Strong cation exchange polymer integral column capillary tube and its production method and use

A strong cation exchange and capillary technology, which is applied in the field of strong cationic polymer monolithic column capillary and its preparation, can solve the problems of inability to meet detection technical requirements, good reproducibility, long time consumption, etc., and achieve reliable and high-sensitivity analysis methods, extraction The effect of large capacity and high enrichment factor

Inactive Publication Date: 2009-06-24
WUHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This type of method is efficient and sensitive, but it takes a long time, and the price of the solid phase extraction column is relatively high, which cannot meet the detection technical requirements proposed by the Ministry of Science and Technology (accurate detection, low detection limit, good reproducibility; suitable for on-site, rapid detection; technical Low product or equipment cost, low operating cost)
But there is no 2-acrylamide-2-methyl-1-propanesulfonic acid-ethylene glycol dimethacrylate polymer monolithic column capillary with strong cation exchange effect and hydrophobic interaction, and it is used as a Literature reports on extraction media for the detection of melamine in dairy products

Method used

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  • Strong cation exchange polymer integral column capillary tube and its production method and use
  • Strong cation exchange polymer integral column capillary tube and its production method and use
  • Strong cation exchange polymer integral column capillary tube and its production method and use

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Example 1: Preparation of 2-acrylamide-2-methyl-1-propanesulfonic acid-ethylene glycol dimethacrylate polymer monolithic column capillary

[0021] Functional monomer: 10 mg of 2-acrylamide-2-methyl-1-propanesulfonic acid, cross-linking agent: 70 μL of ethylene glycol dimethacrylate, porogen: 220 μL of N,N-dimethylformamide and 110mg of polyethylene glycol 6000, initiator: 1mg of azobisisobutyronitrile, mixed and stirred evenly at room temperature, poured into a vinyl-modified quartz capillary, sealed, and initiated the polymerization reaction at 60°C for 12 hours, and the polymerization reaction was completed Finally, fully wash the capillary with acetonitrile to remove unreacted monomers, cross-linking agents and porogens to obtain 2-acrylamide-2-methyl-1-propanesulfonic acid-ethylene glycol dimethacrylate polymer as a whole Column capillary.

Embodiment 2

[0022] Example 2: Preparation of 2-acrylamide-2-methyl-1-propanesulfonic acid-ethylene glycol dimethacrylate polymer monolithic column capillary

[0023] Functional monomer: 15 mg of 2-acrylamide-2-methyl-1-propanesulfonic acid, cross-linking agent: 65 μL of ethylene glycol dimethacrylate, porogen: 200 μL of N,N-dimethylformamide and 100mg of polyethylene glycol 4000, initiator: 2mg of azobisisobutyronitrile, mixed and stirred evenly at room temperature, ultrasonically oscillated for 10 minutes to remove oxygen, poured into a vinyl-modified quartz capillary, sealed, and initiated at 65°C After 14 hours of polymerization reaction, after the completion of the polymerization reaction, fully wash the capillary with methanol to remove unreacted monomers, cross-linking agents and porogens to obtain 2-acrylamide-2-methyl-1-propanesulfonic acid-ethylene glycol Dimethacrylate polymer monolithic column capillary.

Embodiment 3

[0024] Example 3: The detection of melamine in milk powder samples with the monolithic column capillary prepared in Example 1 as the extraction medium

[0025] The polymer monolithic column microextraction device provided by the patent number ZL200520095986.1 was used to analyze the melamine in the milk powder sample by using the high performance liquid chromatography analysis method.

[0026] Extraction and chromatographic analysis conditions: the extraction flow rate is 0.06mL / min, and the extraction time is 5min. The analytical column was an Agilent Eclipse XDB-C8 column (150mm×4.6mm i.d., 5μm), and the mobile phase was a buffer solution (pH3.0) containing 10mM citric acid and 5mM sodium octanesulfonate and methanol at a ratio of 80:20 (v / v) Mixing, flow rate 1 mL / min. The detection condition is an ultraviolet detector, and the detection wavelength is 240nm.

[0027] Milk powder sample analysis: Collect milk powder samples, add 1% trichloroacetic acid solution and 22g / L ...

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Abstract

The invention discloses a monolithic column capillary of a strong cation interchange polymer as well as a preparation method and the application thereof. The monolithic column capillary comprises a quartz capillary modified by ethylene and a monolithic column generated through in-situ polymerization in the capillary; and the monolithic column is 2-acrylamide-2-methyl-1-propane sulfonic acid-glycol dimethyl methacrylate polymer. A 2-acrylamide-2-methyl-1-propane sulfonic acid is taken as a functional monomer, glycol dimethyl methacrylate is taken as a crosslinking agent, N, N-dimethylformamide and polyethyleneglycol are taken as a mixed perforating agent, and azodiisobutyronitrile is taken as an evocating agent; the materials are evenly stirred at room temperature, injected into the quartz capillary modified by ethylene, and then sealed off; polyreaction is performed through heating; and the monolithic column capillary is finally prepared through being washed by acetonitrile or methanol. The monolithic column capillary has strong cation interchange sites on a skeleton surface, has good biocompatibility, does not perform nonspecific adsorption with proteins, etc., is used as an extraction medium for measuring melamine in milk-containing products, and has large extraction capacity and high enrichment factor.

Description

technical field [0001] The invention relates to a strong cationic polymer monolithic column capillary and a preparation method thereof, in particular to a 2-acrylamide-2-methyl-1-propanesulfonic acid-ethylene glycol dimethacrylate polymer monolith The column capillary and the use of the monolithic column capillary for the detection of melamine in milk products belong to the field of polymer chemistry and also belong to the field of analytical chemistry. Background technique [0002] At present, the analytical objects faced by analytical chemistry are becoming more and more complex, the concentration of the analyte is usually trace or ultra-trace level, and the coexisting interfering substances are complex and may interact with the target analyte. Therefore, an effective Sample preparation techniques play a key role in the development of analytical methods. [0003] In 2007, a pet food contamination incident broke out in the United States. After the event, the investigation ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/60G01N30/08C08F220/56C08F220/18C08J9/06
Inventor 冯钰锜马乔胡西洲
Owner WUHAN UNIV
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