithic column of the ionic liquid polymer capillary tube in manners of cleaning and drying. The micro-extraction monolithic column is simple and convenient in synthetic process, controllable in reaction, and low in cost. The prepared micro-extraction column for the capillary tube has good permeability, porosity, and chemical and mechanical stability; a plurality of interaction sites such as an imidazole ring with positive electricity and different lengths of carbon chains and the like are formed on the surface; the micro-extraction monolithic column has good extraction ability on the substances such as phenolic environmental hormone and the like, and is quick to extract, and easy to build an analysis method with high sensitivity by combining with capillary electrochromatography.

Description

technical field [0001] The invention belongs to the field of macromolecular materials and analytical chemistry, and in particular relates to an ionic liquid polymer capillary microextraction integral column and a preparation method thereof. Background technique [0002] In most cases, actual biological samples or environmental samples are often extremely complex, and there are a large number of coexisting substances that affect the separation and detection of the components to be tested, and the content of the components is generally at trace or ultra-trace levels, although instrumental analysis techniques have been achieved so far. With great development, it is still difficult for samples to directly enter the instrument for qualitative and quantitative analysis. About 3 / 4 of the entire analysis process is often used for sample pretreatment. Therefore, the development of efficient sample pretreatment technology (including extraction, purification and enrichment of component...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F220/18C08F226/06C08F222/14C08J9/28B01J20/285B01J20/30B01D15/20
Inventor 吴晓苹吴祥宗丁春玉汤燕虾
Owner FUZHOU UNIV
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