Hydrophilic hydroxyl polychlorinated biphenyl molecularly imprinted solid-phase extraction filler as well as preparation method and application thereof

A hydroxypolychlorinated biphenyl and molecular imprinting technology, applied in other chemical processes, chemical instruments and methods, etc., can solve the problems of staying in the evaluation stage of polymer physical properties and separation performance, and solve the problem of template leakage, The effect of improving selectivity and improving sensitivity

Inactive Publication Date: 2014-11-19
YANTAI INST OF COASTAL ZONE RES CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] After literature search, it was found that the article "selective separation of hydroxyl polychlorinated biphenyls (HO-PCBs) by the structural recognition on the molecularly imprinted polymers: direct separation of The thyroid hormone active analogues from mixtures” used the sol-gel method to synthesize molecularly imprinted hydroxy-PCBs and used them as packing materials for chromatographic columns to separate hydroxy-PCBs from mixtures, but the article only Stuck in the evaluation of polymer physical properties and separation performance

Method used

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  • Hydrophilic hydroxyl polychlorinated biphenyl molecularly imprinted solid-phase extraction filler as well as preparation method and application thereof
  • Hydrophilic hydroxyl polychlorinated biphenyl molecularly imprinted solid-phase extraction filler as well as preparation method and application thereof
  • Hydrophilic hydroxyl polychlorinated biphenyl molecularly imprinted solid-phase extraction filler as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Take the separation and enrichment of hydroxy-polychlorinated biphenyls in water as an example. The operation steps are as follows:

[0045] (1) Preparation of hydrophilic hydroxy-polychlorinated biphenyl molecularly imprinted solid-phase extraction packing material and solid-phase extraction column

[0046] Dissolve 0.5 mM 4,4-dihydroxy-biphenyl and 3 mM acrylamide in 30 mL of acetonitrile solution, place in the dark for 1 hour, add 3 mM trimethylolpropane trimethacrylate (TRIM) and 50 mg azobisiso Nitrile (AIBN). Nitrogen gas was passed into the solution for 10 minutes, sealed, and reacted in a constant temperature oil bath at 70°C for 24 hours. The obtained polymer was vacuum-filtered to dryness, placed in a filter paper tube, and methanol-acetic acid (7:3, V:V) was used as the eluent, and the dummy template molecules were removed by Soxhlet extraction for 48 hours. The obtained imprinted polymer was vacuum-dried at 45° C. for 24 hours to obtain a hydroxy-PCB molecu...

Embodiment 2

[0057] Take the separation and enrichment of hydroxy-polychlorinated biphenyls in water as an example. The operation steps are as follows:

[0058] (1) Preparation of hydrophilic hydroxy-polychlorinated biphenyl molecularly imprinted solid-phase extraction packing material and solid-phase extraction column

[0059] For the preparation method of hydrophilic hydroxypolychlorinated biphenyl molecularly imprinted solid-phase extraction filler and solid-phase extraction column, except that the template molecule is changed to 0.5mM 4-hydroxybiphenyl and 0.5mM 2-hydroxybiphenyl, please refer to the steps in Example 1 for other steps (1).

[0060] (2) Use the obtained solid-phase extraction column to separate and enrich the hydroxy-PCBs in the water

[0061] For the method of separating and enriching hydroxy-polychlorinated biphenyls in water using the obtained solid-phase extraction column, please refer to step (2) in Example 1.

Embodiment 3

[0063] Take the separation and enrichment of hydroxy-polychlorinated biphenyls in water as an example. The operation steps are as follows:

[0064] (1) Preparation of hydrophilic hydroxy-polychlorinated biphenyl molecularly imprinted solid-phase extraction packing material and solid-phase extraction column

[0065] For the preparation method of hydrophilic hydroxypolychlorinated biphenyl molecularly imprinted solid-phase extraction filler and solid-phase extraction column, except that the functional monomer is changed to 2,6-diaminopyridine, please refer to step (1) in Example 1 for other steps.

[0066] (2) Use the obtained solid-phase extraction column to separate and enrich the hydroxy-PCBs in the water

[0067] For the method of separating and enriching hydroxy-polychlorinated biphenyls in water using the obtained solid-phase extraction column, please refer to step (2) in Example 1.

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Abstract

The invention belongs to the technical field of hydroxyl polychlorinated biphenyl separation and enrichment, and particularly relates to a hydrophilic hydroxyl polychlorinated biphenyl molecularly imprinted solid-phase extraction filler as well as a preparation method and an application thereof. Hydroxyl biphenyl compounds serving as virtual template molecules have a polymerization reaction in the presence of a hydrophilic functional monomer, a hydrophilic cross-linking agent, a pore-foaming agent and an initiator and the virtual template molecules are removed after the reaction is completed, thus obtaining the hydrophilic high-selectivity hydroxyl polychlorinated biphenyl molecularly imprinted solid-phase extraction filler; the preparation method comprises the following steps of: carrying out a precipitation polymerization reaction of the virtual template molecules in the presence of the hydrophilic functional monomer and the cross-linking agent to prepare hydroxyl polychlorinated biphenyl molecularly imprinted polymer microspheres; and filling a polypropylene solid-phase extraction column with the obtained imprinted polymer to prepare a hydroxyl polychlorinated biphenyl molecularly imprinted solid-phase extraction column. According to the invention, a molecularly imprinted polymer is synthesized by adopting a virtual template method, so that a template leakage problem is solved under the condition that good imprinting effect is effectively guaranteed; in addition, use of a great deal of poisonous and harmful hydroxyl polychlorinated biphenyl is avoided.

Description

technical field [0001] The invention belongs to the technical field of separation and enrichment of hydroxy polychlorinated biphenyls, and in particular relates to a hydrophilic hydroxy polychlorinated biphenyl molecularly imprinted solid-phase extraction filler and its preparation and application. Background technique [0002] Polychlorinated biphenyls (PCBs), as a synthetic organic compound, are widely used in electric power, chemical industry and other fields. Its physical and chemical properties are stable and difficult to degrade, and it has high toxicity, high carcinogenicity and high bioaccumulation. With the development of industrial and agricultural production, PCBs have become a global pollution. In bacteria and higher organisms (including humans), PCBs are oxidatively metabolized by cytochrome P450 enzymes to mainly form hydroxypolychlorinated biphenyls (OH-PCBs). Because the chemical structure of OH-PCBs is similar to thyroid hormone, it has estrogen-like effec...

Claims

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Application Information

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IPC IPC(8): C08F220/56C08F222/14C08F226/06C08J9/26B01J20/26B01J20/285B01J20/30
Inventor 秦伟赵焱梁荣宁苏阳
Owner YANTAI INST OF COASTAL ZONE RES CHINESE ACAD OF SCI
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