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Method for producing solid-phase microextraction capillaries

A capillary and extraction technology, applied in the field of analytical chemistry, achieves the effect of simple method, good reproducibility and large extraction capacity

Inactive Publication Date: 2007-11-21
WUHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there is no extraction capillary for solid phase microextraction prepared by glycidyl methacrylate-ethylene glycol dimethacrylate polymer.

Method used

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  • Method for producing solid-phase microextraction capillaries
  • Method for producing solid-phase microextraction capillaries
  • Method for producing solid-phase microextraction capillaries

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Functional monomer: 5 μL of glycidyl methacrylate, crosslinking agent: 65 μL of ethylene glycol dimethacrylate, porogen: 10 μL of toluene and 180 μL of dodecanol, initiator: 0.8 mg of azobisisobutyronitrile Mix and stir evenly at room temperature, pour into a vinyl-modified quartz capillary, seal, and initiate polymerization at 60°C for 20 hours. After the polymerization is completed, fully wash the capillary with methanol to remove unreacted monomers, crosslinking agents and Pore ​​agent. The obtained monolithic column capillary was washed with 0.1 mol / L sulfuric acid for 3 hours to obtain a hydroxylated glycidyl methacrylate-ethylene glycol dimethacrylate polymer monolithic column capillary.

[0020] With the prepared hydroxylated glycidyl methacrylate-ethylene glycol dimethacrylate polymer monolithic column capillary as the extraction medium, the in-tube solid phase microextraction and high performance liquid chromatography provided by the patent number ZL 03 2 54844...

Embodiment 2

[0025] Functional monomer: 10 μL of glycidyl methacrylate, crosslinking agent: 70 μL of ethylene glycol dimethacrylate, porogen: 15 μL of toluene and 210 μL of dodecanol, initiator: 1.2 mg of azobisisobutyronitrile Mix and stir evenly at room temperature, sonicate for 10 minutes to remove air bubbles, pour into a vinyl-modified quartz capillary, seal, and initiate polymerization at 65°C for 16 hours. After the polymerization reaction is complete, the capillary is thoroughly washed with acetonitrile to remove unreacted monomer, crosslinker and porogen. The resulting monolithic column capillary was washed with 0.5 mol / L sulfuric acid for 3 hours to obtain a hydroxylated glycidyl methacrylate-ethylene glycol dimethacrylate polymer monolithic column capillary.

[0026] With the prepared hydroxylated glycidyl methacrylate-ethylene glycol dimethacrylate polymer monolithic column capillary as the extraction medium, the in-tube solid phase microextraction and high performance liquid c...

Embodiment 3

[0031]Functional monomer: 5 μL of glycidyl methacrylate, crosslinking agent: 70 μL of ethylene glycol dimethacrylate, porogen: 20 μL of toluene and 180 μL of dodecanol, initiator: 1.0 mg of azobisisobutyronitrile Mix and stir evenly at room temperature, sonicate for 5 minutes to remove air bubbles, pour into a vinyl-modified quartz capillary, seal, and initiate polymerization at 55°C for 24 hours. After the polymerization reaction is completed, the capillary is thoroughly washed with acetonitrile, methanol, or tetrahydrofuran to remove unreacted monomers, crosslinkers, and porogens. Then rinse the resulting glycidyl methacrylate-ethylene glycol dimethacrylate polymer monolithic column capillary with diethylamine for 2 hours, seal it, and react at 70°C for 5 hours to obtain diethylamine derivatized methacrylic acid shrink Glyceride-ethylene glycol dimethacrylate polymer monolithic column capillary.

[0032] Using the monolithic column capillary of glycidyl methacrylate-ethylen...

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Abstract

The invention is concerned with the prepare method of capillary for solid phase microextraction. The methacrylic acid glycidyl is function monomer, the ethyleneglycol dimethacrylate is vulcanizing agent, toluene and dodecyl are mixed pore-causing agent, and 2,2'-azobisisobutyronitrile is initiator. Mix and mill the stuff and pour into quartz capillary disposed with ethylene, close and heat to polymerization. After the reaction, use solvent to clean capillary and remove the rudimental monomer, vulcanizing agent and pore-causing agent to get whole capillary with the polymer of methacrylic acid glycidyl and ethyleneglycol dimethacrylate. Use vitriol to clear the whole capillary to get hydroxylation, or clear the capillary with diethylamine and close to heat at 65 to 75 degree to get the capillary with the polymer of methacrylic acid glycidyl and ethyleneglycol dimethacrylate derived from diethylamine. The method is easy and low cost and the extraction agency stuff is fit to set up a credible and high sensitive analysis method.

Description

technical field [0001] The invention relates to a method for preparing a capillary for solid-phase microextraction, in particular to the preparation of a monolithic column extraction capillary of glycidyl methacrylate-ethylene glycol dimethacrylate polymer that can be used in solid-phase microextraction The method belongs to the field of analytical chemistry. Background technique [0002] At present, the analytical objects faced by analytical chemistry are becoming more and more complex, and the coexisting interfering substances are complex and may interact with the target analyte. The concentration of the target analyte is usually trace or ultra-trace level. Therefore, an effective Sample pretreatment technology plays a key role in the establishment of analytical methods. So far, there have been more than a dozen sample pretreatment methods, the purpose of which is to remove the sample substrate interference as much as possible and to enrich the analytes in the sample to t...

Claims

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Application Information

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IPC IPC(8): B01D15/08B01D11/00
Inventor 冯钰锜文毅
Owner WUHAN UNIV
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